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Design and Construction of Laboratory Size Coke Oven

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[Proceedings, 4th Engineering Forum] 14-17 October 2008
DESIGN AND CONSTRUCTION OF LABORATORY SIZE ANODIZING CELL
Egunlae O.O and Kutelu B.J
Mineral Resources Engineering Department, Federal Polytechnic, Ado Ekiti

Abstract
This paper reports the work done on the design, construction and testing of anodizing cell for use as-cast
aluminium profiles against corrosion. The basic features include the pre-treatment baths consisting of
degreasing, pickling, and desmulting units; anodizing cell and post anodizing baths (sealing and colouring
baths) intermittently followed by rinsing baths. The suitable pre-treatment solutions and solvents used include
detergent, NaOH, HNO3, kerosene and distilled water. The pre-treatment baths were made of polyethylene
plastic containers while the anodizing bath was built with Polyvinyl Chloride (PVC). 1MH2SO4 electrolyte was
used, Graphite rod was used as the cathode while the Aluminium to be protected was made the anode. Four
anodizing electrolytes tested include sulphuric acid H2SO4, chromic acid, phosphoric acid and oxalic acid,
show acceptable performance in aluminium anodizing using graphite rods (cathode). The various optimum
working parameters like electrode separation, concentration, voltage, time and temperature were determined.
The machine is cheap and simple to operate with low level of environmental contamination.

Keywords: Anodizing cell, anodizing bath, electrolyte, concentration

Introduction relatively known scientific theories of electrolysis,


The application of aluminium in engineering cannot electrochemistry, and heat and mass transfer and
be underestimated. Anodizing or anodic oxidation chemical reactions.
as applied to metallic surface is the production of a Pre-treatment Operations are the various forms
coating generally of oxide on the surface by of preliminary operations that must be performed to
electrolyte treatment in a suitable solution, the prepare the surface of the metal for proper and
metal being the anode. Aluminium may be adequate coating. (SIRI, 1990; Smithels, 1978;
protected by artificial formation of oxide film on SCT, 2003)
the surface in an electrolytic cell having a suitable Degreasing is a cleaning process, done to remove
acidulated electrolyte; the commonest being is dirt, oil and other foreign materials that might have
sulphuric acid. (Denny, 1982; Duda,1977; Fontana, adhered to the surface of the metal in course of
1986) manufacture, transport and storage. For subsequent
The oxide thus formed will have a depth of 25 to anodizing to be done successfully, one or more of
500 times than which occurs in air. In addition to these cleaning process such as alkaline cleaning.
aluminium and magnesium, titanium and tantalum Pickling is another pre-anodizing process applied
and their alloys are of the most commercially after rinsing. The aluminium metal piece is lowered
important applications of anodizing but a variety of into the pickling baths which contains sodium
other metals can be treated in a similar manner, hydroxide. The purpose of the treatment process is
such include niobium, zirconium, and tungsten. to remove the natural oxide film form on the
(Gabe, 1984; Liucien,1985, Naran, 1999 and Niebel surface of the metal and to remove scratches and
et al, 1993 marks on the metal surface. The maximum
This work entails the designing and fabrication of a operating temperature of the etching bath is 70Oc.
laboratory size-anodizing cell with the pre- Desmulting: The active chemical in this bath is
treatment stages of anodizing. Four selected acids nitric acid. Its purpose is to neutralize the action of
were used as the suitable electrolytes while the sodium hydroxide used in the pickling of the
electrodes used are Aluminium profile anode and aluminium. The operating temperature of the
Graphite rod as Cathode. (Olatuja 1992; o
desmult bath is 27 C. Dilute aqueous solution of
Paunovic,1998; Philiph, 1986; Serope, 1997;
any acid can also be used in removing unwanted
Trenthewey and Chamberlain ,1995) . The
preformed scales on metals and oxides on the metal
designing and fabrication of the cell were carried
out based on some calculations and chemistry of

109
[Proceedings, 4th Engineering Forum] 14-17 October 2008
which cannot be removed in the emulsifying baths QA = qPVC + qacid = MPVCC (T1) + Macid
or pickling. Cacid (T1)
Anodizing Process
Heat given out by the Ice-block = Mice x Cice x
The bath may contain sulphuric acid, oxalic,
chromic or phosphoric. The anodizing bath also change in temperature of Ice = MCT2
consists of a cooling device that reduces the where T1 = (t - x) and T2 = (x + 4)
temperature to 20Oc. (Smithels, 1978; SCT, 2003) Electrolysis of acidulated water
Sulphuric Acid Anodizing Baths At cathode, H + + e- = H
The sulphuric acid process is most widely used for also H + H = H2
decorative and protective anodizing, although it is
not suitable for fabricated or riveted parts, where OH- and SO42- ions move towards the anode. Only
traces of acid retained in interstices after treatment
the OH- loses electrons to the anode and is
may lead to corrosion.
Hot Sealing discharged. SO42- ions remain in solution.
After anodizing and colouring, the porous oxide At anode, OH- - e- = OH
film is perfectly sealed in water or steam to ensure also OH + OH = H2O + O
good corrosion and abrasion resistance of the metal.
Sealing is designed to close the porosity of the and again, O + O = O2
oxide film giving it an optimum chemical inertia. At the anode, the O2 liberated will form oxide on
Hard Anodizing is applied in moving machine one Al to give Al2O3
parts where abrasion resistance is of critical 4Al + 3O2 = 2Al2O3 (oxide film)
importance. Hard anodizing can be obtained by
varying the temperature of the bath, sulphuric acid
Materials
bath temperature ranges between 18Oc and 25Oc As-cast aluminium profiles were gotten from the
but during operation at temperature -5Oc and +5Oc foundry shop of Mechanical Engineering dept,
very hard coating are obtained. This is called low Federal Polytechnic Ado Ekiti. All other materials
temperature anodizing. ( SIRI, 1990) were purchased.
Design parameters
Determination of current and mass deposition of Methods
oxide at anode A. Preparation of samples
Faraday’s first law of electrolysis (i) Cutting the Aluminium bar to specification
m α q where q = Quantity of (30mm x 30mm x 5mm)
electricity in coulombs (ii) Filling
q = It where I = current; t = time. (iii) Polishing: 3 grades of emery paper 320µm,
Current density = Current =I (amps) 400µm, 600µm sizes.
Area of Aluminium Profile A(m2) B. Procedures and conditions for Anodizing
(i) Rinsing in distilled water at 27OC for 1min
Heat calculation
(ii) Cleaning in Kerosene at 27OC for 1min.
Volume of Ice used to cool the bath temperature.
specific heat capacities (iii) Cleaning in Detergent at 50 - 100OC for 1min.
Water = 4200 J/Kgk, Ice = 2100 J/Kgk (iv) Water rinsing at 27OC for 1min
Joule’s law Q = McT (v) Washing in 40g/l NaOH solution at 70OC for
where Q = heat 1min
Heat given out by the ice block bath = heat received
by anodizing bath. (vi) Water rinsing at 27OC for 1min
Heat received by anodizing bath QA = heat (vii) Desmulting 1M HNO3 at 27OC for 1min.
received by PVC(qPVC) + heat by acid qacid (viii) Water rinse at 27OC 1min
(ix) Water rinse 27OC 1min

110
[Proceedings, 4th Engineering Forum] 14-17 October 2008
(x) Weighing of Aluminium Specimen (W1)g anodizing plant for our local aluminium smiting
and smelting industries who produces on small
(xi) Anodizing in 5% H2SO4 at 30OC for 1200sec
scale our house ware and utensils.
to 3600sec Adequate materials preparation should be done that
(xii) Hot water rinsing (sealing) 100OC for 1min is, smooth and clean surfaces of both anode and
(xiii) Drying in air (27OC) cathode as the presence of impurities (MnO2,
(xiv) Reweighing (W2)g and visual examination of NH4Cl) present on the carbon graphite rods (obtain
anodized Al2 from the dry cells) produces toxic fumes of Cl2 gas.
(xv) Determination of weight difference ∆W = Wf -
REFERENCES
Wi
Denny A.J. (1982): Principle and Protection of
corrosion 2nd Ed. Macmillan Pub. Co.
Results and Discussion New York. pp15-53
Figure 1 shows the picture of the laboratory size of Duda W.H. (1977): Aluminium data book Inter-
anodising cell. The weight gained is almost equal in process Engineering in the Chemical
all the three profile used (Table2). The surface Industry, 2nd Ed. MacDonald & Evans,
becomes dull black as bubbles were being formed London pp. 19 – 23
on the two electrodes, the greater weight gain Fontana M.G. (1986): Corrosion Engineering Mc
difference in profile B might have been due to Graw-Hill Inc, New York. Pp. 304-307.
surface scratches. Gabe D.R (1984): Coating and surface treatment
The weight gain increases as the voltage and time for corrosion and wear resistance, (Ed.
increase in Table3 and Table4 respectively. The d.c K.N. Strafford Etal), Chi Chester, Ellis
power supply shows drastic voltage drop at high Horwood. p. 62.
applied voltage (12V). More bubbles were Liucien C. (1985): Fundamentals of metallurgical
produced on the surface of the aluminium specimen processes 2nd Ed. Robert Maxwell, M.C.
(anode) Crenoble University, France. pp 43-56
The bubble continues in all time studied, the table Naran Resources Plc (1999): Technical Study for
shows that there is weight gain increase as the time integration of a new plant into existing
is increased. The presence of Oxygen at the choice plant. NR Plc, USA. pp3-6
of high Voltage 12V. The d.c power source shows Niebel B.W, Draper A.B, Wysk R.A (1993):
that there is drop in voltage across the cell, this Modern Manufacturing Process
might have been due to the increase. Engineering, Mc Graw Hill. pp21-103
The closer the electrode the greater the rate of Olatuja H.F. (1992) Design And Construction Of
reaction (bubble formation) at the anode. The Electrolytic Plant. B.Eng. Thesis, FUT,
presence of Oxygen on the surface was greater at Akure. (Unpublished ) pp2- 49
the shorter distance (150mm). The weight gain Paunovic M. and M. Schlesinger (1998):
decreases as the distance is decreased (Table5). At Fundamentals of Electrochemical
smaller electrode separation the conducting Deposition, Wiley, New York. pp57-98
electrolyte shows lower resistance (Ohm’s law V = Philiph H. Rieger (1986): Electrochemistry
IR) and hence more current can flow to the anode at Prentice Hall New Jersey. pp. 418-410.
the constant voltage. Serope K. (1997): Manufacturing Process for
engineering materials 3rd Ed. Addison
Conclusion and Recommendation Wesley Pub. Co., Great Britain, pp173-
The design and construction of a prototype 177.
laboratory size-anodizing cell has brought closer to Small Industry Research Institute (1990): Modern
the grass root the idea of what really happens in the manufacturing formulas, (Patent) SIRI,
larger anodizing industry. New Delhi, India. pp.34-45
The plant prototype is economically affordable Smithels C.J. (1978) Metal Reference Book, 5th Ed.
efficient and of compact size which application can Butterworth. pp241-367
be of advantage in the setting up of small scale

111
[Proceedings, 4th Engineering Forum] 14-17 October 2008
Surface and Coatings Technology (2003) http://www.sciencedirect.com/science/jou
Proceedings of Frontiers of Surface rnal/02578972
Engineering, Vol.169- Trenthewey K.R. and Chamberlain J. (1995):
170,2June,2003,pp91-95 Corrosion for science and Engineering 2nd
Ed. Longman England. pp1-201

Table 1: Selection of Materials


The selection of all materials depend on the many factors such as the engineering properties, condition
of application, cost and availability of the material.
Part Material Characteristics/Application
Pre treatment bath plastic containers withstand heat.
Heater polymer-coated, 500W to increase bath temperature
electric boilers
Vat Polyvinyl chloride(PVC) Transparent, non-corrosive to acid,
Cathode Graphite rod Conductivity, Insoluble
Anode Aluminium Profile Conductivity, Insoluble
Rinsing Distilled water
Reagents
i Detergent dissolve kerosene from profile surface
ii NaOH cheap, used in large
iii HNO3 aggressive to Al
Solvent Kerosene safe to handle
Electrolyte H2SO4 high conductivity, used in
large scale in industry
Stirrer 12V d.c electric motor low energy agitation
low power consumption
Timing Table clock accuracy
Electrode separation 30cm rule accuracy
Temperature O
100 C thermometer accuracy
Transfer of profile Curtain rail and hooks good conductor
aluminium hangers
Wiring Flexible copper wire good conductor

Test Results

Table 2: Anodizing under optimum anodizing condition


Anodizing time = 20 min, Electrode dist 150 mm, voltage 12V, Current 1Amp, Surface finish = 600 µm, 5%
H2SO4 electrolyte
Profiles A B C
Weight difference 0.09 0.10 0.09

Table3: Voltage variation

Time = 20min, electrode distance = 200mm, current= 1A (1Amp), 5% H2SO4 surface finish 600µm
Voltage Initial weight Final weight Weight difference
6 14.26 14.31 0.05
9 14.41 14.48 0.07
12 14.33 14.44 0.11

112
[Proceedings, 4th Engineering Forum] 14-17 October 2008

Table 4: Time Variation

Voltage 12V, current = 1A, electrode distance 200mm.


Time (min) Weight difference
20 0.05
40 0.09
60 0.16

Table 5: Electrode distance


Voltage 12V, current =1A, 5% H2SO4, time 60min,
Electrode distance Weight difference
150 0.17
200 0.12
250 0.10

Figure 1: Picture of anodising cell constructed

113

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