Surface Treatment For Erosion Resistance: 28 July 2015

Surface Treatment for Erosion Resistance
28 July 2015
By Juthamate Jaruratchataphun
Faculty of Engineering Chulalongkorn University
Star Petroleum Refining Public Co., Ltd.
Objectives of Internship
To study and understand surface treatment application that is
available for industrial use.
To study of a coating application for slurry pumps
To provide recommendation or solution guidance for surface
treatment method for using in hot slurry system.
Contents
Theory of Surface Hardening Methods
Case study on the coating application for slurry
pumps(16G204A/B/C)
Lab Results Summary
Recommendations
Theory of surface hardening methods

Methods for surface hardening
Layer addition
Substrate treatment
Hardfacing
- fusion deposit
- Thermal spray process
Coating
- Electrochemical plating
- PVD
- CVD
- Ion mixing
Diffusion methods
- Carburizing
- Nitriding
- Sulphonitriding
- Nitrocarburizing
- Boriding
- Titanium-Carbon
- Toyota diffusion Process
Selective hardening
methods
- Flame hardening
- Induction
Hardening
- Laser Hardening
- Electron beam
hardening
- Ion Implantation
Layer addition
Hardfacing is the deposition of a special alloy material
on a metallic part, by various welding processes, to

obtain more desirable wear properties and/or
dimensions
Fig1- cross section layer of hardfacing method
Fusion deposits : require melting of the substrate.

Ex. Gas Tungsten Arc Welding, Submerged Arc Welding, Flux Core
Arc Welding
Thermal spray process
Ex. Flame Spraying, Plasma Arc Spraying, High Velocity Oxy Fuel
Layer addition
Weld Hardfacing
Advantages
Inexpensive
Applicable to large components
Localize coating possible
Excellent coating/substrate adhesion
High deposition rate possible
Disadvantages
Residue stresses and distortion can cause serious problems
Weld defects can lead to joints failure
Minimum thickness limit (It is impractical to produce layer less than
2 to 3 mm thick)
Limited number of material available, compare to thermal spraying
Layer addition
Thermal spray
Advantages
Wide selection of spray/substrate materials
Fig 2- thermal spray method
Fast speed of coating formation
Wide range of substrate formation
On-site work possible
Coating can be from when keeping substrate at low temperature
Low environment impact due to dry process
Disadvantages
Thick coats are difficult to achieve
Low degree of adhesion (spray efficiency) on small
substrate/substrate with small curvature
Thermal spray coating does not always indicate the characteristics
of the original material
Layer addition
Coating
Electrochemical plating
Chemical Vapor deposition(CVD)
Physical vapor deposition (PVD)
Ion mixing
Fig 3- electroplating method
Fig 4- PVD and CVD methods
Fig 5 ion mixing method
Substrate Treatment
Diffusion methods
Carburizing
Nitriding
Carbonitriding
Nitrocarburizing
Boriding
Titanium-Carbon
Toyota diffusion process
13
Carburizing
heat treatment process
increases strength and wear resistance by diffusing of carbon into
the surface at temperature condition about 800-950 C
maintaining toughness and strength of the core (work piece : low
carbon alloy steel 0.2-0.3 %C)
Type of carburizing
Gas Carburizing
Vacuum Carburizing
Pack Carburizing
Liquid Carburizing
Fig 7- pack carburizing method
14
Carburizing
2CO C (in austenite) + CO2
(1)
CO C + 1/2O2
(2)
CH4 C (in austenite) + 2H2
(3)
CO + H2 C(in austenite) + H2O
(4)
Equation (1) and (4) are main reactions in Gas Carburizing.

Sometimes, enriched gas technique, addition hydrocarbon gas into
atmosphere, is used.
CH4 + CO2 2CO + 2H2
CH4+ H2O CO +3H2
15
Caburizing
Advantages
Good combination of hard layer and tough core
Good adherence by diffusion
Disadvantages
dimensional deviations by the high temperature process and the
hardening treatment
Selective increase of the angle points; expensive machining
The dimension of the work piece is limited to the size which fits the
hardening furnace.
16
Nitriding
Nitriding is conducted in atmosphere that decomposed
Ammonia to provide Nitrogen into the surface
Low process temperature (Around 500- 550 C)
Fig 8 - before and after Nitriding process structure
17
Types of Nitriding
Gas nitriding
Liquid nitriding
Plasma nitriding
18
Gas Nitriding
Gas Nitriding is a case-hardening process whereby nitrogen is
introduced into the surface of a solid ferrous alloy by holding the
metal at a suitable temperature in contact with a nitrogenous gas,
usually ammonia.
Fig 9 - Gas Nitriding process
19
Liquid nitriding
Nitriding in a molten salt bath employs the temperature range as
gas Nitriding (510-580 C).
fused-salt bath containing either cyanides or cyanates
20
Plasma Nitriding
Apply voltage between batch and furnace wall in gas Nitriding
process.
A glow discharge with a high ionisation level (plasma) is generated
around the parts. Active nitrogen permeates into the surface.
Fig 10 - comparison structures between salt baht, Gas and Plasma Nitriding
21
Sulphonitriding
Surface modification treatment that can be used to treat objects with
complex shapes that are not suitable for salt bath Nitriding.
Effective with regard to changes in dimensions and distortion due to
low process temperature.
Sulphonitride layer improves seizing resistance, galling resistance
and dissolved loss resistance.
Hard Nitride layer contributes to wear resistance.
Fig 11 Sulphonitriding typical structure, plain carbon steel base.
23
Sulphonitriding
Advantages
Improve wear resistant, galling resistant, seize resistant, dissolved loss
resistance.
Less dimension change, distortion due to low temperature.
Can be applied with every contours
Disadvantages
If a part is accidentally overheated the loss of surface hardness is
permanent
Nitride layer is hard but brittle.
24
Boriding
Thermochemical surface hardening process which gives very hard
surface layer (1400-1900 HV in ferrous metal) and case depth
0.0005-0.020 mm.
Boriding process involves the use of specially formulated boronyielding material heated to temperatures between 1300 and
1830F(700-1000 C). Boron atoms diffuse into the substrate,
forming very hard borides within the surface of the material.
Fig 12 - Boriding typical structure of carbon steel base material.
25
Hardness comparing
Fig 16- Range of hardness levels for various materials and surface treatments. EB, electron
beam; HSLA, high strength, low-alloy
Source : ASM Surface Hardening of Steels: Understanding the Basics
30
Case study
The surface treatments for slurry pump(16G204A/B/C)
31
Objective
To study about increasing erosion-corrosion resistance
for slurry pump parts by Multi-nite technique.
32
Factors of Erosion-Corrosion
Erosion - Corrosion
-
Flow rate/ Velocity

Size of particle
Angle of impact
Material/ Hardness
- pH
- Temperature
- Corrosive product
ex. Sulphur
- Material
33
Material
SS410 (CA6NM) Is a hardenable Fe-(11-14%)Cr-(3.5-4.5%)Ni-(0.41%)Mo alloy, martensitic stainless steel. SS410 type has high
corrosion resistance properties. Therefore, main problem of failure
is from Erosion.
Fig 17- Stainless steel 410 round bars
Fig 18 - Stainless steel 410 sheets
34
History of failure
16G204A/B/C are the slurry pumps in A4 (RFCCU). The pumps
made from CA6NM (SS410 mod).
Fluid inside the pump is mainly Heavy hydrocarbon with sulfur 1.76
wt% at operation temperature around 350 C
Fine catalyst, contaminated product which accelerates erosion, size
20- 50 microns, which main compositions are Al2O3 and SiO2 is
increasing in the system. Results in severe erosion on parts of slurry
pumps. The pump service life was about 6 months.
Fig 19- damaged impeller
Fig 20 - damaged volute
Fig 21- damaged casing
35
Why selects Multi-nite ?
Source: khun Findlay
36
Selective method
Surface treatment for increase erosion resistant by multi-nite
technique (Sulphonitriding)
Multi-nite is a thermochemical process to add nitrogen and sulfur
into surface of materials to form compound layer, and hard diffusion
zone layer
Fig 22- Multi-nited impeller
Fig 23- Multinited volute
Fig 24- Multi-nited Casing
37
Erosion
Multinite
pressure
temperature
Diffusion
zone
Hardness
time
material
N2 , NH3 and NM gases
38
Multi-nite Process
Receive
works from
customer
Shipping
to customer
Incoming
inspection
Issue
inspection
report
Issue
HTOS
Hardness
inspection
Vacuum
Washing
Heat
treatment
(Multi-nite)
39
Multi-nite reaction equations

NH3 = 1/2 N2 + 3/2 H2
N2 = [N]
[M] + [N] = MN
2[Cr] +[N] =Cr2N
M: Alloy elements ex. Al, Mo, Fe
= Austenite matrix/phase
Fig 25 - Schematic cross section of nitriding region of an iron-base ferritic

specimen/component showing the compound layer and the diffusion zone with
their (possible) constituents
40
Diffusion of nitrogen
Fig 26 Schematics of phase distribution within a nitrided case on steel and

accompanied nitrogen depth concentration.
41
Assumptions of case study

The higher temperature results in the thicker diffusion zone
nitrogen and sulfur affect to surface hardness of materials. By
forming compound with base material, nitrogen and sulfur make
surface of materials harder.
42
Parameters
Materials: SS410 (CA6-NM)
Process time: Std. time Vs Std.+ minutes
Temperature: 510 and 560 C
testing technique : SEM
Indicated by : thickness of band of diffusion zone
Volume of N2,NH3, NM gases (fixed)

Vacuum Pressure (fixed)
510 C
Std. exposer time
560C
Std. exposer time +
additional time
43
Samples
(a)
(b)
Fig 25
the 1st sample

Non Multinite
Part:
Volute
Material:
SS410
Sample sizing: 1x1x0.5 cm
Testing:
Hardness
SEM JSM-5410LV
EDS
44
Samples
Fig 26 -
the 2nd sample

Multinite at 5100C
Part:
Volute
Material:
SS410
Sample sizing: 1x1x0.5 cm
Testing:
Hardness
SEM JSM-5410LV
EDS
45
Samples
Fig27 -
the 3rd sample

Multinite at 5600C
Part:
Volute
Material:
SS410
Sample sizing:
1x1x0.5 cm
Testing:
Hardness
SEM JSM-5410LV
EDS
46
Steps of testing
Hardness test
Tested sample number 1,2 and 3 by micro vicker hardness testing
machine. collected the hardness of diffusion layer and base material,
present in graph
Hardness VS case depth graph (by vender)
SEM JSM-5410LV
Take the photos of microstructure of sample number 1,2 and 3 for

study the thickness of compound layer, diffusion zone and base
material.
EDX
Use spot analysis techniques to collect elements component of sample

1,2 and 3
47
Results
Microstructures, x100, of the 1st sample (a)
Existing
Coating ?
140 m
Fig 28- inner cross section
Fig 29 intermediate microstructure
inner
outer
Hardness
(HV)
Fig 30 outer cross section
Point 1
Point 2
Point 3
Base
Material
501.74
560.54
597.90
397.62
48
Results
Microstructure, x100, of the 1st sample (b)
Fig 31 inner cross

section
Fig 32- intermediate

microstructure
Fig 33 outer cross section
outer
inner
Hardnes
s (HV)
point1
point2
point3
average
356.48
347.62
361.04
355.05
49
Results
Microstructures, x100, of the 2nd Sample
22 m
24 m
Fig 34-inner cross section
Fig 35- intermediate microstructure
inner
Hardness
(HV)
Fig 36- outer cross section
Point 1
Point 2
Point 3
Base
material
1149.17
1149.17
1149.17
393.93
outer
50
Results
Microstructures, x500, of the 2nd Sample
22 m
24 m
Fig 37 inner cross

section, diffusion zone.
Fig 38 outer cross

section, diffusion zone
51
Nihons lab Result
Fig -Microstructure at surface of 2 nd

Samples batch
Fig- case depth hardness graph of 2 nd samples batch
Compound layer 5.0 m

Diffusion zone 42.5 m
Actual Hardness 1172 HV
52
Results
Microstructures, x100, of the 3rd sample
78 m
75 m
Fig 39- Inner cross section
Fig 40 Intermediate microstructure
inner
outer
Hardness
(HV)
Fig 41- outer cross section
Point 1
Point 2
Point 3
Base
material
1007.15
1007.15
1007.15
322.95
53
Results
Microstructures, x500, of the 3rd sample
78 m
Fig 42 inner cross section,

diffusion zone.
70 m
Fig 43 outer cross section, diffusion

zone.
54
Nihons lab Results
Fig -Microstructure at surface of 3 rd

Samples batch
Fig- case depth hardness graph of 3 rd samples

batch
Compound layer 5.5 m

Diffusion layer 91.9 m
Actual Hardness 1190 HV
55
Results
Hardness Test
1
Diffusion zone
Base material
Load HV 0.3
Point 1
point2
point3
3 points avg
point4
1st sample
510.74
560.54
597.90
556.39
397.62
2nd sample
1149.17
1149.17
1149.17
1149.17
393.93
3rd sample
1007.15
1007.15
1007.15
1007.15
322.95
56
Results
EDX test the 1st sample (a) (base)
Elmt Element%
Atomic%
Si
Cr
Mn
Fe
Ni
Au
Total
100.00
0.83
13.07
0.54
73.44
3.75
8.37
100.00
1.73
14.68
0.58
76.80
3.75
2.48
Fig 45- microstructure of the 1st base material

Fig44: EDX Spot analysis on the 1st samples base material
57
Results
EDX test the 1st sample (a) (grey band)
Elmt Element%
Atomic%
O
Si
Cr
Mn
Fe
Ni
Au
Total
100.00
18.28
1.25
17.97
0.43
48.05
5.49
8.54
100.00
45.03
1.75
13.62
0.31
33.90
3.68
1.71
Fig 47- grey band at inner surface

Fig 46: EDX Spot analysis on the 1st samples grey band
58
Results
EDX 2nd Sample (diffusion zone)
Elmt Element%
Si
Cr
Mn
Fe
Ni
Au
Total
Fig 48: EDX Spot analysis on the 2nd samples diffusion zone
0.83
13.07
0.54
73.44
3.75
8.37
100.00
Atomic%
1.73
14.68
0.58
76.80
3.75
2.48
100.00
Fig 49- diffusion zone at inner surface
59
Results
EDX 2nd Sample (base material)
Elmt Element% Atomic%

Si
Cr
Mn
Fe
Ni
Au
Total
Fig 50: EDX Spot analysis on the 2 samples base material

nd
0.92 1.93
12.45 14.11
0.70 0.75
72.50 76.45
3.91 3.93
9.51 2.84
100.00
100.00
Fig 51- the 2nd base material
60
Results
EDX 3rd Sample (diffusion zone)
Si
Cr
Mn
Fe
Ni
Au
Total
1.34 2.80
17.20 19.38
0.60 0.64
67.69 71.00
3.23 3.22
9.93 2.95
100.00
100.00
Fig 53 diffusion zone at inner surface

Fig 52: EDX Spot analysis on the 3rd samples diffusion zone
61
Results
EDX the 3rd Sample (base material)
Si
Cr
Mn
Fe
Ni
Au
Total
0.73 1.53
12.52 14.17
0.72 0.78
72.85 76.76
4.02 4.03
9.16 2.74
100.00
100.00
Fig 55 the 3rd base material

Fig 54: EDX Spot analysis on the 3rd samples base material
62
Discussions
Sample
Diffusion
thickness
hardness
% hardness
2nd (510C)
23 m
755.24
192%
3rd (560C)
74 m
684.2
212%
Hardness : (hardness of base metal) ( diffusion zones hardness)
Hardness results form laboratory and vender are not exactly

amount, but are in the same trend, because of measuring
techniques.
Maximum hardness at surface for each sample are closely because
it depends on base materials
Temperature at 560 C results in thicker diffusion zone than lower
temperature at 510 C
Labs surface preparing affects to destroyed compound layer. So,
we could not see compound layer form microstructures pictures.
63
Discussion
EDX spot analysis technique might not proper to detect volume of N
due to limitation of Carbon coating is not available in the laboratory.
EDX line scan may be a proper method for detecting the volumes of
elements in diffusion zone.
XRD may be a good alternative to analyze compounds at the
surface for test a result between chromium compound and
hardness.
64
Summary
Mult-nite process improves surface hardness by forming
compounds
at compound layer and diffusion of elements in
diffusion zone.
Multi-nite process improves surface hardness of CA-6NM. At 510
C, hardness increases from 393.93 HV to 1149.17 HV (192%). At
560 C, hardness increase form 322.95 HV to 1007.15 HV
(212%)
Muliti-nite process at 560 C gives thicker case depth and higher
hardness than process at 510 C.
65
Recommendation
Multi-nite process at 560 C is an optimum method for improving
erosion resistance on 16G204A/B/C because this process was
proved that can increase about 3 times hardness at the surface
without distortion problems.
To inspect the pump parts after start running, by follow the previous
interval, to confirm erosion rate and effectiveness of Multi-nite.
66
Reference
https://books.google.co.th/books?
id=1awuxJ5v2ucC&pg=PA290&lpg=PA290&dq=sulphonitriding+disadvantage&source=bl&ots=vF
Alexx8qV&sig=zLrslK8sGqBCvWkde8aImh1iLqg&hl=th&sa=X&ei=huKdVZS4L8TluQTUgKHYDA
&ved=0CCEQ6AEwAA#v=onepage&q=sulphonitriding%20disadvantage&f=false
http://www.testing-engineers.com/coating.pdf
http://www.sepi.esimez.ipn.mx/superficies/assets/archivos/praticalapplications.pdf p3
http://www.metlabheattreat.com/carburizing.html
http://www.slideshare.net/zeeshi1111/carburizing
http://personal.sut.ac.th/heattreatment/context/metal_11.html
http://www.eurotherm.com/industries/heat-treatment/heat-treatment-applications/gas-carburisingfurnace-control/gas-carburising-process
/
http://www.geartechnology.com/issues/0310x/vacuum.pdf
https://www.staff.ncl.ac.uk/s.j.bull/mmm452/gears/sld041.htm
David Pye (2003) Practical Nitriding and Ferritic Nitrocaburizing, 1st edn., United State of
America: ASTM International
http://
www.struers.com/resources/elements/12/101812/Application%20Notes%20Nitrided%20coatings%
20English.pdf
https://www.scribd.com/doc/52320567/55/Advantages-and-disadvantages-of-nitriding
http://www.ibccoatings.com/boriding-boronizing-dhb
http://www.nihon-techno.co.jp/english/mutinite_process_e.htm
http://www.daidodms.co.jp/en/topbox/pdf/PSG_PWG.pdf
http://www.precisioncoatings.com/what-is-thermal-spray.html
67
Thank you
68

Surface Treatment For Erosion Resistance: 28 July 2015

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Surface Treatment For Erosion Resistance: 28 July 2015

Uploaded by

Copyright:

Available Formats

Surface Treatment for Erosion Resistance

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Theory of surface hardening methods

Star Petroleum Refining Public Co., Ltd.

Hardfacing is the deposition of a special alloy material

on a metallic part, by various welding processes, to

Fig1- cross section layer of hardfacing method

Fusion deposits : require melting of the substrate.

Star Petroleum Refining Public Co., Ltd.

Fig 3- electroplating method

Fig 4- PVD and CVD methods

Fig 5 ion mixing method

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Fig 7- pack carburizing method

Star Petroleum Refining Public Co., Ltd.

CH4 C (in austenite) + 2H2

CO + H2 C(in austenite) + H2O

Equation (1) and (4) are main reactions in Gas Carburizing.

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Fig 8 - before and after Nitriding process structure

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Fig 9 - Gas Nitriding process

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Fig 11 Sulphonitriding typical structure, plain carbon steel base.

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Fig 12 - Boriding typical structure of carbon steel base material.

Star Petroleum Refining Public Co., Ltd.

Source : ASM Surface Hardening of Steels: Understanding the Basics

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Flow rate/ Velocity

Star Petroleum Refining Public Co., Ltd.

Fig 17- Stainless steel 410 round bars

Fig 18 - Stainless steel 410 sheets

Star Petroleum Refining Public Co., Ltd.

Fig 19- damaged impeller

Fig 20 - damaged volute

Fig 21- damaged casing

Star Petroleum Refining Public Co., Ltd.

Why selects Multi-nite ?

Source: khun Findlay

Star Petroleum Refining Public Co., Ltd.

Fig 22- Multi-nited impeller

Fig 23- Multinited volute

Fig 24- Multi-nited Casing

Star Petroleum Refining Public Co., Ltd.

N2 , NH3 and NM gases

Star Petroleum Refining Public Co., Ltd.

Star Petroleum Refining Public Co., Ltd.

Multi-nite reaction equations

Fig 25 - Schematic cross section of nitriding region of an iron-base ferritic

Star Petroleum Refining Public Co., Ltd.

Fig 26 Schematics of phase distribution within a nitrided case on steel and