Dual Core Manual

CD2.
01-002 DUAL SPINDLE CORE DEPOSITION SYSTEM

REFERENCE MANUAL
ASI/SILICA MACHINERY, LLC.

Head Office 515 Loring Avenue Los Angeles, CA 90028 United States of America PH: +1 (818) 920 1962 FAX: +1 (818) 920 1792 www.asisilica.com Manufacturing Facility 1210 East 223rd Street Carson CA 90745 United States of America PH:+1 (310) 835 3368 FAX: +1 (310) 835 3378 www.asisilica.com
CORE DEPOSITION MACHINE CD2.01-002
Table of Contents
1.0 2.0
2.1 2.2 2.3 2.4 2.5 2.6 2.7
Safety........................................................................................................................................... 7 Material Safety Data Sheets .................................................................................................. 8

MSDS OXYGEN ...................................................................................................................................9 MSDS HYDROGEN ...........................................................................................................................19 MSDS NITROGEN .............................................................................................................................27 MSDS SILICON TETRACHLORIDE...............................................................................................35 MSDS HYDROGEN CHLORIDE .....................................................................................................44 MSDS GERMAINIUM TETRACHLORIDE.....................................................................................53 MSDS ACETYLENE ..........................................................................................................................59
3.0 3.1 4.0

4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 4.10
System Requirements........................................................................................................... 68 Space Requirements ............................................................................................................. 68 Core Deposition Operating Procedure ............................................................................. 69
Materials/Tools needed for the process .............................................................................................69 How to set up and load mandrel assembly........................................................................................69 Checklist for an OVD Core run .........................................................................................................72 Loading a recipe ..................................................................................................................................74 Editing a Recipe ..................................................................................................................................75 Running a Recipe ................................................................................................................................78 OVD Core Run Characteristics .........................................................................................................79 Shutdown Procedure...........................................................................................................................82 Preparation for sintering ....................................................................................................................83 Materials Usage Totals .......................................................................................................................84
5.0
5.1 5.2
Core Deposition Software .................................................................................................... 85

Startup.................................................................................................................................................85 Function Screens .............................................................................................................................85
Configuration Screen Configuration Screen ..................................................................................................................... 86 ..................................................................................................................... 86
5.2.1 5.2.2
D/A output controls (Blue) ....................................................................................................................................... 87 A/D input indicators (Green) ................................................................................................................................... 87 DIO Out (Orange) .................................................................................................................................................... 87 DIO In (Gray) ........................................................................................................................................................... 87 5.2.3 5.2.4 5.2.5 Motor Screen ..................................................................................................................................... 88 .................................................................................................... 90 ...................................................................................................... 90
Scales and Controllers Screen Image Configuration Screen
ASI/SILICA MACHINERY LLC
5.2.6 5.2.7 5.2.8
Monitor Screen
............................................................................................................................... 91
Monitor Mode Controls and Indicators .................................................................................................. 92 Recipe Editor Screen ..................................................................................................................... 94
5.2.9 5.2.10 5.2.11 5.2.12 5.2.13
Manual Torch Screen MFC Sizing Screen Information Screen Alarm Screen Auto Zero Screen
.................................................................................................................... 95 ..................................................................................................................... 98 ...................................................................................................................... 98 .............................................................................................................................. 99 ..................................................................................................................... 101
5.2.14
Gas Usage Screen
................................................................................................................... 102
6.0
6.1 6.2 6.3 6.4 6.5 6.6 6.7
ASI GeCl4 Vaporizer System............................................................................................. 104

GeCl4 Vaporizer System Description........................................................................................104 GeCl4 Vaporizer System Fume Stream ....................................................................................107 GeCl4 Vaporizer System Operation...........................................................................................108 GeCl4 Vaporizer System Process Mode ..................................................................................109 GeCl4 Vaporizer System Purge Mode.......................................................................................109 GeCl4 Vaporizer System Start Up ..............................................................................................109 How To Fill The GeCl4 Vaporizer System ................................................................................110
Pre-requisites ............................................................................................................................................. 110 Instructions................................................................................................................................................. 110
6.7.1 6.7.2
6.8
6.8.1 6.8.2
Warming Up the Vaporizer (and Burp the Vaporizer During Heat Up ..........................111
Pre-requisites ............................................................................................................................................. 111 Instructions................................................................................................................................................. 111
6.9
6.9.1 6.9.2 6.9.3
GeCl4 Vaporizer System Controlled Fume Production........................................................111

Pre-requisites ............................................................................................................................................. 111 Start Up Sequence .................................................................................................................................... 112 Shut Down Sequence ............................................................................................................................... 112
6.10
GeCl4 Vaporizer System Maintenance .....................................................................................113

How to Swap Out a GeCl4 Mass Flow Controller (MFC) ............................................................ 113 Pre-Requisites ............................................................................................................................. 113 Pre-Requisites ............................................................................................................................. 113 Purge MFC to be Changed ....................................................................................................... 113 Cool Down the GeCl4 Vaporizer ............................................................................................. 113 Warm Up the GeCl4 Vaporizer ................................................................................................. 114 6.10.1.1 6.10.1.2
6.10.1
6.10.2
Method .................................................................................................................................................... 113
6.10.2.1 6.10.2.2 6.10.2.3
CORE DEPOSITION MACHINE CD2.01-002 6.10.3 Replacing the (BARITRON) Pressure Sensor And/OR Rupture Disc ..................................... 114 Pre-Requisites ............................................................................................................................. 114 Equipment Needed ..................................................................................................................... 114 Method ........................................................................................................................................... 114
6.10.3.1 6.10.3.2 6.10.3.3
Appendix 1 - Full State Table .............................................................................................................. 116 7.0 Dual Spindle Clad Deposition System Maintenance .................................................. 117
7.1
7.1.1 7.1.2 7.1.3 7.1.4 7.1.5
Maintenance & Lubrication of Linear Positioning Tables ...................................................117

Drive Mechanisms .................................................................................................................................... 117 Acme Screws ............................................................................................................................................. 117 Ball Screws ................................................................................................................................................. 117 Lubrication (Acme Screws) .................................................................................................................... 117 Lubrication (Ball Screws)........................................................................................................................ 118
7.2 7.3 7.4

7.4.1
Trouble Shooting the End Burner Flame .................................................................................119 Applying Heating Tape .................................................................................................................120 Torch Alignment .............................................................................................................................121
Torch Position Relative to Mandrel Centerline ................................................................................. 121
7.5 7.6 7.7
Emptying Vaporizer Tank and Preheater .................................................................................123 Maintenance & Lubrication of Linear Positioning Tables ...................................................131 Temperature Controller Setup ....................................................................................................132
8.0
8.1
Dual Spindle Clad Deposition System Maintenance .................................................. 137

Load Cell Readout and Load Cell Calibration ........................................................................137
Scale Readout Screen.............................................................................................................................. 137 Dual Spindle Scale Readout Screen Descriptions ........................................................................... 137 Zero ..................................................................................................................................................... 137 Mode ................................................................................................................................................... 137 Tare ..................................................................................................................................................... 138 Print ..................................................................................................................................................... 138 _/Test/Clr ............................................................................................................................................ 138 1/Tare/Val ........................................................................................................................................... 138 2/Status/Bar....................................................................................................................................... 139 3/Lb/Kg ............................................................................................................................................... 139 4/ ......................................................................................................................................................... 139 5/ ....................................................................................................................................................... 139 6 Setpoint............................................................................................................................................. 139 7 Option ............................................................................................................................................... 140 8/Cal ..................................................................................................................................................... 140 9/ ......................................................................................................................................................... 140 0/Exit.................................................................................................................................................... 140 Enter .................................................................................................................................................... 140 8.1.1 8.1.2
8.1.2.1 8.1.2.2 8.1.2.3 8.1.2.4 8.1.2.5 8.1.2.6 8.1.2.7 8.1.2.8 8.1.2.9 8.1.2.10 8.1.2.11 8.1.2.12 8.1.2.13 8.1.2.14 8.1.2.15 8.1.2.16 8.1.3 8.1.4 8.1.5
Dual Spindle Scale Calibration Procedure (Hard Calibration)....................................................... 141 Setting The Zero Calibration Value ...................................................................................................... 141 To zero the scales ................................................................................................................................ 143 Setting The Span Calibration Value ..................................................................................................... 144
8.1.4.1
CORE DEPOSITION MACHINE CD2.01-002 8.1.6 8.1.7 8.1.8 Checking the Weight of the System. .................................................................................................... 145 Tare and Zero the Scale Read Outs. .................................................................................................... 145 Trouble Shooting the Scale Readout. .................................................................................................. 145
9.0
9.1 9.2 9.3
Spindle Leg Chiller Connection ....................................................................................... 146

Uncrating and Mechanical Installation .....................................................................................146 Electrical Installation PDU ...........................................................................................................148 Programming and Temperature Setting...................................................................................149
Selecting the Sensor Type...................................................................................................................... 149 UM4300 Controller Temperature Settings .......................................................................................... 150
9.3.1 9.3.2
9.4
Chiller Programming Chart ..........................................................................................................151
10.0
10.1
Trouble-Shooting For Deposition & Sintering & Process Activities ...................... 152
Process Activities ..........................................................................................................................152
Introduction ........................................................................................................................................... 152 Ideal Refractive Index Profile ........................................................................................................... 152 Various modes in the recipe............................................................................................................... 153 10.1.1.1 10.1.1.2 1. 2. 3. 4. 5. 6. 7. 8. 10.1.2 10.1.3 10.1.4 10.1.4.1 10.1.4.2 10.1.4.3 10.1.5 10.1.6 10.1.7 10.1.8 10.1.8.1 10.1.8.2 10.1.9 10.1.10 10.1.11 10.1.12 10.1.13 10.1.1
Mandrel Flame Polish Mode ......................................................................................................................... 153 Carbon Coating Mode ................................................................................................................................... 153 Carbon Flame Polish Mode ........................................................................................................................... 153 Centerline Mode (SiCl4 only) ......................................................................................................................... 153 Core A Mode (SiCl4 + GeCl4) ........................................................................................................................ 153 Core B Mode (SiCl4 + GeCl4) ........................................................................................................................ 153 Clad Mode Oscillation 1 (SiCl4 only) ......................................................................................................... 153 Clad Mode Oscillation 2 (SiCl4 only) ......................................................................................................... 153 Tuning centerline refractive index ................................................................................................... 154 Tuning Refractive Index Delta ........................................................................................................... 154 Examples of Index Profiles and Methods of Tuning ................................................................... 155 Profile with a high dip ........................................................................................................................ 155 Delta with slanted slopes .................................................................................................................... 155 Delta Height Adjustment ................................................................................................................... 156 Changing SiCl4 and GeCl4 flows in the recipe ............................................................................. 157 Oscillations at the Delta ..................................................................................................................... 158 How To Calculate Core Weight Given a Core/Clad Diameter Ratio......................................... 159 Measurement Diffraction Type Problem ......................................................................................... 160 Example 1: Power loss in the center ................................................................................................ 160 Example 2: Power loss at the edges ................................................................................................... 160 How To Do A Manual Density Profile .............................................................................................. 161 Troubleshooting Torch Buildup. ...................................................................................................... 163 Flow Analysis ........................................................................................................................................ 165 Recipe Command Spreadsheet ........................................................................................................ 167 Sudden Change in Index Profile (delta/shape) Between Preforms ......................................... 170 Surface Smoothness (ripples) .......................................................................................................... 170 Density Control ..................................................................................................................................... 170
10.2
PHYSICAL TUNING / CONTROL .................................................................................................170
10.2.1 10.2.2
CORE DEPOSITION MACHINE CD2.01-002 10.2.3 1) 2) 3) 4) 5) 6) 10.2.4 10.2.5 10.2.6 10.2.7 10.2.8 Deposition Rate .................................................................................................................................... 171 Traverse Speed ............................................................................................................................................... 171 Temperature/ heat (hydrogen flow) ............................................................................................................... 171 SiCl4 flow rate ............................................................................................................................................... 171 Cleanliness of fume tubes .............................................................................................................................. 171 Makeup flow rate ........................................................................................................................................... 171 Alignment ...................................................................................................................................................... 171 Diameter Variation ............................................................................................................................... 172 Soot Cracking at Handle Interface ................................................................................................... 173 Splits ........................................................................................................................................................ 173 Warts ....................................................................................................................................................... 174 Core/Clad Cracking After Sintering ................................................................................................. 174 Modefield Diameter Out of Specification ....................................................................................... 175 Cutoff Wavelength Out of Specification ......................................................................................... 176 Core/Clad Concentricity ..................................................................................................................... 177 High Attenuation................................................................................................................................... 178 Gas Bubbles .......................................................................................................................................... 180
10.3
FIBER TUNING/CONTROL ...........................................................................................................175
10.3.1 10.3.2 10.3.3 10.3.4 10.3.5
1.0
Safety
Forward
In common with all manufacturing equipment, the ATMOSPHERIC CHEMICAL VAPOR CORE SYSTEM contains potential hazards to the operator.
Warning
In order to avoid serious injury or death and or damaging the equipment, it is very important that only qualified and properly trained people should be allowed to operate these equipment. The ACVC system runs on chemicals and gases that could be: Extremely corrosive, and or simple asphyxiant. Therefore: All piping connecting these chemicals to the system must be tested for leaks and certified prior to operation. Piping materials must be compatible with the commodity to be handled. The site must be equipped with gas detectors that are capable of detecting any leaks in the area, and shutting down the supply at the source. The equipment must be connected to a pollution control system that is capable of handling the type of chemicals used and generated. The ducting connecting the equipment to the pollution control system must be capable of handling heat and corrosion.
Material Safety Data Sheets are provided in this section for the various chemicals used and generated; operators of this equipment should take the time and familiarize themselves with the information provided in these data sheets, and follow the safety guidelines and the handling procedures they contain.
2.0
Material Safety Data Sheets
The following section contains the material safety data sheets for the material used with the ACVC02 Dual Spindle Core Deposition System.
2.1
MSDS OXYGEN
10
11
12
13
14
15
16
17
18
2.2
MSDS HYDROGEN
19
20
21
22
23
24
25
26
2.3
MSDS NITROGEN
27
28
29
30
31
32
33
34
2.4
MSDS SILICON TETRACHLORIDE
35
36
37
38
39
40
41
42
43
2.5
MSDS HYDROGEN CHLORIDE
44
45
46
47
48
49
50
51
52
2.6
MSDS GERMAINIUM TETRACHLORIDE
1.6.1. PRODUCT AND COMPANY IDENTIFICATION Product Identifier: Germanium Tetrachloride General Use: Telecommunications fiber production Product Description: High purity inorganic chloride MANUFACTURER: Eagle-Picher Technologies, LLC Electro-Optic Materials P. O. Box 737 Hwy. 69A East Quapaw, OK 74363 EMERGENCY TELEPHONE NUMBERS: Eagle-Picher EOM (01) 918/673-1650 (USA) 8 am-4:30 pm CST M-F INFOTRAC 800/535-5053 24 hours everyday 1.6.2. COMPOSITION/INFORMATION ON INGREDIENTS CAS # CHEMICAL NAME % VOLUME EINECS# 10038-98-9 Germanium Tetrachloride 100 233-166-7 Chemical Formula : GeCl4 Hazard Symbols: C Risk Phrases: 14 34 OSHA REGULATORY STATUS: While this material is not classified as hazardous under OSHA regulations, this MSDS contains valuable information critical to the safe handling and proper use of the product. This MSDS should be retained and available for employees and other users of this product. 1.6.3. HAZARDS IDENTIFICATION EMERGENCY OVERVIEW: Warning! Water reactive, producing toxic and corrosive fumes. Causes eye and skin irritation. Causes irritation of the digestive and respiratory tracts. Fumes in moist air. May form hazardous decomposition products which may cause irritation and possible burns. Vapors can cause eye irritation. TARGET ORGANS: None known POTENTIAL HEALTH EFFECTS: ROUTES OF ENTRY: Skin Contact: Yes Skin Absorption: No Ingestion: Yes Eye Contact: Yes Inhalation: Yes HEALTH EFFECTS: Irritant: Yes Sensitization: No Teratogen: No Reproductive Hazard: No
53
CORE DEPOSITION MACHINE CD2.01-002 EXPOSURE LIMITS: PEL-OSHA: None Listed TLV-ACGIH: None Listed NIOSH: None Listed INHALATION: Irritating to upper and lower respiratory tracts. Symptoms may include coughing, labored breathing and excessive salivary and sputum formation. Excessive irritation of the lungs causes acute pneumonitis and pulmonary edema which could be fatal. EYE CONTACT: Lacrymator. May cause irritation and possible burns. SKIN CONTACT: May cause irritation, and possible burns, especially if skin is wet or moist. . INGESTION: May cause severe gastrointestinal tract irritation and possible burns. CHRONIC: May cause liver and kidney damage. NFPA Hazard Codes System HMIS Hazard Codes Ratings Not Published Not Published 0 = No Hazard 1 = Slight Hazard 2 = Moderate Hazard 3 = Serious Hazard 4 = Severe Hazard See Section 8 for Personal Protection information. See Section 11 for Toxicological information. POTENTIAL ENVIRONMENTAL EFFECTS: The ecotoxicity and environmental fate of Germanium Tetrachloride is currently not available. 1.6.4. FIRST AID MEASURES INHALATION: Remove victim of exposure to fresh air immediately. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Seek medical aid immediately. EYE CONTACT: Immediately flush eyes, including under eyelids, with large amounts of water for at least 15 minutes. Seek medical aid immediately. SKIN CONTACT: Remove contaminated clothing (including shoes) as soon as possible. Flood skin with large amounts of water for at least 15 minutes. Seek medical aid immediately.
54
CORE DEPOSITION MACHINE CD2.01-002 INGESTION: If swallowed, DO NOT induce vomiting. Never give anything by mouth to an unconscious person. If conscious, have victim rinse mouth liberally with water. Seek medical aid immediately. 1.6.5. FIRE FIGHTING MEASURES Flashpoint and Method: None / Not Applicable Flammable Limits: Not Flammable Autoignition Temperature: None LEL (%): None UEL (%): None HAZARDOUS COMBUSTION PRODUCTS: None Sensitivity to Mechanical Shock: None Sensitivity to Static Discharge: None NFPA Rating: Not Published FIRE FIGHTING INSTRUCTIONS: Germanium Tetrachloride REACTS VIOLENTLY WITH WATER OR STEAM TO PRODUCE HYDROCHLORIC ACID. FIRE FIGHTING EQUIPMENT: Use normal firefighting procedures which include wearing NIOSH/MSHA approved self-contained breathing apparatus in pressure-demand. Wear MSHA/NIOSH approved, flame and chemical resistant clothing; hats, boots and gloves. If without risk, remove material from fire area. EXTINGUISHING MEDIA: Use media appropriate for surrounding materials. Product reacts with water to form corrosive fumes. 1.6.6. ACCIDENTAL RELEASE MEASURES Evacuate personnel from affected area. Use proper personal protective equipment as indicated in Section 8. SPILLS / LEAKS: Absorb spill with inert material then place into a chemical waste container. Provide ventilation. Refer to section 13 for disposal considerations. 1.6.7. HANDLING AND STORAGE HANDLING: Use only in a well ventilated area. Do not allow water to get into container because of violent reaction. Avoid contact with eyes, skin and clothing. Avoid ingestion and inhalation. Wash thoroughly after handling. Remove contaminated clothing and wash before reuse. STORAGE: Store in tightly closed container in a cool , dry, well ventilated area away from incompatible substances (See Section 10).
55
CORE DEPOSITION MACHINE CD2.01-002 1.6.8. EXPOSURE CONTROLS/PERSONAL PROTECTION EXPOSURE LIMITS: PEL-OSHA : None Listed TLV-ACGIH: None Listed NIOSH: None Listed ENGINEERING CONTROLS: The use of local exhaust forced ventilation is recommended to prevent accumulation above the exposure limits of hydrochloric acid. Provide mechanical ventilation of confined spaces. Use explosion-proof ventilation equipment in accordance with electrical codes. PERSONAL PROTECTION: RESPIRATOR: NIOSH/MSHA approved respirator with an organic vapor cartridge. Follow OSHA regulations in 29 CFR 1910.134 or European Standard EN 149 as appropriate. Always use a NIOSH or European Standard EN 149 approved respirator when necessary. Positive pressure air line with full face mask and escape bottle or self-contained breathing apparatus should be available for emergency use. PROTECTIVE CLOTHING: Protective Safety Glasses or Chemical safety goggles as described by OSHA regulations in 29 CFR 1910.133 or European Standard EN166 as appropriate. Rubber gloves, lab coat and apron, flame and chemical resistant coveralls as appropriate. Other / General: Safety Shower and Eyewash fountain available. 1.6.9. PHYSICAL AND CHEMICAL PROPERTIES Parameter Value Units Vapor Pressure: 72 Not Applicable Specific Gravity (H2O=1): 1.844 g/cm3 Solubility in Water: Hydrolyzes Not Applicable pH: Not Available Not Applicable Boiling Point: 82 - 84 @ 760.00 mm Hg C Decomposition Temperature: Not Available Not Applicable Viscosity: Not Applicable Not Applicable Vapor Density (Air=1): Not available Not Applicable Evaporation Point: Not Available Not Applicable Freezing / Melting Point: -49.5 C Odor: Acrid, irritating Not Applicable Odor Threshold: Not Available Not Applicable Appearance: Colorless Not Applicable Physical State: Fuming Liquid Not Applicable Molecular Formula: GeCl4 Not Applicable Molecular Weight: 214.4 Not Applicable 1.6.10. STABILITY AND REACTIVITY CHEMICAL STABILITY: Stable under normal temperatures and pressures.
56
CORE DEPOSITION MACHINE CD2.01-002 INCOMPATIBLE MATERIALS AND CONDITIONS TO AVOID: Rapidly reacts with water or steam to form hydrochloric acid, which reacts to most metals and many organic materials with the evolution of heat and hydrogen gas. Incompatible materials, contact with water or exposure to moist air. HAZARDOUS DECOMPOSITION PRODUCTS: Hydrochloric acid. Hazardous Polymerization: Will not occur. 1.6.11. TOXICOLOGICAL INFORMATION RTECS# : LY5225000 LD50/LC50: LC50=44 gm/m3/2H (inhalation, mouse) Carcinogenicity: Not listed by ACGIH, IARC, NIOSH, or OSHA Epidemiology: Not Available Teratogenicity: Not Available Reproductive Effects: Not Available Neurotoxicity: Not Available Mutagenicity: Not Available Other: Not Available See Section 3 for Potential Health Effects. 1.6.12. ECOLOGICAL INFORMATION Ecotoxicity: Not Available Environmentl Fate: Not available Physical / Chemical: Not Available Other: Not Available 1.6.13. DISPOSAL CONSIDERATIONS Return to supplier or dispose of in accordance with all current local, State and Federal Regulations. RCRA D-Series Manimum Concentration of Contaminants: None Listed RCRA D-Series Chronic Toxicity Reference Levels: None Listed RCRA F-Series: None Listed RCRA P-Series: None Listed RCRA U-Series: None Listed 1.6.14. TRANSPORT INFORMATION
Shipping Name Hazard Class UN Number Packing Group DGC
US DOT Corr Liq, Acidic, Inorg, N.O.S.* 8 3264 II -IMO Corr Liq, Acidic, Inorg, N.O.S. 8 3264 II -IATA Corr Liq, Acidic, Inorg, N.O.S.* 8 3264 II -RID/ADR Corr Liq, Acidic, Inorg, N.O.S. 8 3264 II 8 (66B) Can. TDG Corr Liq, Acidic, Inorg, N.O.S. 8 (9.2) UN3264 II --
57
CORE DEPOSITION MACHINE CD2.01-002 1.6.15. REGULATORY INFORMATION US FEDERAL: TSCA (Toxic Substance Control Act): Listed on the TSCA inventory. Health Safety Reporting List: Not listed. Chemical Test Rules: Not listed. Section 12b: Not listed TSCA Significant New Use Rule: No SNUR under TSCA SARA: Section 302 (RQ): No RQ Section 302 (TPQ): No TPQ Section 313: Not Reportable. Clean Air Act: Does not contain any hazardous air pollutants. Does not contain any Class 1 Ozone Depletors. Does not contain any Class 2 Ozone Depletors. Clean Water Act: Not listed as hazardous Substance under the CWA. Not listed as Priority Pollutants under the CWA. Not listed as Toxic Pollutants under the CWA. OSHA: Not considered highly hazardous by OSHA. STATE: Germanium Tetrachloride is not present on State lists from CA, PA, MN, MA, FL, or NJ. California No Significant Risk level: Not listed. European / International : European labeling in accordance with EC Directives: Hazard Symbols: C Risk Phrases: R 14 Reacts violently with water. R 34 Causes Burns Safety Phrases: S 25 Avoid contact with eyes. S 36/37/39 Wear suitable protective clothing, gloves, and eye/protection. S 45 In case of accident or if you feel unwell, seek medical advice immediately (Show the label where possible). S 8 Keep container dry. WGK (Water Danger / Protection): No information available. Canada: Is listed on Canadas DSL/NDSL List. Does not have a WHMIS Classification. Is not listed on Canadas Ingredient Disclosure List. Exposure Limits: OEL-RUSSIA : STEL 1 mg/m3 1.6.16. OTHER INFORMATION MSDS Creation Date: September , 1979 MSDS Revision Date: February, 2001 THE STATEMENTS CONTAINED HEREIN REPRESENT THE BEST INFORMATION CURRENTLY AVAILABLE TO US, AND IS OFFERED FOR INFORMATIONAL PURPOSES ONLY. THIS INFORMATION IS INTENDED TO BE FOLLOWED BY PERSONS HAVING RELATED TECHNICAL SKILLS AND AT THEIR OWN DISCRETION AND RISK. SINCE CONDITIONS AND MANNER OF USE ARE OUTSIDE OUR CONTROL, WE MAKE NO WARRANTIES, EXPRESS OR IMPLIED, AND ASSUME NO LIABILITY IN CONNECTION WITH ANY USE OF THIS INFORMATION.
58
2.7
MSDS ACETYLENE
59
60
61
62
63
64
65
66
67
3.0 3.1
System Requirements Space Requirements
BLOWER
VAPORISERS AND WATER BATH
CHILLER
200 cm CTRL CABIN MAIN GAS PANEL DEPOSITION MACHINE
FRONT OF MACHINE
441 CM
68
4.0
Core Deposition Operating Procedure
4.1 Materials/Tools needed for the process

Mandrel Handle Three O-rings: 75 Vinton; Size 2.4 x 7.6 V block inserts (replace if deteriorated) Teflon Plug Gases and Chemicals (Hydrogen, Oxygen, Nitrogen, Acetylene, GeCl4, SiCl4) Isopropanol and clean-room wipers Igniter (to light up the torch) Allen wrench (to tighten cap onto chuck)
4.2 How to set up and load mandrel assembly

Clean the mandrel thoroughly with alcohol and appropriate wiper. Slide two O-rings (75 Viton; Size 0.312ID x 0.5) into the mandrel so that they are about 200mm and 250mm from the end with a bigger diameter. The mandrel will be pulled out after deposition, so it is designed to be tapered, with diameter of one end bigger than the other.
1) Slide the handle into the mandrel from the end that has a smaller diameter.
69
4) Slide the handle all the way so that the o-rings are inside the handle as shown on the picture below. Leave about 35mm-40mm of mandrel length behind the handle.
Notice that the 2 O-rings have rolled towards the left when the handle is being slid through. The Orings need to be located at a maximum of 130mm from the wide end of the handle. Too close to the end burner flame will cause the O-rings to burn and melt. 5) Insert the hollow Teflon plug through the mandrel from the left end and push in firmly to help secure the handle on the mandrel.
6) Put in the chuck cap and an o-ring into the mandrel at the handle end, leaving about 1 cm of mandrel length behind.
7) Insert that end into the left chuck and lay the other end onto the Teflon V-block. (Replace Vblock inserts if deteriorated)
70
8) Secure the mandrel by tightening the two screws, which hold the cap to the chuck.
9) Adjust the handle position so that the distance between the tip of the handle and the end of the chuck cap is 273mm +/- 2mm.
71
4.3 Checklist for an OVD Core run

1. SiCl4 delivery system ready? Valves open? 2. SiCl4 tank level is high enough? 3. GeCl4 delivery system ready? Valves open? 4. Pushing Oxygen has a pressure of 30psi-35psi? 5. GeCl4 tank level is high enough? 6. Acetylene delivery system ready? 7. Are exhaust flows about 2300 ft/min for the center and 800 ft/min for the sides? 8. Chamber and filters are clean? 9. Temperatures of chemlines, makeup lines, SiCl4 vaporizer tank and SiCl4 vaporizer chamber are close/ equal to set points? 10. SMR temperature and pressure and hotbox temperature of the GeCl4 vaporizer system close/equal to set points? 11. Re-zero GeCl4 and SiCl4 mfcs? 12. Replace V block inserts? (If the original ones deteriorated) 13. Scrubber is on?
72
After loading in the mandrel and completing the items on the startup checklist, the user is now ready to use the program and start a run. In all times ASI software, Core Version X.X should be running, if this is not so, click on the desktop. After configuration, the program should be on standby/ready mode, showing the main screen as below.
The user can access various functions of the program by using the icons on the top of the screen.
73
4.4 Loading a recipe

In order to run a recipe, that recipe has to be loaded first by clicking on main screen. Then the recipe editor screen will be shown as below. icon on the top of the
Click on the icon on the top left corner. A directory will appear, select the appropriate recipe. You can only load a recipe with a seq extension. The selected recipe will be shown in a spreadsheet format called recipe editor. The first column displays a description of what the step does. The second column contains action commands and the third column displays input parameters, which are to be passed to the corresponding commands. The last column shows the units of the parameters, these units do not have any impact on recipe execution. After loading a recipe, you may click on to return to the main screen.
74
4.5 Editing a Recipe

Editing a recipe is also being done on the recipe editor screen. A complete reference of the functions and arguments available to use in the sequence editor is provided. The sequence looks like an Excel spreadsheet, but you cannot type in the cells directly. To create or modify a recipe, use the Recipe Editing tools:
The test name and units are comment fields that they do not get executed and are present to make the recipe steps more clear. The VI name is a ring list of all the commands available to the sequence editor. The input buffer contains the arguments that will be passed to the selected function. The number of arguments will depend on the particular function. The delete button deletes an entire row. Use of the other controls will be illustrated in the following examples: To modify an existing line:
In this example, we want to change MFC 4 setpoint from 15 to 20 lpm. Select the row and click
75
The current parameters are now displayed in the text boxes. The comma (,) is always used as the field delimiter. Select the desired field in the input buffer.
Change to the desired setting, 20.
Click on The new values is updated:
To create a new line, the process is similar. For example, we want to add a 1 second delay between row 54 and 55: Select either row 54 or 55. You can insert a new row above or below the selected row. In this case we will select row 55. Click on
Click on
and select a VI from the ring list:
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Then fill (overwrite) the other fields of the editing tool.
Click on
The new row is now inserted. Note: If row 54 was selected previously, One can also insert a blank line by using should be used. and with empty editing cells.
To copy and paste a line, click on the line that is to be copied, and then click on , editing cells will then be filled with by the copied values. Click on the line that is to be pasted and click .
Before exiting, save changes you might want by clicking on
icon.
To proceed, click on the icon. This will set the current recipe into the computers memory. This action will also return to the main screen.
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4.6 Running a Recipe

After loading a recipe, click on the monitor mode icon, recipe. The following screen will be shown. Then for starting a run based on the loaded
different actions will be taken according to the recipe. The left upper window shows the status and which command is being executed. After some initialization of motors, controllers communication, etc, a dialog will show up as below:
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This dialog prompts for operators name, performs ID, carbon coating length, perform length, initial weight of the mandrel with handle setup, core weight, final weight (core plus clad weight) and data file name. The core weight determines when the program switches core mode (depositing both SiCl4 and GeCl4) to clad mode (SiCl4 only). The final weight determines when the run will be terminated. The data file name is the name of the file where all the process variables will be written. After entering information into the dialog box, click on OK and the program will continue to run according to the sequence in the recipe. If for any reasons that the run needs to be aborted, click onto the icon on the upper right hand corner of the monitor mode screen. Another option is to press on the EMO button on the machine. This will shut down the whole machine including power.
4.7 OVD Core Run Characteristics

This system is able to run continuously while monitoring and controlling the process. Since each run is a significant investment, any shut down must be avoided. The operator must make sure that the machine and process will have all the chemical resources that it needs prior to the start of the run. In addition: Constant supply of N2 is required for purging when the unit is not in run mode. 100-PSI gas is required to operate the Nupro valves in the vaporizer and gas cabinet. Sufficient push gas pressure for both GeCl4 and SiCl4 delivery. Then sequence of events take place as follows, according to a standard recipe: Data acquisition begins. HEPA blower turns on. SiCl4 vaporizer tank temperature ramps to set point. Preform rotation initiates. Traverse and end burner move to their starting positions. Tare scales. Ignite torches and end burners. The operator will need a flame starter. During ignition of the left torch, the program will ask if operator is ready to ignite. When OK is clicked, hydrogen will start flowing. Use a flame starter with a tip at least 5 inches long to start the flame. As a safety measure, the computer will ask for confirmation of ignition. If the computer does not receive a confirmation, it will shut off hydrogen and start the ignition sequence over again. After the left torch is ignited. The process will go through different modes. A typical ASI core-making recipe includes seven modes in a run. 1. 2. 3. 4. Mandrel Flame Polish Mode Carbon Coating Mode Carbon Flame Polish Mode Centerline Mode (SiCl4 only) 79
5. 6. 7. 8.
Core A Mode (SiCl4 + GeCl4) Core B Mode (SiCl4 + GeCl4) Clad Mode-Oscillation 1 (SiCl4 only) Clad Mode-Oscillation 2 (SiCl4 only)
Depending on the recipe, the operator will often asked to confirm ignition and move torches in at the transition of the first 5 modes. Before doing so (clicking ok), make sure that all gases and chemicals flows are close to their set points. When SiCl4 starts flowing out from the torches, the flames should immediately turn bright and white and have a well-defined shape, similar to the images below.
Flame with GeCl4 only is not bright and white like flame with SiCl4. There is only a very minor brightness difference between flame with and without GeCl4. One way to test is to place a piece of glass on top of the torches to see if there is any chemical deposited on it. During the run, operator should make sure that the process parameters behave in a normal fashion. From the monitor screen, observe the following for the SiCl4vaporizer: Tank pressure: The pressure and tank temperature for the vaporizer is directly related. Therefore as tank temperature is increasing, tank pressure will also increase and vice versa. The normal operating tank temperature is 770C-790C. This line normally has a cyclic pattern due to on/off SiCl4 refill. Every refill will bring down the tank temperature by a few degrees. The tank then slowly heats up back to the set temperature, then another refill lower the temperature again and so on. If the tank pressure continues to increase (line is going up), this is a sign of running out of SiCl4, i.e., no refill. This might due to empty SiCl4 source tank or insufficient push gas pressure.
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Loadcell:
The vaporizer has been programmed to refill whenever the level drops below 3.5V and stop filling when the level has reached 3.8V, as shown on the right most indicator above the monitor.
Normal Exit Sequence When the current preform weight exceeds target weight, the program will commence the exit routine.
Cut gases and chemicals to the torches. Cut gases to the end burners. End traverse oscillations. Prompt to stop rotation. Return to main screen. Put SMR back to purge state. Put Vaporizer tank to standby stage.
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4.8 Shutdown Procedure

In the event that a situation arises where the operator deems it necessary to shut down the process, click on the button located monitor screen.
In doing so, the program will do the following:

Cut off all gases and SiCl4 (and GeCl4) flow so that the torch and end burners are extinguished. Put SMR to purge state. Put the vaporizer tank temperature controller in standby mode. Prompt operator to stop preform rotation. Return to main screen. The computer will take about 5 to 10 seconds from the time the button is toggled to respond. Once pressed, there is no going back.
Emergency Shutdown If the program does not respond, the EMO switch may be used. The EMO will immediately cut all power to every circuit in the system. The EMO is the red button located on top of the left door panel of the deposition cabinet.
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Caution
The EMO should be avoided unless absolutely necessary because it may damage the computers hard drive as well as corrupt the scale and temperature controllers.
If the EMO is used, refer to the RESTART procedure. The EMO is the red button located on top of the left door panel of the deposition cabinet. Restart after an EMO shutdown 1. Press the RESTART button. (Green button next to the EMO red button) 2. During the computers boot up sequence the operator will be asked to run the utility SCANDISK. Select OK and the program will check the hard drive for damage. Usually the program will check the file allocation system and repair a file. If the program goes into a sector-by-sector surface scan, it could be a sign that the hard disk is about to fail. 3. When Windows 2000 is running, click on the clad icon, labeled Core x.x version.
4. ASI software will start running, configuring and return to the standby/main screen.
4.9 Preparation for sintering

After the exit sequence, the program will return to the main screen. Use the motor screen and move preform to the left almost. Let the preform cool down a little and then move it back to the middle. Start a slow rotation and by using a knife, trim off loose soot at both ends, so the ends are flat and hard, as shown as below.
The reason to trim away loose soot is that the soot density difference causes different shrinkage and might add some bending to the preform upon sintering. Take out the preform from the deposition cabinet. Place it in a safe place and let it cool down before pulling out the mandrel. One way to speed up the cooling process is to blow Nitrogen through the mandrel to speed up cooling. Be Careful of the Nitrogen coming out of the mandrel, which is very hot. When the outgoing Nitrogen gets to about room temperature, mandrel can be pulled out.
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To pull out the mandrel, wear gloves, hold the handle and land the preform vertically on the floor, put some cushion in between for protection. Very carefully, tap the preform on the floor but do not break the mandrel. Be cautious; do not smash the bottom part of the soot preform on the floor. When the mandrel pops up through the handle, pull it out upwards. Be careful that the mandrel may be still hot.
When mandrel is taken out the soot core preform is ready to be sintered. Hang preform onto core sinter coupler and refer to sinter process manual for sintering procedure.
4.10 Materials Usage Totals

User can obtain data of material consumed after each run. To analyze the materials usage for a particular run, use the main screen and click on the gas usage icon how to use the Gas Usage Screen. . Refer to software section on
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5.0
Core Deposition Software Startup

, labeled Core x.x version.
5.1
Start the program by double clicking on
The program will configure the motors and solenoids then initialize the communications with the scale, gas panel, HEPA blower, temperature controllers and SiCl4 and GeCl4 vaporizers.
5.2
Function Screens
At the top of the main screen are icons that allow the operator to access the various parts of the program. Below is an explanation and descriptions of each icon.
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5.2.1
Configuration Screen
It allows the user to set the communication parameters to the temperature controllers and scale, the scaling factors to the motors and the file path of the recipe and data file. This does not need to be modified unless new hardware is installed.
5.2.2
Configuration Screen
This screen is normally used for troubleshooting and maintenance. It allows the user to control all the MFCs, valves and relays of the system and verify if they are functioning normally.
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D/A output controls (Blue) These are digital controls for oxygen, hydrogen, acetylene, SiCl4 and GeCl4 MFCs and HEPA blower. The input range is 0-5 volts for oxygen, hydrogen and GeCl4 MFCs; this range covers the whole capacity of the MFC itself. HEPA blower has a range of 0-10V and the four SiCl4 vaporizer MFCs are 4.8-12mA. A/D input indicators (Green) These are indicators of actual output flows of various MFCs and HEPA. Clicking on other variables like vaporizer load cell, pressure sensor, etc, will show their current values. DIO Out (Orange) The three orange columns are DIOs that turn on relays/solenoids. Buttons labeled with GPV# means gas panel valve #, these numbers corresponds to the MFC numbers on D/A and A/D columns. AV# and SMR# are valves on the SiCl4 and GeCl4 vaporizer systems. Other buttons turn on certain devices/functions as labeled; refer to the I/O signal chart for more specifics on the conversions and explanation. In addition, as a safety feature, the enable bit must be ON for the machine to function. On the other hand, the neg enable bit will disable the machine if it switched on. DIO In (Gray) The last column includes DIO In. If description on the buttons label is true, the button will be turned on (green).
Warning
Opening or closing the wrong vaporizer valves could cause contamination and tank overfills. Leaving an oxygen or hydrogen line open without lighting it is a serious explosion hazard.
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5.2.3
Motor Screen
The motor system has three axes, which can be manually controlled by this screen.
Axis 1 Rotational Motor (upper left window) Axis 2 Right End Burner Motor (upper right window) Axis 3 Traverse Motor (lower left window) For Axis 1, user is able to set the velocity (rpm) and acceleration (rpm2) for preform rotation. Similarity, the velocity (mm/min), direction, distance (mm) and acceleration (mm/min2) for Axis 2 and Axis 3 can also be specified. Left and right limits indicators will be on (red) if the corresponding limits are hit.
Start Initiate motion Stop Stop the motor Quit - Return to the main function screen E-Stop Stop all the motors. Set Zero Set encoder reading to zero. Home Send right end burner or traverse back to home positions. The traverse can be set to oscillate through Oscillation Traverse (lower right) window. Enter desired traverse distance (mm) for each pass and set the starting direction from Axis 3, lower left window. V1 is the speed for initial direction and V2 is the speed for the other direction. Offset and total offset are extra distances ran by the traverse aimed to reduce ripples on preform surface. For example, with L=distance, initial direction set to left, offset = 1 and total offset = 3, the traverse will move left and right in a pattern described below.
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L+3 L L-1 L L-1 L L-1 L L+3
The total offset can be any number as long as it can be divided by interlace offset and gives a whole number. Click on to initiate oscillation.
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5.2.4
Scales and Controllers Screen
This function can be used to read and send set points to the temperature and pressure controllers. The program can read the weight and tare the scales. Scale E is the sum of Scale A and Scale B. This screen is useful in verifying that serial communication between the instrument and PC is working properly. Note that communication enabled buttons (located on the right top corner of the screen) have to be clicked on for communications.
The blocks on the screen represent temperature and pressure controllers. Each of them shows the current process value, PV and current set values, SV. PV and SV should read the same as on the controllers themselves when communication is functioning properly. New set points can be inputted . by entering them in the SP window and then click on
5.2.5
Image Configuration Screen
This screen is used to calibrate the camera so that the diameter can be obtained. The procedure is explained in the maintenance section.
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5.2.6
Monitor Screen
This function is used to do a preform run in recipe mode. The screen is as shown below.
There are two types of display objects. One is control and the other is indicator. The program will read a control and a change in an input parameter will occur. Controls can have several forms such as digital, knob and slide. Digital controls have increment buttons. The other type of display object is an indicator. An indicator simply displays a process variable and cannot be used to affect a change in input.
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5.2.7
Monitor Mode Controls and Indicators
The following Controls and Indicators are outlined below along with an explanation as to what these particular icons control or indicate.
This icon should be used if the operator wishes to abort a run. The gases to the torch and end burners will be cut off, the traverse will be sent home and the system will be put back in standby mode. If you choose to abort, you cannot continue where you left off, you must start over again. This is an on/off switch which turns on the water pump of the vaporizer. It is not normally used during operation, it is provided as a redundancy in case the tank temperature controller fails and there is a temperature runaway in the tank.
Shows the alarm screen that allows the user to silence the alarm, check which parameters trigger the alarm and to do alarm setup. Refer to alarm screen for details.
Shuts down GeCl4 flows. Pulls out motor screen. User can enter control parameters through it to override settings from the recipe being run.
Shows the alarm screen that allows alarm settings. Refer to alarm screen for details.
Pulls out scale and temperature control screen. User can input new set values/temperatures to the controllers, overwriting what is on the recipe being run.
Indicates the starting time of the run in AM/PM format.
Shows the elapsed time since the start time in HR:MIN:SEC format.
Shows the elapsed time since the torch was moved into position in HR:MIN:SEC format.
Shows the current recipe being executed.
Shows the Preform ID of the preform being deposited.
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CORE DEPOSITION MACHINE CD2.01-002 The following controls can be used to make changes to various process parameters. It is not necessary to use these features because the recipe already incorporates desirable settings for these process parameters. These controls are not normally used during a run, but add a degree of flexibility to the user.
Warning
Using these controls improperly may cause an entire production run to be wasted and severe damage to the system could occur.
Echoes the final desired weight clad + core) that the operator entered in the beginning of the recipe. This value may be changed during the run should the operator find this necessary. The exit sequence for reaching the final weight is different than the abort exit. If a change is made, be certain the value you enter is greater than the current weight. Or else, the run will be stop immediately. Echoes the final desired core weight that the operator entered in the beginning of the recipe. This value may be changed during the run (core mode) should the operator find this necessary. This weight determines when to switch from core to clad mode. If a change is made, be certain the value you enter is greater than the current weight.
The process can be closely monitored by the above indicators. Density, diameter and mass are physical data of the preform being deposited. Tank volume and tank pressure are used to monitor any abnormal activities within the silica tetrachloride tank, like overfilling, low level, etc. The second column tells the what mode is the process currently in and also the position of the traverse. The third column shows parameters useful for run monitoring and troubleshooting.
This is the main readout/control cluster provides the current process information as well as the ability to manipulate all of the MFCs in the OVD core system. The readouts are grouped by left torch and right torch.
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The two columns in the middle under ACT shows the actual output flows of the MFCs. The two columns to next to them, under SET show the flows set points. These set points come from the recipe being run and can be overwritten. To do so, click on the square (under columns named OVR) next to the set point window, overwrite the desired flow on that window and press ENTER. The color of the window should turn red to indicate that it was modified. Unchecking the square will change the set point back to the value recipe is calling for. All flows for the hydrogen, oxygen and acetylene are in liters/min. For SiCl4 and GeCl4 vapor, the units are grams/minute. If a variable is overwritten, the color of the window will turn red to indicate that it was modified. Flows and other process variables are also recorded on a chart during the run. This serves as a good tool in tracing and monitoring any abnormal activities with the process.
5.2.8
Recipe Editor Screen
This screen is used to load and edit recipe. Refer the to the operation section for instructions.
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5.2.9
Manual Torch Screen
This is a very useful screen/function for diagnostics and testing. It can also be used to deposit a preform with manual control instead of recipe control.
All the gas and chemical vapor flows controls are grouped by left and right torches and end burners. They are color-matched with the torch top view diagram on the upper left of the screen. The GeCl4 SMR Control block allows user to select the desired SMR stage.
Normal mode for the SMR with MFCs being purged with Nitrogen.
When selected, SMR to ready to deliver GeCl4 and there is no flow through MFCs Has to be selected for GeCl4 flows. It opens the guarding valves after the MFCs.
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The Vaporizer Control block is used for refilling SiCl4 (manually and automatically) when running in non-recipe mode.
SiCl4 MFCs are normally being purged at all times, this button, when clicked, will switch off the purge and have the MFCs ready to output SiCl4.
Allows the user to select between auto and manual refilling of vaporizer tank.
For manual refilling only. This button turns on and shuts down SiCl4 filling into the tank.
Turns cooling water circulation on when clicked; used when tank is overheated. Turns on tank heater relay. This has to be on when auto tank temperature control (below) is being used. Auto vaporizer tank temperature control. SiCl4 flows normally require a tank temperature of 770C. Vaporizer tank volume and pressure indicators for monitoring purpose.
The upper section of this manual torch screen includes functions (green buttons) that are useful for depositing a preform in a non-recipe mode and are used to set alarms and exit.
Allows user the set oscillation parameters. Upon clicking, a pop-up screen will be shown:
Starts oscillation using the parameters inputted through the screen above.
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Moving the torches in/out. Start and Stop acquiring manual run data. When clicked, motor screen will pop. Return to manual torch screen by clicking quit or EXIT on the motor screen. Show temperature and scale control screen when clicked. To return to manual torch screen, click on the EXIT. Reset the pass # counter. Get a diameter measurement (that will be shown on the diameter window) whenever this button is clicked. Take diameter measurement every 10 seconds when turned on by clicking. Turns camera light on and off when toggling.
Or
Show either run notes or preform picture on the window in the middle of this screen upon toggling the button.
This button will appear when the window is showing run notes. Click to save notes entered.
Shut down all flows and valves; reset set values to zero.
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Both buttons will show the following alarm screen when clicked.
OR
Refer the alarm screen section on how to setup the alarm. Should the alarm go on when using manual torch screen, click on Alarm Occurrence and the above screen will be shown. This screen allows user to silence the alarm and so informs user which parameter triggers the alarm, those parameter will then be in red instead of green.
5.2.10 MFC Sizing Screen

This screen allows user to enter different conversion factor for different MFC capacities. This screen is reversed for ASI/Silica Machinery.
5.2.11 Information Screen

This is the About ASI software screen, which shows the version of the software.
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5.2.12 Alarm Screen

This screen allows the user the silence any alarm and to set up the alarm system.
Alarms can be set up for deviation in various process variables as labeled on the three columns of buttons on the screen. Alarms that are disabled will be shown in gray. When an alarm is set, the corresponding button is in green. In any cases, should the alarm be triggered, user should go to this screen through main, monitor mode or manual torch screen to silence to alarm. Any deviation that triggers alarm will turn the button red. Operator can ignore the alarm for the rest of the run by clicking on that particular red button; this will change the color from red to white.
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To disable or set up an alarm click on
, an alarm setup screen will appear as below:
To set up or disable an alarm, first select the process parameter from pull-down menu will be shown:
,a
Then enter the deviation on and delay time (seconds). If a process variable is above or below set + value for over a delay time, then the alarm will turn on. To disable an alarm, choose or . After editing the alarm settings, user can choose either to return to the main alarm screen.
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5.2.13 Auto Zero Screen

This screen allows user to do an auto-zeroing on the four SiCl4 vaporizer mfcs.
User can either choose cancel or ok. Upon clicking ok, the system will run a zeroing routine. This can prevent the MFCs from drifting but does not need to be run for every fun, approximately once a week is recommended. Note: Every time ASI software is started, this screen will appear on top of the main screen, asking if auto-zeroing SiCl4 MFCs needs to be done as a reminder.
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5.2.14 Gas Usage Screen

This screen provides data on material used for a particular run. The material usage program is a post run operation that reads and processes data from file. The benefit of streaming data to disk and processing it later is an enormous saving in processor and memory load. In order for the program to recognize the data properly, it must be in the same format as it was originally written to. If the spreadsheet data is manipulated, then the file should be saved under a different file name. The usage for the oxygen, hydrogen and acetylene are calculated by data from the respective MFCs and presented in liters per minute. GeCl4 usage is calculated from MFCs data. The usage for silicon tetrachloride is calculated from the load cell data as we have found that to be a little more reliable parameter than the SiCl4 MFCs. Silicon tetrachloride usage is presented in grams/min. The screen appears as followed:
The actual data recorded for the MFCs and load cell are displayed in spreadsheet form. Each row represents a 10-second interval. Underneath the spreadsheet are the totals for each channel. There are two indicators showing the combined oxygen and hydrogen usage.
To load a file to analyze, click on the load icon, The following dialog will appear.
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Select the file to load and click on
The program will parse the incoming data and fill the rows and columns automatically. The whole process will take a few seconds. If the operator wishes to look at the usage immediately after the conclusion of a run, then click on the icon. By using this step, the program will use the path of the last data file in memory.
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6.0 6.1
ASI GeCl4 Vaporizer System GeCl4 Vaporizer System Description
The GeCl4 vaporizer is a compact unit which when full contains approximately 1 litre of material. The unit is a self- metering design which uses a valve and float arrangement to allow a constant flow of material equal to the amount of material which is being vaporised at any one time to replace a liquid being lost to the process.
Figure 1 GcCl4 Vaporizer The inlet GeCl4 supply is attached to the Manual Valve M1 and must be pressurised so that it is 15 -25 psi above the operating pressure of the vaporizer. The vaporizer operates at an absolute pressure of about 1100 Torr (mmHg), which is approximately equal to 7 psig. The final set point value will depend upon prevailing conditions that will be determined during commissioning. Based on current experience this means that the GeCl4 supply pressure must be between 22 -32 psi.
Failure to do this will mean that the vapour stream will be insufficient to keep up with the flows rates required by the process and this will lead to a potential loss of end product i.e. core rods.
The vaporizer flow streams are left and right handed as per the torches. The GeCl4 fume stream is mixed with the make up oxygen before this mixture is merged with the main SiCl4 stream.
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Figure 2 GeCl4 Vaporizer P&ID
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CORE DEPOSITION MACHINE CD2.01-002 Below is a picture of the GeCl4 Vaporiser Enclosure that is supplied with ASI Core Machines:
Figure 3 - GeCl4 Vaporizer
Legend:
AV-1 = Automatic Valve (AV) N2 Supply AV-3 = Drying Gas AV-5 = GeCl4 Out LHS AV-7 = GeCl4 Out RHS AV-9 = Purge Supply AV-11 = Upper Sight Tube Isolation Valve AV-12 = Lower Sight Tube Isolation Valve MV-1 = Liquid GeCl4 Isolation valve R1 = Purge Regulator R2 = Solenoid Regulator AV-2 = O2 Supply AV-4 = GeCl4 Vapour AV-6 = MFC Purge Valve AV-8 = Vessel Purge AV-10 = GeCl4 Supply Valve
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6.2
GeCl4 Vaporizer System Fume Stream
The Vaporizer fume streams are handed left and right as per the main Torches. The GeCl4 fume streams are injected into their respective Make-up oxygen flows, which are then merged with their respective SiCl4 streams. The pressure of each mixture will be monitored during the Preform production process and may be used to characterise the combined flow. The combined flow is then burnt in the torch flame as it leaves the fume tube.
Makeup Oxygen GeCl4 Vaporizer P SiCl4 Vaporizer Torch Figure 4 - Combined Fume Stream
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6.3
GeCl4 Vaporizer System Operation
The general GeCl4 vaporizer unit has three basic modes of operation:
1. Standby (and Shutdown) 2. Process mode 3. Purge mode
Here Is the State table for the GeCl4 Vaporizer system:

Vaporizer Functions Standby Mode Process Mode Vapor Flow: (MFC-1 and MFC-2) Purge Mode AV6 AV7 AV8 AV9 AV4 AV10 AV11 AV12 MV1 (NO) 1 1 0 0 1 1 0 0 0 0 0 1 0 1 0 0 1 0 0 0 0 0 0 0 1 1 0 Note MV1 can be closed or open for this
AV1 AV2 AV3 AV5 0 0 1 0 0 0 0 0 0 0 1 1
Table 1 - Vaporizer State Table
Legend 0= Closed 1=OpenNO=Normally Open (AV-6 only)
Standby mode In is mode the following will be true: The GeCl4 vessel is at its operating pressure and temperature. The GeCl4 supply is switched off so no new GeCl4 can enter into the float and valve mechanism. All the automatic valves are closed inside the GeCl4 enclosure.
*Note: The manual valve M1 must be closed if the GeCl4 System is to be switched off or if the standby exceeds 24 hours.
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6.4
GeCl4 Vaporizer System Process Mode
In this mode the following will be true: 1. The GeCl4 is at its operating pressure and temperature. 2. The following valves are open. MV-1, AV-10, AV-4, AV-5 and AV7. AV-6 is normally open and will be closed. This will allow vaporised GeCl4 to flow through the Mass flow controllers and to the process while also allowing liquid GeCl4 to replenish the material that has just been consumed by the process. 3. The self- metering vaporizer will take an amount of GeCl4 equal to that which is being used by process at any given time. 4. The pressure gauge indicates the liquid GeCl4 supply pressure which must be maintained at 22 -23 psi.
* * Note the reserve inside the vaporizer will give approximately 10 to 15 minutes of uninterrupted GeCl4 flow if the supply is not maintained. If this occurs there will not be enough GeCl4 present to complete the Preform making process. If this happens then the temperature will be greater than the standard set point and an over temperature alarm will shut the process down. This will prevent unnecessary chemical wastage.
6.5
GeCl4 Vaporizer System Purge Mode
In this mode the vaporizer will be isolated from the mass flow controllers but the MFCs will be being purged from AV1 or AV2 (Depending on whether Oxygen or Nitrogen has been selected to purge the MFCs). The following valves will be open: AV-1 (or AV-2), AV-9, AV-6, AV-5 and AV-7 The Mass flow controllers will have a nominal set point of 10% applied to them.
6.6
GeCl4 Vaporizer System Start Up
Safety systems Shutdown Conditions under normal Operation

1. Over temperature - in the event of the vaporizer exceeding the set point by XXX C an internal sensor will shut the vaporizer heat circuit down. 2. Over pressure - if the pressure exceeds a safe limit (XXX Torr) then the heater circuit will be shut down. 3. Ruptured disc This is a mechanical device and a s such will depend on operator intervention. *
*Note: The control system will respond to these situations but vigilance has to also be maintained by the operators to help prevent chemical/product loos in the event of one of the above.
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6.7
How To Fill The GeCl4 Vaporizer System
This section describes how to fill an empty GeCl4 vaporiser, which has just been installed.
6.7.1 Pre-requisites
1. The machine has been installed and fully leak tested. 2. The Extraction system has been connected to the main exhaust system such that fumes can be released inside the Deposition machine. 3. All Mechanical & Electrical services are available 4. The MFCs have been purged with nitrogen Switch on the GeCl4 system but ensure that power is isolated from the GeCl4 vaporizer heaters (Hot Box and GeCl4 vaporizer). Once this has been done the GeCl4 System can be filled.
6.7.2 Instructions
Switch off /remove the Vaporizer & hotbox Power circuit breakers/fuses. Place the priming magnet under the base of the vaporizer. (See picture above below). 3. Select Manual Mode and open AV10 (and AV4 as they are linked). 4. Open MV-1 to allow the GeCl4 Supply System to feed liquid into the base of the vaporizer. 5. Check the pressure gauge PG2 is indicating between 22 32 psig.
1. 2.
Note: If the pressure gauge reads above this value. Close MV-1 immediately and check the liquid GeCl4 supply pressure.
1. 2. 3. 4. 5. 6. 7. 8.
Wait 5 minutes. Close MV-1 Open AV-11 and AV-12 (the sight tube isolation valves) Observe the height of the liquid in the sight tube. If GeCl4 is seen in the tube close AV-11 and AV-12. Open MV-1 and allow more GeCl4 into the vessel. Repeat steps 3 through 10 until the liquid level is at Normal. Remove the Priming magnet from the base of the vaporizer.
Notes: a) If the GeCl4 level does not change then the valve seat at the base of the vaporizer may need a little encouragement with a light duty plastic hammer. Use the hammer to firmly tap the base of the vaporizer. b) If the liquid GeCl4 is being weighed by the delivery system then the amount of material being transferred can be accurately determined. Vaporizer contents = 1litre = 1.5 kg (Roughly)At this point there is sufficient liquid present to allow a heat up cycle to occur.
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6.8
Warming Up the Vaporizer (and Burp the Vaporizer During Heat Up
Once the vaporizer has been filled (between 75 and 100%) of its capacity then the vessel can be heated up.
a) The machine has been installed. b) The machine has been leak tested. c) The Extraction system has been connected to the main exhaust system such that fumes can be released inside the Deposition machine. d) All Mechanical & Electrical services are available. e) the MFCs have been purged with nitrogen
6.8.2 Instructions
1. 2. 3. 4.
Place the Deposition machine into Standby Mode. Ensure that MV-1, AV-11 and AV12 are closed. Switch on refit the Vaporizer & hotbox Power circuit breakers & fuses. Observe the pressure and temperature rise to their respective set points: The pressure set point is approximately 1150 Torr. The temperature set point is approximately 110 C
The heat-up time will depend on the local conditions and will take between 1 2 hours by which time the system will have reached equilibrium. The system can now be set to Standby Mode. Burping the vessel Note: The main torches must be lit before carrying out this procedure During the warm up sequence the vessel may need to be burped unless the system. This can be achieved by opening valves: AV-4, AV-5 & AV-7 and allowing the mixture of GeCl4 and internal gases to pass through the Mass Flow Controllers (MFCs). This will allow this mixture to be burnt at the main torches.
6.9
GeCl4 Vaporizer System Controlled Fume Production
a) The machine has been installed. b) The machine has been leak tested. c) The Extraction system has been connected to the main exhaust system such that fumes can be released inside the Deposition machine. d) All Mechanical & Electrical services are available. e) The MFCs have been purged with nitrogen
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6.9.2 Start Up Sequence

1. 2. 3. 4. 5. 6. Setup the flows accordingly (as per recipe XXX) Light The Main Torches Allow the flows to stabilise Select Process Mode GeCl4 Fumes will now be delivered to the main torches. Observe that the GeCl4 flows stabilise after several seconds Note: the flame will be a dull white when three is no SiCl4 present tin the flame. 7. Ramp up each flow in 10% steps until the 100% is reached. 8. Allow the flows to stabilise between each 10% increment.
6.9.3 Shut Down Sequence

1. Switch the Gecl4 vaporizer from process to purge mode. 2. Allow the MFCs to be purged for 10 t 15 minutes 3. Switch the operational mode from purge to standby mode The System is now in standby.
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6.10 GeCl4 Vaporizer System Maintenance 6.10.1 How to Swap Out a GeCl4 Mass Flow Controller (MFC) 6.10.1.1 Pre-Requisites
1. The machine has been installed. 2. The machine has been leak tested. 3. The Extraction system has been connected to the main exhaust system such that fumes can be released inside the Deposition machine. 4. All Mechanical & Electrical services are available. 5. The MFCs have been purged with nitrogen for at least one hour at full flow and this flow has been observed.
6.10.1.2
Pre-Requisites
2 x Adjustable wrenches 2 x VCR Gaskets Fresh Ammonia solution or other suitable test for GeCl4 PPE (Personal Protective Equipment) for the technician carrying out the work
6.10.2 Method 6.10.2.1 Purge MFC to be Changed
1. Close MV1 2. Light the main torch(s), which corresponds to the MFC to be changed. (Left or Right torch) 3. Allow the flows to stabilise 4. Put the GeCl4 Vaporiser into Purge Mode 5. Leave for 20-30 minutes (or until the flame indicate that there is no GeCl4 present tin the flame). 6. Switch the torch flame off 7. Allow the Torch to cool for 5 minutes 8. Use the ammonia solution to check the fume stream exiting the Torch for signs of GeCl4 fume. 9. If there are no fumes then the MFC is ready to be removed.
6.10.2.2
1. 2. 3. 4. 5. 6. 7. 8.
Cool Down the GeCl4 Vaporizer
Remove the fuses and open the circuit breakers Allow the GeCl4 Hotbox to cool down (50 C) Open the hot box Release the MFC from the base of the Vaporizer enclosure. Use the adjustable wrenches to undo the VCR connections Remove the faulty MFC Replace the faulty MFC using new VCR Gaskets Use snoop to leak check the new connections
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6.10.2.3
Warm Up the GeCl4 Vaporizer
Warm the GeCl4 Vapouriser Back up 1. Close the hot box 2. Refit the fuses and close the circuit breakers 3. Allow the GeCl4 Hotbox to warm up to operational pressure and temperatures (this will take about 1 hour 110 C) 4. Open MV1 The new MFC is now ready for use.
6.10.3 Replacing the (BARITRON) Pressure Sensor And/OR Rupture Disc 6.10.3.1 Pre-Requisites
1. The machine has been installed. 2. The machine has been leak tested. 3. The Extraction system has been connected to the main exhaust system such that fumes can be released inside the Deposition machine. 4. All Mechanical & Electrical services are available. 5. The MFCs have been purged with nitrogen for at least one hour at full flow and this flow has been observed.
6.10.3.2
Equipment Needed
2 x Adjustable wrenches 2 x VCR Gaskets Fresh Ammonia solution or other suitable test for GeCl4 PPE (Personal Protective Equipment) for the technician carrying out the work
6.10.3.3
Purge GeCl4 Vaporizer
1. Close MV1 2. Light the main torches
Method
3. Allow the flows to stabilise 4. Put the GeCl4 Vaporiser into Process Mode Note the GeCl4 flows will become unstable 5. Leave for 20-30 minutes (or until the vaporizer alarm indicate an over temperature or until the flame indicate that there is no GeCl4 present tin the flame). 6. Open the valves as per the sate table below: This will allow the Nitrogen or Oxygen if AV2 is selected to purge the remaining GeCl4.
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Note: It may be advisable to use oxygen while the GeCl4 is being burnt off, as O2 is combustible.
Vaporizer Maintenance Functions Vaporizer Full Purge to POU
AV1 AV2 AV3 AV5 (NO) AV7 AV8 AV9 AV4 AV10 AV11 AV12 MV1 1 0 1 1 0 0 1 1 1 0 1 1 0
Remove pneumatic supply from AV11
AV6
This will allow the purge Nitrogen to evaporate all of the remaining GeCl4 in the vessel (including what is in Purge The Sight Tube). Once the GeCl4 has been emptied out the torches can be switched off. Cool down the GeCl4 Vaporizer 1. Remove the fuses and open the circuit breakers 2. Allow the vessel to cool down during cool down the next step can be carried out Test for fumes 1. Us the Ammonia solution to check the exhausts flow for signs of fumes 2. When the GeCl4 mixes with ammonia it will produce a dense white cloud. Return to Standby mode 1. Select Standby Mode The GeCl4 Vaporizer is now ready for removal or extended shutdown.
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Appendix 1 - Full State Table

Vaporizer Functions AV1 AV2 AV3 AV5 AV6 AV7 (NO) AV8 AV9 AV4 AV10 AV11 AV12 MV1
Vapor Flow MFC-1 Vapor Flow MFC-2 Vapor Flow MFC-1 &MFC-2 Vaporizer Maintenance Functions Vaporizer Prime Vaporizer Bubble Purge to POU Base Bubble Purge to POU Vaporizer Full Purge to POU
0 0 0
0 0 0
0 0 0
1 0 1
1 1 1
0 1 1
0 0 0
0 0 0
1 1 1
1 1 1
0 0 0
0 0 0
1 1 1
AV6 AV1 AV2 AV3 AV5 (NO) AV7 AV8 AV9 AV4 AV10 AV11 AV12 MV1
0 1 1 1
0 0 0 0
0 0 1 1
0 1 1 1
0 0 0 0
0 0 0 0
0 1 0 1
0 1 0 1
1 1 1 1
1 0 0 0
1 1 1 1
1 1 1 1
1 0 0 0
Remove pneumatic supply from AV11 Remove pneumatic supply from AV10 Remove pneumatic supply from AV11
MFC Maintenance AV6 AV1 AV2 AV3 AV5 AV7 AV8 AV9 AV4 AV10 AV11 AV12 MV1 (NO) Functions MFC-1 Purge to Point of Use MFC-2 Purge to Point of Use MFC-1 & MFC-2 Point of Use 1 1 1 0 0 0 0 0 0 1 0 1 0 0 0 0 1 1 0 0 0 1 1 1 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0
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7.0 7.1
Dual Spindle Clad Deposition System Maintenance Maintenance & Lubrication of Linear Positioning Tables
7.1.1 Drive Mechanisms

The main function of the drive mechanism within a positioning table is to move the load. It is an element that contributes to position accuracy, repeatability, speed, and mechanical system resolution. Two different types of drive mechanisms are used in the deposition and sintering systems.
7.1.2 Acme Screws

Typically use a turcite (polymer), or bronze nut. The nut, which is attached to the table carriage, moves back and forth along the linear bearing system as the screw rotates. The nut threads ride in the matching acme screw threads, much like the ordinary nut and bolt system. All the drives in the sintering system use Acme screws for safety. The drive that controls the position of the right end burner in the deposition station also uses an Acme screw.
7.1.3 Ball Screws

Are the screw of choice for high duty cycle, high speed, and long life applications. The ball screw nut uses one or more circuits of recirculating steel balls which roll between the nut and ball screw grooves, providing an efficient low friction system. The nut, which is attached to the table carriage, moves back and forth with the linear bearing system as the screw rotates. Low wear and long life are key features of a ball screw system. It is used in the deposition station preform translation only, since several thousand passes are expected to be made during each run, and at relatively higher speeds than the other drives.
Acme Screw Ball Screw
7.1.4 Lubrication (Acme Screws)

Because acme screw driven positioning tables have a solid surface contacting a solid surface, sufficient lubrication becomes a must. If there is not proper lubrication, the high frictional forces of these nuts will cause excess wear to the assembly, thus preventing required positioning table life from occurring. Applying lubrication directly onto the entire length of the screw on a regular basis is highly recommended.
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7.1.5 Lubrication (Ball Screws)

Ball driven positioning table, the many built-in pockets within the nut assembly will allow the adhesive properties of most lubricants to be stored, and used by the re-circulating balls for extended periods of time. Thus, as the positioning table moves back and forth, lubrication is applied to the ball screw. The nut assembly will pick up grease, or oil that is spread over the entire length of the screw. Therefore, applying lubrication directly onto the entire length of the screw on a regular basis is recommended.
CAUTION
Use of WD-40, or other cleaning solvents, should strictly be avoided, as they can cause damage
to the linear bearings and drive screw nut.
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7.2
Trouble Shooting the End Burner Flame
If the end burner flame looks a lot shorter, sharper and more bluish than normal, it indicates that its oxygen-hydrogen ratio too high. On the other hand, if the flame looks very orange, wavering, there should be too much hydrogen. Solution: Check if oxygen and hydrogen lines going into the end burners are switched or not. (Note: If the lines are switched, the flame will be in orange and flickering.) Check if the signal cables are going into the correct MFCs. Check if the oxygen and hydrogen MFCs are reading in and outputting the correct flows.
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7.3
Applying Heating Tape
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7.4
Torch Alignment
7.4.1 Torch Position Relative to Mandrel Centerline

Goal: The purpose of this step is to ensure that the torches centerline is parallel to the mandrel while traversing. How to check: a) Load the standard aligning mandrel. b) Measure the distance between two torches (90mm).
c) Using tapes, attach a laser pointer onto the mandrel, pointing it down to the torch, as shown on the Figure (Note: pointer does not necessarily have to be perpendicular to the mandrel, since this is just used as a reference of one torch to another.) d) Focus the laser onto a spot on one torch and remember the location of that spot. e) Move the traverse by the distance between two torches. f) Check if the laser light is landing on the same location of the other torch. g) Run the traverse back and forth between the two torches for a few times to assure the laser is landing on the spot of a torch. How to align: If the laser light is not landing on the same location of the other torch, the torches axis needs to be adjusted. This can be done by loosing a set screws, which hold the torch bracket, adjust the angle and tighten set screw. Repeat check procedure above until torches axis is parallel to mandrels along the traverse.
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7.5
Emptying Vaporizer Tank and Preheater
Objective: The following procedure explains how to empty the vaporizer and preheater. This procedure to be used for: 1) Emptying & flushing vaporizer & preheater, in the event of contamination in Silicon Tetrachloride supply.
2) Replacing the vaporizer and or the preheater.
WARNING
This procedure should only be performed by trained individual(s). Set vaporizer chamber and tank temperature controllers to standby by pressing "ENTER" twice.
1.
2.
Turn off "CHAMBER" in manual function screen by clicking on icon labeled "Chamber" marked below
3.
Turn off the switches at the back of the signal control part and pre-heater.
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Back of Signal Control
Back of Preheater
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CORE DEPOSITION MACHINE CD2.01-002 4.
While waiting for the temperature of the chamber and tank to go down, connect a Tee at MV-11 behind the vaporizer tank. Setup a nitrogen cylinder as shown below. Using 1/4" Teflon tube, connect the metering valve on the nitrogen line to this tee. This line is labeled as outlet 1. Where N2 is coming out, as shown in schematic below.
5.
Connect outlet 2 from the tank drain to the liquid side of an empty tank as shown in this section.
IMPORTANT
The empty tank must be purged with Nitrogen prior to filling.
6.
Connect the gas side of the empty tank to the exhaust ducting as shown in the figure in this section.
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CORE DEPOSITION MACHINE CD2.01-002 7.
With the main valves on empty tank turned off, open bypass valve #1 and set metering valve to 3 lit/min, to allow nitrogen to purge the line from the drain to the empty tank. This process takes about 6 hours.
8.
Turn off bypass valve #1 and open the 2 valves of the empty tank.
9.
Flow N2 into the inlet of pre-heater so as to pump silica liquid out of the vaporizer tank by opening bypass valve #2.
10.
Turn switch AV-1 on the manual function screen, this will open valve AV-11 shown in this section.
11.
Turn off the metering valve completely.
12.
Open MV-11 in the vaporizer.
13.
Check if liquid is flowing out from MV-11 to the empty tank. This should be visible in the semi-transparent teflon line.
14.
Check if tank level indicator is dropping. The level is shown in voltage.
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15.
After the liquid level levels out, allow Nitrogen to purge the vaporizer tank for at least 1 day.
16.
Close MV-11 and the 2 main valves on empty tank. Also close N2 supply to the preheater by turning off AV-11, and shutting off bypass valve #2, set the metering valve on the drain line to 3 lit/min, and open bypass valve #1. Allow lines to purge for at least 2 hours. On the manual faction screen, turn on AV-2 and AV-3, since AV-3 is a normally open value, this will turn the valve OFF, and AV-2 being normally closed, this will turn the value ON. This allows purge N2 to flow into the preheater from the outlet side and forces liquid back to the supply tank through the inlet. Immediately open the main valves on the supply tank to allow liquid to flow back. Important: Make sure bypass valve #2 is off. This procedure takes about 5 hours.
17.
18.
Turn off AV-2 and AV-3 from manual function screen. Please read explanation of the nature of these valves in step 17 above. Turn off the main valves on the supply tank.
19.
Flow N2 into preheater inlet by opening bypass valve #2, and the N2 supply valve. Turn off MV-11, and open AV-16 and AV-14. Allow to purge for an additional day. These are labeled in the manual function screen as AV-6 and Av-4.
20.
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21.
Shut all valves off. The vaporizer and preheater now are empty and ready for removal.
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Vaporizer System Gas Flow Diagram
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Tank Connection for emptying/replacing Vaporizer System
7.6
Maintenance & Lubrication of Linear Positioning Tables
At the beginning of a run, it is necessary to clean the inside of the clad hood of the SiO2 that accumulates during the run. If the hood is not cleaned, the accumulation in the next run will build faster. When the accumulation is enough, it will fall. If it falls onto the preform, the torch may deposit over it, creating an aberration in the final product. The first step is to use a wet rag to wipe down the interior of the clad unit.
Next, use a compressed gas to blow the accumulation off the main exhaust skirt. The majority of the SiO2 should be picked up by the suction of the scrubber. Use a vacuum cleaner to clean off the SiO2 that falls onto the surface. Make sure the vacuum cleaner has a good quality filter so that the particles do not escape into the air.
7.7
Temperature Controller Setup
The controller front menu panel has the following appearance
MENU: Use this button to advance to the next setting or sub menu. ENTER: Access a menu and store settings. /MAX: To scroll through flashing selections and for numbers from 0 to 9. / MIN: Go back to previous top menu and scroll through number fields from left to right. The first two controllers (vaporizer chamber and tank) are process type controllers while the others, for heated lines are RTD type controllers. The setup procedures from temperature controllers are the following:
I. Dip Switch settings for vaporizer chamber and vaporizer tank
II. Vaporizer chamber and vaporizer tank set-up procedures
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133
III. Dip switch settings for oxygen line and chem. line temperature controllers
IV. Oxygen line and chem. line set-up procedure
134
135
V. Dip switch settings for Vaporizer Safety PID
VI. Setup procedure for vaporizer safety PID
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8.0 8.1
Dual Spindle Clad Deposition System Maintenance Load Cell Readout and Load Cell Calibration
8.1.1 Scale Readout Screen

Below is a representation of the Scale Readout Panel.
8.1.2 Dual Spindle Scale Readout Screen Descriptions 8.1.2.1 Zero
Used in Gross mode to zero the display to within the tolerance level. This function can be used as many times as desired as long as the total does not exceed the value entered as the zero tolerance. The zero key is also used to exit a menu after entering number(s) without changing the original number. For example - when entering a Span value (18), the user decides that the original number (15) is OK. By pressing the Zero Key you can exit the menu without changing the original number (15), even though you have typed new numbers and they appear on the display.
8.1.2.2
Mode
In standard controllers, the mode key toggles between gross and net weight. In controllers with any one or all of the mode options (Total Mode, Peak Hold Mode, or Rate of Change Mode) installed the mode key toggles between gross/net weight and the option(s).
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8.1.2.3
Tare
The Tare button captures the current Gross weight at the instant the Tare button is pressed and places it in the tare register setting the Tare Value. The tare value is the difference between the Net (e.g. Vessel weight) and Gross weight (e.g. vessel weight + material weight). You can also type in the Tare Value by using the 1/Tare Val key. The Tare function can also be actuated by activating the appropriate remote function pin. See Remote Function Configuration in Chapter 4.
8.1.2.4
Print
Transmits data to the printer.

NOTE: The serial port must be configured as a printer. If the serial port is not configured as a printer port, the print key is not going to respond, and you cannot print. NOTE: The print function cannot print data if the weight is in motion or exceeds the capacity of the scale.
8.1.2.5
_/Test/Clr
The Test/Clr function Initiates one of the selected tests Self Test - "SLFTST" on the display. Integrated Technician - "IT SEC" on the display. This () key is used to enter a minus sign (-) for a negative number. This function can be used only when the display reads the number 0. The clear "CLR" function is operable when the controller is a menu requiring a numeric input. Use this key to clear the display before entering a new value.
8.1.2.6
1/Tare/Val
This function displays the current Tare value stored in the Tare Register. (See paragraph 5.1.3) This function allows the user, after pressing the "Clr" button, to enter a Tare Value using the numeric keys. To exit the Tare Val menu press the Zero button. The key also enters the digit "1".
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8.1.2.7
2/Status/Bar
The Status/Bar toggles between the mode settings and the bar graph. The Status function indicates the following: Selected Mode Selected Engineering Unit: lbs/kg Status of Relays 1 & 2 The Bar Graph function displays in graphical form the value of the mode (Total, Gross, Net, ROC, Peak) selected in the bar graph setup menu.
NOTE: The bar graph mode and the display mode are totally independent. Make sure you know what mode each are in before reading.
The key also enters the digit "2"
8.1.2.8
3/Lb/Kg
Toggles between read pounds (Lb.) or kilograms (Kg.). The key also enters the digit "3".
8.1.2.9
4/
This key moves forward through a menu, step by step and will wrap to the beginning of the menu. The key also enters the digit "4" Resumes the Self Test
8.1.2.10 5/
Moves the decimal point position to the left when in Calibration Mode. Selects user selectable formats in the serial and optional BCD menus. The key also enters the digit "5".
8.1.2.11 6 Setpoint
This key is used to enter the Set point Menu Values for standard and optional Relays. Set point Values Deadband Values Preact Values The key also enters the digit "6".
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8.1.2.12 7 Option
This key selects the standard serial ports and available option menus: Rate of Change Analog Transmitter(s) BCD Port Remote I/O PROFIBUS The key also enters the digit "7".
8.1.2.13 8/Cal
This key opens the Calibration set up menu. The key also enters the digit "8".
8.1.2.14 9/
This key moves backward through a menu, step by step and will wrap to the beginning of the menu. Selects user selectable formats in the Serial and optional BCD menus. Pauses the Self-Tests. The key also enters the digit "9".
8.1.2.15 0/Exit
This key Exits a menu/sub-menu back to the normal operating mode when text is on the screen
NOTE: The zero key is used to exit a menu when numbers are entered (See Zero).
The key also enters the digit "0".
8.1.2.16 Enter
When changing numerical values in a sub-menu, this key accepts or rejects the value. When a value is accepted a "GOOD" message will appear on the display and step forward to the next item on the menu. When a value is rejected an "ERR" message will appear on the display, and will display the entered value allowing the user to change the value..
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8.1.3 Dual Spindle Scale Calibration Procedure (Hard Calibration)

NOTE: Hard Calibration is the traditional method of calibration that uses test weights. We recommend that the test weights total 80 to 100% of the scale weight. NOTE: Hard Calibration must be performed with the instrument in GROSS MODE. Selecting the Hard Calibration Sub-Menu Step 1.Make sure that the instrument is in Gross Mode. Step 2.From the Weight Display, Press the 8/Cal button. The Security Code (SEC CD) displays. Step 3.Press the Enter Button. A flashing zero (0) appears. Step 4.Enter the security code number (5321), then press the Enter button. The Unit of Measure UNIT Sub-menu appears. Step 5.Press the down arrow until the CALSub-Menu appears. Step 6.Press the Enter button. The Hard Calibration HD CAL Sub-Menu appears. Step 7.Hard Calibration requires a zero point and the physical placement of test weights on the scale. Step 8.Press the Enter button. The ZERO sub-menu appears.
8.1.4 Setting The Zero Calibration Value

NOTE: At this point the spindle legs need to be raised from the load cell and supported by blocks so that no load is present on the load cells. Place blocks under the rotation motors shown by the blue arrows below. NOTE: On the diagram below looking from the front of the machine the calibration is done first on the front spindle 1 and then on the rear spindle 2. NOTE: Left and right legs on each spindle act as a weight summation to weight the total weight of the perform.
141
Load Cells
Support Blocks Under Rotation Motors Load cells exposed with spindle legs raised and supported by blocks to allow unweighted load cells to be zero calibrated.
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8.1.4.1
To zero the scales
Step 1.Remove all weight "live load" from the scale and place support blocks under the spindle motors to raise the legs sufficiently on both left and right of the spindle legs so a test weight can be placed on the load cells. Step 2.Press the Enter button. A dash "--" appears. Step 3.Press the -/Test/Clr button. A "0" appears. Step 4.Wait 12 seconds. Step 5.Press the Enter button. Step 6.Either a GOOD or ERR# appears. Step 7.If an ERR number appears go to Chapter 8, Troubleshooting in the manufacturers manual for more information. Step 8.If a GOOD appears the Span (SPAN) display appears. NOTE: The resistance baseline for non C2 load cells, is also set when the Zero Calibration Value is entered.
143
8.1.5 Setting The Span Calibration Value
Left Load Cell
Right Load Cell
Test weights on the Load Cell Step 1.Place a certified test weight on each of the load cell scales. Step 2.Press the Enter button. A dash "--" appears. Step 3.Press the -/Test/Clr button. The previous span value appears. Step 4.Press the -/Test/Clr button. A "0" appears. Step 5.Use the numeric keys to enter the value of the test weight. (Example If a 50 lb weight is used, enter 50). NOTE: Ideally the Cumulative test weight used for the dead load should be the typical weight that will be measured in the application using both load cells, example if a 10Kg load is used for each load cell then the span will be 0 to 20 Kg. Step 6.Wait 12 seconds. Step 7.Press the Enter button to set the span. The Linear Correction (LINCOR) Sub-Menu appears. Press the -/Test/Clr button two times. The Return (RETURN) Sub-Menu appears. The Return (RETURN) Display The RETURN Display allows the user to change any setting(s) entered in the Hard Calibration Sub-Menu. Step 1.Push the up arrow which takes you back to the Zero Sub-Menu. Step 2.Press the up arrow until you reach the sub-menu you want to change and press enter. Step 3.Follow the procedures for each Sub-Menu you want to change. Step 4.If you want to accept the Hard Calibration parameters entered, press the Enter button. The End Calibration END CAL message is displayed. Step 5.Press the Enter button. This seals all calibration settings and exits the Hard Calibration Menu. Once you have done the front spindle then repeat the process to do the rear spindle The total weight of the front and rear spindles should be approx 45Kg each
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8.1.6 Checking the Weight of the System.

When the scale reads approximately 45 Kg hit the Tare key on the front panel. Then switch the mode to Net, the scales should read 0 Kg, if it does not hit the Tare button this should zero the scale. Place the test weights that you used in the above calibration on the top of the rotation motors (example if two 5 Kg test weights were used place one 5 Kg test scale on one side of the spindle leg and the other 5 Kg weight on the other spindle leg, the scale should read 10 Kg. If the system does not read the desired weight repeat the calibration procedure.
8.1.7 Tare and Zero the Scale Read Outs.

After the calibration process and in Gross Mode press TARE. The unit will tare the weight of the legs on the scale readout. Put the scales in Net Mode and ensuring there is no load on the spindle legs apart from the legs themselves press Zero, this will Zero the scales. Ensure that before each run you Zero the scales.
8.1.8 Trouble Shooting the Scale Readout.

Please refer the Hardy Manual Trouble Shooting Section.
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9.0 9.1
Spindle Leg Chiller Connection Uncrating and Mechanical Installation
Pull the top cover off the machine. Remove the feet and any other fittings from the fluid basin Do not lose any of the screws Remove the screws from the front panel Remove the front panel
Latch Controller 2 Controller 1
Controller 1 on the left hand side is to set the set point of the temperature in the first closed loop, the set point SP = 45C Controller 2 has the controller which contains the RTD Specification Setting, the dip switch settings and temperature set points of the other closed loop as well as the alarm set points Temp Set Points SP1L = 40C and SP1H = 50C Alarm Set Points A1SP = 50C and A2SP = 35C See next section for details
Flow Regulator
Filter
Ensure that the filter is tightly closed Set the water pressure regulator to 20PSI otherwise you may blow the gaskets in the spindle legs and have water pouring out of them, the pressure regulator is set to max from the factory. With the pressure regulator, turn the machine on, check the pressure, if it exceeds 20 PSI switch the machine off and adjust the regulator down. Switch the machine and check again until you bring the pressure down to approx 20 PSI
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The flow regulator on the front of the panel controls the flow to each of the hose outputs, as hose lengths may be different resistance in the lines may cause uneven flows, this can be regulated to ensure equal flows to the spindle legs.
A: S1L Out B: S1L In C: S1R Out D: S1R In

A B C D
E: S2L Out F: S2L In G: S2R Out H: S2R In

F G H
I: Factory Water Out J: Chilled Factory Water In Pipes do not have to be same length as the flow can be balanced via the front panel
Rear of Machine S1L S1R
Underside Connections of references above. This is because the tubing is crossed over through the E Chains to even weight distribution
S2L Front of Machine
S2R
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9.2
Electrical Installation PDU
Inside PDU
HASKRIS PWR CABLE M C B GROUND
NEUTRAL FUSES
ACTIVE
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9.3
Programming and Temperature Setting Selecting the Sensor Type
9.3.1
Under the Set Setup Menu in section 1-5 Menu Overview select of the programming manual provided by Haskris, the programming page is contained in this section of this manual;
Choose IN1 Sensor Type Selection Select Pt.dn which is the PT100 DIN Curve Refer Page 7 of Manual UM43001A see programming table in this section RTD PT100 DIN STD I/P
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9.3.2
UM4300 Controller Temperature Settings
Using the programming table contained in this section set the following; SP1L = 40C SP1H = 50C Using the programming table contained in this section set the following; Under the User Menu scroll through to A1SP and A2SP set them to the following; ALARM 1 A1SP = 50C ALARM 2 A2SP = 35C On the control panel to the left (See Picture Below) of the Haskris set the set point to 45C SP = 45C
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9.4
Chiller Programming Chart
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10.0 Trouble-Shooting For Deposition & Sintering & Process Activities 10.1 Process Activities 10.1.1 Introduction 10.1.1.1 Ideal Refractive Index Profile
An ideal refractive index profile plot is one with a square index step, as follows,
Deposition of GeCl4 can raise refractive index, thus, theoretically, GeCl4 should have a constant flow rate throughout core deposition in order to obtain the ideal index profile. However, due to diffusion of GeCl4 during drying and sintering, GeCl4 flows need to be controlled and modified in order to tune the profiles as ideal as possible. The fundamental of refractive index profile tuning is by increasing GeCl4 flow when index is low and decrease if too high. There are three stages/modes during a core preform deposition run, that determine the refractive index profile. They are Centerline Mode, Core A Mode and Core B Mode.
10.1.1.2 Various modes in the recipe

A typical ASI core-making recipe includes seven modes in a run. 1. Mandrel Flame Polish Mode Heating up the mandrel with a lame flame for 2 traverse passes. This is to clean off dust particles on the mandrel surface so as to avoid contaminants on the centerline for carbon coating between mandrel and centerline will eventually be burnt off. Note: too high of a mandrel polish flame may damage the mandrel. 2. Carbon Coating Mode Applies carbon coating to the mandrel before depositing soot. The carbon acts as a lubricant when pulling out the mandrel. Therefore, when experiencing difficulties in pulling out the mandrel, increase acetylene flow or the number of carbon coating passes. 3. Carbon Flame Polish Mode A few pass of slow flame polish for removing loose carbon particles and smoothening out the coating surface. 4. Centerline Mode (SiCl4 only) Soot deposition starts by depositing SiCl4 only for the center of the core (Initial soot passes). These centerline passes are one of tools for index profile tuning. The index of the center of the core can be adjusted by controlling the density of the centerline, since, centerline density affect GeCl4 migration to the inside center. See Section B for further explanation. 5. Core A Mode (SiCl4 + GeCl4) After centerline deposition, GeCl4 is added into the SiCl4 streams for the purpose of raising refractive index. Amount of GeCl4 used directly affect the core perform s index profile, thus this is where profile should be tuned. 6. Core B Mode (SiCl4 + GeCl4) Same function as Core A Mode. The reason for breaking core mode into A and B is to give more flexibility of index profile tuning. Note: In ASI core-making recipes, the total amount of SiCl4 + GeCl4 used during both Core A and Core B Mode is always maintained at 40g/min. See section C for details. 7. Clad Mode Oscillation 1 (SiCl4 only) Deposition of core preform over clad. The refractive index of soot deposited during this mode should give an index close to or equals zero. 8. Clad Mode Oscillation 2 (SiCl4 only) Continue deposition of over clad. Dividing cladding process to two different mode 1 and 2 gives more flexibility in tuning, e.g. tuning density and for smoothness.
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10.1.2 Tuning centerline refractive index

In order to avoid problems with closing the hole in the center of the core preform, only SiCl4 is deposited for the initial soot passes (centerline passes). The refractive index of the center of the core preform can be tuned by controlling the density of these centerline passes. During sintering, GeCl4 deposited at Core Mode will diffuse into the centerline; the level of migration is related closely to centerline density. Lower centerline density makes diffusion easier and can raise the refractive index. In a typical recipe, there are about 4-10 passes of centerline passes. Parameters that can be used to tune centerline include speed, SiCl4 flow and number of passes.
10.1.3 Tuning Refractive Index Delta

Though, in theory, constant flow of GeCl4 should be used for producing a square index profile, it needs some tuning in order to get close to sqaure. This is due to Ge migration/diffusion into the centerline and outside to the clad during drying and sintering stages, slopes in profiles indicate migration. Refractive Index Delta plot is mostly determined by deposition of GeCl4, which takes place during Core Mode A and Core Mode B. The purpose of dividing core deposition to two modes is to allow more flexibility in tuning refractive index profiles. GeCl4 and SiCl4 flow according to exponential equations (or linear equation with exponent set to zero) from the recipe. Core Mode A and Core Mode B have their own flow ramping equations. This enables GeCl4 and/or SiCl4 flows to ramp down, up or stay constant in Core A and / or Core B. The divide line between Core A and Core B is based on the number of passes of Core A that is specified in the recipe. ASI s typical recipes switch Core Mode A to Core Mode B at about half-stage of core deposition. Note1: All gas flows, except GeCl4 and SiCl4 flows, have only one ramping equation throughout Core A and Core B mode. Note2: Instructions on how to set ramping equations can be found in recipe command spreadsheet.
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10.1.4 Examples of Index Profiles and Methods of Tuning 10.1.4.1 Profile with a high dip
In tuning profiles similar to this, more GeCl4 can be added at the beginning of Core A Mode, so that, more can diffused into the centerline and brings the centers index up. To lower the peaks, less GeCl4 flow at the end of Core A which is also the beginning of Core B, since the peaks occur at about the middle of core deposition which is close to Core A and Core B transition according to ASI s recipes. As a result, GeCl4 should ramp down during Core A, starts higher and ends lower flow.
10.1.4.2 Delta with slanted slopes
Profiles with slanted slopes can be tuned more squared, by increasing GeCl4 at the end of Core B deposition, which corresponds to the edges of the delta and increases the indexes of the edges. Thus, set a ramping up equation for GeCl4 flows during Core B will be helpful.
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10.1.4.3 Delta Height Adjustment
If the delta is too high or too low, a way to tune is to keep the GeCl4 flow pattern during Core deposition (A&B) and increase or decrease the flows by a percentage similar to the index deviation percentage.
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10.1.5 Changing SiCl4 and GeCl4 flows in the recipe

Note that the total amount of SiCl4 and GeCl4 used during core Mode (Core A Mode and Core B Mode) is always 45g/min (22.5g/min/torch). Therefore, in order to maintain the sum, when increasing GeCl4 flow, SiCl4 flow has to be decreased and vice versa. When the program switches from Core B Mode to Clad Mode, each SiCl4 mfc should have a flow rate of 11.25g/min. For example, If GeCl4 flow has to be increased from 1.8 g/min to 2 g/min per mfc. Before 2 x GeCl4 mfcs = 2 x 1.8 g/min = 3.6 g/min 4 x SiCl4 mfcs = 4 x 10.35 g/min = 41.4g/min Total flow = 3.6 g/min + 41.4 g/min = 45g/min After 2 x GeCl4 mfcs = 2 x 2.0 g/min = 4.0 g/min 4 x SiCl4 mfcs = 4 x 10.25 g/min = 41.0 g/min Total flow = 4.0 g/min + 41.0 g/min = 45g/min
In both Core Mode A and Core Mode B, GeCl4 and SiCl4 flows can be ramped up or down exponentially with initial flow rate, factor and exponent specified in the recipe. In order to maintain a total flow of 45g/min during ramping, SiCl4 ramp exponent should be the same as GeCl4 s, so that the ramp is the same. However, the factor should be 0.5 times of GeCl4s. This is because SiCl4 uses 4 mfcs while GeCl4 has only two and the negative sign is to compensate for increasing / decreasing GeCl4. Below is an example of setting GeCl4 and SiCl4 flow ramp for each mfc.
The third column includes parameters in the order of factor, exponent and initial value. Looking at the first and third rows, which specify GeCl4 and SiCl4 flow ramping equations, the initial values are 2.5 and 9.9, respectively. Multiplying these numbers by the number of mfcs (2.5g/min x 2 + 9.9g/min x 4 = 45g/min). Also note that the factor of SiCl4 is 0.5 times of GeCl4s. For instance, in Core A 0.005 for GeCl4 and 0,0025 for SiCl4 and so as Core B. One has to pick the right factor and exponent so that the chemical flows at the end of one mode match to the initial of the next mode. All the flows and transition time can be estimated by using ASI Flow Analysis spreadsheet
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10.1.6 Oscillations at the Delta

If there are oscillations or noises appear at the delta, they can be related to GeCl4 flows. To avoid GeCl4 flows instability: i) Check if the GeCl4 are functionally correctly with manual torch screen. ii) Make sure all GeCl4 mass flow controllers are zeroed before each run. iii) Check SMR temperature consistency, unstable SMR temperature can cause variation/ oscillations in GeCl4 flows. iii) Make sure the airflow in and out of the machine is normal.
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10.1.7 How To Calculate Core Weight Given a Core/Clad Diameter Ratio
Core/Clad ratio = d/D (after sinter)
Core Weight = volume x density = (d2/4) (L) () Clad Weight = volume x density = (D2/4) (L) ()
Thus, Core Weight/Clad Weight = [(d2/4) (L) ()] / [(D2/4) (L) ()]
=> Core Weight/Clad Weight = d2/ D2 = (Core/Clad ratio) 2
For example, Core/Clad ratio = 0.28 Target core preform weight = 5kg d2/ D2 = Core weight/ (5kg) 2 = 0.282 Core weight = 0.282 x (5) 2 Core weight = 0.392kg
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10.1.8 Measurement Diffraction Type Problem

Sometimes profiles came out to be unreadable. This can happen when the light beam is scanned across the preform, part of the deflection beams escape from the detector, these loss are reflected by the power plots. Dips/Spikes on power plots reveal power losses. Below are two examples on power loss plot:
10.1.8.1 Example 1: Power loss in the center

As shown on the profile below, there is a very high sharp peak at the center. Very likely, this profile is very likely not true at the center and can be verified by looking at the power plot.
From the above power plot on the right, there is a sharp dip at the center, meaning there is a power loss when the beam came through the middle part. Since this loss occurs at the center, it is likely that improper hole closure causes this problem.
10.1.8.2 Example 2: Power loss at the edges
Above is another pair of unreadable profile and its power plot from a high clad density preform. From the power plot, it is obvious from the dips that there are power losses when scanning the edges of a preform. Since the beam hit on one of the edges first and that deflection data was used as reference for the rest of the scan, the whole profile is not accurate.
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10.1.9 How To Do A Manual Density Profile

Density profile is very useful tool in process troubleshooting and preform analysis. Besides using the density data taken from the camera during the process, it is also possible to obtain more precise data by working out a density profile manually. Steps for doing manual density profile: 1) Cut a section, (preferably middle section with less diameter variation) of length L (e.g. 500mm) from the preform.
2) Measure D1, D2 and D3 and weigh the section. Record down all the data 3) Using a blade, slice on the preform surface along the section. 4) Peel out the outer layers. Try to keep the diameter variation along the section as little as possible. 5) Measure D1, D2 and D3 again and weight the preform section again, record the data. 6) Repeat 3-5, the more times these steps are repeated, the more data points for the profile and thus more accurate. 7) Prepare a density calculation spreadsheet similar to the one below:
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The first seven columns are data from the previous steps; Dave is the average of D1, D2 and D3. Volume is the soot volume peeled off, calculated from the formula above. Layer density is density of the layers peeled out. Using the above data as example, the instantaneous density of the soot peeled off the first round is: (68g-54g)/ 17.541cm3) = 0.798 g/cc Soot Volume is the volume is the preform section. Divide this soot volume with soot weight of the preform section will generate average density.
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10.1.10
Troubleshooting Torch Buildup.
Glass can buildup on the surface of the torch, mainly at the tip of chemical tube, causing the SiO2 (+ GeO2) stream to be diverted as shown in the attached figure. Torch buildup, depending on how severe it is, will affect the deposition rate, preform shape and hence affect the soot density, and this may result in the preform cracking. Potential causes for torch buildup include: 1 - Leaks in Chemical Lines Solutions:
Check the chemical fittings, particularly fittings numbered 7 and 8 in the attached figure. Inspect ferrules and the condition of the Teflon tube. Tighten and or replace as necessary.
2 - Inner Shield Absent or Reduced: Solutions:

Check the MFC flows set point and actual. Check the solenoid responsible for operating the inner shield valve. Check nitrogen line pressure.
3 - Silicon Tetrachloride in Chemical Lines: Solutions:

Check the heating tape on the chemical lines. Check the reading of the temperature controllers. Check for cold spots on the chemical lines, particularly at the fittings.
4 - Chemical Tube Dirty: Solutions:

Check if the chemical tube needs deburring. Check for glass buildup within the edge of the tube. Check the condition and age of tube. Clean or replace as necessary.
5 Makeup Oxygen Flow not hot or high enough Solutions: Check if makeup oxygen line is at 112oC, temperature not high enough will be the SiCl4/SiO2 to condensate and build up on the torch. Check if the makeup oxygen flow is delivering the correct flow. Too low of a flow will lower the velocity of the chemical stream and also may not provide sufficient heat for the conversion reaction
163
164
10.1.11
Flow Analysis
In most cases, process engineer needs to estimate or analyze flows of a run with different ramping parameters, especially when estimating flows at the end of each mode and check if those match the initial set point of the next mode. ASI provides customers with a gas flow analysis spreadsheet, ASI Core Recipe Spreadsheet that is very helpful in doing so.
Input all the required parameters on the spreadsheet and it will generate various charts with flow estimation. Note that the items: actual length and average traverse velocity are calculated by the spreadsheet and does not have to be imputed.
165
Charts that estimate all flows during Core deposition
Charts estimating all flows for cladding.
166
10.1.12
Recipe Command Spreadsheet
167
168
169
10.1.13
Sudden Change in Index Profile (delta/shape) Between Preforms
If there is a sudden change in Index Profile (delta/shape) between preforms when using the same recipe, check the following: a) Are the measurements reliable? b) GeCl4 mfcs functioning properly? c) Re-zeroed SiCl4 and GECl4 mfcs before starting the run? d) Air circulation inside deposition chamber the same? Check both exhaust and intake flows. e) In sintering, Chlorine and He mfcs functioning properly? Since, drying process affects GeCl4 migration f) Tip plug are used every time?
10.2 PHYSICAL TUNING / CONTROL 10.2.1 Surface Smoothness (ripples)

If a preform has a rippled surface, certain actions can help smoothening out the surface: 1) Lower traverse speed Lowering traverse speed can reduce ripples on preform surface; however, it will also decrease deposition rate and increase density. 2) Changing total interlace and interlace offset in the recipe A different interlace settings can change the deposition pattern and might help to even out deposition along the preform. Unlike #1 method, this will not have any effect density and deposition rate. Refer to ASI Recipe Commands spreadsheet for definitions on total interlace and interlace offset. 3) Setting a flip-flop function Flip-flop function changes fast and slow traverse direction every number of passes. The purpose is too have a cross and mix pattern on the preform. Using different flip-flop parameters can generate different results.
10.2.2 Density Control

Density control is very crucial in OVD process. Too low of a density can cause soot cracking, or, preform becomes too big for the sintering system. However, too high will limit gas penetration during drying and sintering. The following actions can be taken to increase soot density 1) Lowering traverse speed 2) Increasing heat (Hydrogen) 3) Decrease SiCl4 flow rate 4) Increase makeup oxygen flows but note that too high will cause instability. (Do the opposite for lowering density) The trade-off for increasing density by any of the above actions is the decrease in deposition rate.
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10.2.3 Deposition Rate

Factors which can affect deposition rate includes: 1) Traverse Speed Faster traverse speed can increase deposition rate exponentially during a run but up to a certain point. But as mentioned above, density will be lowered in doing so. The basic reasoning is when density is lowered, preform becomes larger and has a bigger surface area for deposition, so the more surface area, the faster the preform grows. 2) Temperature/ heat (hydrogen flow) Based on Thermophoretic theory, surface with lower temperature favors deposition, so using lower hydrogen and oxygen flows can increase deposition rate. However, at the same time, density will be lowered as well. 3) SiCl4 flow rate Use a higher SiCl4 flow rate can increase deposition rate. 4) Cleanliness of fume tubes After a certain numbers of runs, fume tubes can have some blockage inside from chemical remains. This can affect deposition. Check the clearance and cleanliness of fume tubes and replace them if necessary. 5) Makeup flow rate Increasing makeup flow can increase density but lower deposition rate, since more makeup oxygen produces more heat. 6) Alignment If the system is not aligned properly, soot capture will be different along the preform; some soot will be lost and lowered deposition rate. Alignment includes mandrel centerline to traverse centerline, torch position to mandrel centerline and chuck to V-block alignment. Misalignment can also cause diameter variation and bending. Refer to Section IV, C on how to do rotisserie and torch alignment.
171
10.2.4 Diameter Variation

Mandrels themselves have a diameter variation of about 2mm end to end; deposition on these mandrels thus produces preforms with some diameter variation. Rod draw process includes a diameter controlloop to control diameters of core rods drawn. If preforms have big diameter variation that the rod draw system becomes unable to handle, some actions can be taken to minimize tapering.
Diameter variation happens on soot preform?
Yes a) Check the alignment of core deposition machine. b) Check exhaust flows of deposition machine. c) Check the intake air filters; replace if d) Check condition of the mandrel
dirty.
No (happens after sintering)
a) Lower sintering temperature b) Lower temperature ramping time c) Increase down feed speed.
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10.2.5 Soot Cracking at Handle Interface

Sometimes cracks can be observed at the tip of the handle (mandrel & handle interface). The soot crack appears at a very early stage and may look similar to a fine line or warty fine crack.
It may or may not be heale d/ cover ed up as the depos ition process continues. Therefore, the best is to prevent it from happening at the beginning. Special attention has to be paid to end burner flame hotness and positioning in order to avoid these cracks. Solutions: 1) Lubricate traverse lead screw to reduce vibration. 2) Make sure mandrel set up, including O-rings, plug and chuck are all secure so set mandrel vibration is reduced to the minimal when traverse is oscillating. 3) Set left end burner flow high enough (i.e., showing a little redness) but not too hot to damage the mandrel. Note: If the mandrel becomes too hot, soot may be pulled apart at the interface, forming a gap or crack. 4) Make sure the left end burner is positioned correctly so that handles tip is at the middle of the flame. Moreover, the flame has to hit on the mandrel assembly, not to the front or back of it. 5) Increase half a liter of hydrogen on the left end burner for the first preheat passes.
10.2.6 Splits
Low soot density or insufficient end burner heat or misaligned end burner(s) can cause splits. If the split begins at end burner region (left or right), most likely that end burner flame is not hot enough, increase its hydrogen flow and make sure the flame is heating on the handle/mandrel. If soot cracks due to its low density, one can increase torches heat or slow down traverse speed. For details, see density section B on density control.
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10.2.7 Warts
Warts is basically unreacted SiCl4 deposited on the preform, once it sees heat, it reacts on the surface and forms warts. Warts that appear on the cylindrical preform body tend to be covered by further soot layers and become inclusions. In few cases, the warts grow together with the preform, since unreacted SiCl4 keeps on being deposited and reacted on the same spot. Warts happen at the cone regions (ends) are likely to grow bigger as the run continues. It is because those areas are heated by the end burners constantly, the surface temperature is high and the heat serves as a catalyst for converting unreacted SiCl4 to SiO2 on the surface. The wart is heated continuously and unreacted SiCl4 keeps on reacting at the wart surface, thus, it gets builds up along the run. Solution is to lower makeup oxygen flows, since the makeup streams are regulated at 112C, lowering makeup oxygen can lower heat content that catalyses unreacted SiCl4 to react on the preform surface. This act will decrease density though.
10.2.8 Core/Clad Cracking After Sintering

In some cases, cracking at core and clad interface are observed when preform is being cooled (after/when preform is taking out of the sinter). Make sure that the cooling process is done is a gradual manner, a way to do so is to raise the preform up slowly and hold it at the top of the sintering tube for some time before taking out of the sintering tube. Another possible reason is density mismatch at Core-Clad transition. To verify, one may do a manual density profile. If there is a sharp density change at the transition, tune the process/density with ways described in density control section.
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10.3 FIBER TUNING/CONTROL 10.3.1 Modefield Diameter Out of Specification
Are several reels from one preform failing?
No (one reel) a) Check if fiber measurements are reliable
Yes (multiple reels)
Is MFC from sister core rods failing?
No
a) Check over cladding process: i) Check if correct cladding weight deposited. ii) Check if the core rod is the one as labeled or if it has been switched.
Yes (core problem) a) Check PK2600 measurement and calibration status.
b) Check whether overclad target weight algorithm needs refining. c) Check whether any large within-core preform trends in index delta or shape, and if so, confirm core deposition machine alignment and core sinter flows and temperatures.
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10.3.2 Cutoff Wavelength Out of Specification
Is MFC from sister core rods failing?
No
a) Check over cladding process: i) Check if correct cladding weight deposited. ii) Check if the core rod is the one as labeled. iii) Check if draw tension is correct.
Yes (core problem) a) Check PK2600 measurement and calibration status.
b) Check whether overclad target weight algorithm needs refining. c) Check whether any large within-core preform trends in index delta or shape, and if so, confirm core deposition machine alignment and core sinter flows and temperatures.
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10.3.3 Core/Clad Concentricity
Is CCC from sister core rods failing? .
No
a) Check over cladding and sintering processes: i) if rod assembly straight ii) if cladding machine alignment iii) if He flow too low during sintering iv) if soot density is too low
Yes (core problem)
a) Check rod draw process for alignment straightness.
and
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10.3.4 High Attenuation
Is attenuation of fiber from sister core rod high?
No
a) Check over cladding process: i) Check overclad sinter furnace set up and leaks. ii) Check if the core rod has been cleaned thoroughly before overcladding.
Yes (core problem)
Hold all other sister core rods while troubleshooting.
Symptoms of a water problem exist?
Yes (High 1380nm Attenuation)
Troubleshoot on core sinter process: i) Check if the tube is cracked. ii) Check if there are pipe work leaks. iii) Check if Cl2 and He flows are correct.
No Troubleshoot on all stages of core process for contamination, especially close to center region of the preform.
No (Highest 1310nm Attenuation elevation)
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i) Make sure mandrel is cleaned thoroughly before deposition. ii) Check if carbon coating (acetylene) is sufficient and if the flow is correct. iii) Check if acetylene delivery system is working properly. iv) Check if the center-hole was contaminated before sintering. v) Check core rod cleaning and handling processes. vi) Check if there is any contamination of center-hole after sintering and before hole closure or rod draw.
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10.3.5 Gas Bubbles
Bubbles appear in center region?
No (core region) a) Check if the helium flow is high enough. b) Check for cracks on the sintering tube. c) Check soaking time, temperature and purge flow
Yes
Was mandrel removal difficult?
Yes a) Check mandrel condition. b) Check the carbon coat coverage, was there sufficient acetylene? c) Cool the inside of the mandrel by blowing through Nitrogen before removing mandrel.
No
Was vacuum correct (<1Torr) during rod
Yes a) Check the vacuum (< 1 Torr). b) Check if the tip plug was used. c) Check the piping system for leaks
draw?
a) Check if the drawing temperature and pull force is correct.
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CD2.

01-002 DUAL SPINDLE CORE DEPOSITION SYSTEM

ASI/SILICA MACHINERY, LLC.

CORE DEPOSITION MACHINE CD2.01-002

Safety........................................................................................................................................... 7 Material Safety Data Sheets .................................................................................................. 8

3.0 3.1 4.0

Core Deposition Software .................................................................................................... 85

Scales and Controllers Screen Image Configuration Screen

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

5.2.6 5.2.7 5.2.8

5.2.9 5.2.10 5.2.11 5.2.12 5.2.13

Gas Usage Screen

ASI GeCl4 Vaporizer System............................................................................................. 104

GeCl4 Vaporizer System Controlled Fume Production........................................................111

GeCl4 Vaporizer System Maintenance .....................................................................................113

Method .................................................................................................................................................... 113

6.10.2.1 6.10.2.2 6.10.2.3

ASI/SILICA MACHINERY LLC

6.10.3.1 6.10.3.2 6.10.3.3

Maintenance & Lubrication of Linear Positioning Tables ...................................................117

7.2 7.3 7.4

7.5 7.6 7.7

Dual Spindle Clad Deposition System Maintenance .................................................. 137

ASI/SILICA MACHINERY LLC

Spindle Leg Chiller Connection ....................................................................................... 146

Chiller Programming Chart ..........................................................................................................151

PHYSICAL TUNING / CONTROL .................................................................................................170

ASI/SILICA MACHINERY LLC

FIBER TUNING/CONTROL ...........................................................................................................175

10.3.1 10.3.2 10.3.3 10.3.4 10.3.5

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

Material Safety Data Sheets

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC

CORE DEPOSITION MACHINE CD2.01-002

ASI/SILICA MACHINERY LLC