FAST ANODIZING OF ALUMINUM PISTON HEADS by JS. Safrany, Pechiney CRV, Voreppe, France and M. Santarini, ALUMiNlUM Pechiney, Voreppe, France

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1 FAST ANODIZING OF ALUMINUM PISTON HEADS by JS. Safrany, Pechiney CRV, Voreppe, France and M. Santarini, ALUMiNlUM Pechiney, Voreppe, France 8 F- * Abstract Hard anodizing of aluminum piston heads for internal combustion engines Is usually performed by immersion, with a time ranging from 40 to 50 minutes. This paper wiii present a new process, based on specially adapted hydrodynamics of the electrolyte, applying electrolysis parameter values outside the usual range and which greatly reduce the treatment time. In addition to applications to other components, it has been tested with Industrial partners on thermal fatigue test pieces and on pistons, with and without a precombustion chamber.the influence of anodizing parameters (pretreatment, electrolyte temperature, current density, bath composition) will be discussed in relationship with the practical properties of the coating layer such as thickness hardness and thermal fatigue resistance. Introduction Among the 37 million passenger cars and 14 million trucks manufactured in the world in 1994, a substantial part is equipped with diesel engines (23 YO of passenger cars in Europe, 50 Yo in France). The proportion is particularly high with the trucks (80 Yo in France for example). Compared with the gas engine, the piston of the diesel car is submitted to a higher working temperature, between 250 and 350 OC (480 and 660 OF), which is going to become higher, due to the increasing power developed by engines. The aluminum piston, generally in cast alloy AI Si 12 Cu Ni Mg, sustains important sollicitations in terms of thermal fatigue. For many years, the solution to minimize the effect of temperature has been to build a thick oxide layer on the piston head by hardcoat anodizing. Due to the low thermal conductivity of alumina (30 times less than the metal conductivity) this layer acts as a thermal barrier during the piston life. The process described in this paper enables the obtention of such layers with operating times significantly shorther than with classical treatments. Hard anodizing and its limits PrinciDle Hardcoat anodizing, which finds many applications in various industrial fields, provides a thick, abrasionresistant oxide film on the aluminum surface. Compared with standard anodic layers, hard films are obtained in specific conditions : - lower temperature : between 0 and 10 "C(32 to 50 OF) against 20 to 25 "C (70 to 75 OF), - higher current densities : between 2 and 3.5 Ndm2 (19 to 33 Nft2) against 1 to 1.2 Ndm2 (9 to 11 A/ft2), - special electrolytes, usually based on sulfuric acid. However, the growth mechanism of the oxide layer is quite similar to classical anodic films (Figure 1) : - initially, a barrier layer is formed when the current is applied, - an evolution to a porous and hexagonal structure then occurs with competition between the oxide formation by the current and its chemical dissolution by the electrolyte. I I formation of the pores on the barrier laver surface growth of the hexagonal cells initiation of the cells Figure 7 : growth mechanism of a porous oxide layer The oxide structure itself will depend on the operating conditions. In particular, the pore-wall thickness will increase with the voltage. 1

2 In the case of hard anodizing, the low temperature of the electrolyte reduces chemical dissolution of the oxide. Coupled with a strong agitation it removes the heat produced by the electric current in the bottom of the pore (Joule's effect) and allows the use of high current densities. The resulting high voltage involves the formation of a more compact structure, a thicker, harder and more abrasion-resistant layer. Moreover, hard anodizing is less sensitive to alloy composition. The reason is the lower dissolution rate of intermetallic compounds which usually give some porosity in the oxides formed at room temperature. I ~imifs m r d A nodizing The use of high current densities accelerates oxide formation. However, the growth of the film will increase the voltage during the anodizing operation (Figure 2). There are two limits : - the power supply capacity, - the "burning" phenomenon. The latter is due to a local heating in the pore, involving a rapid chemical dissolution of the oxide. The current lines distribution is then completely modified, with, as a consequence, a complete stop of the anodizing process. The control of the agitation plays a major role but, when the geometry and the operating conditons are fixed, there is a limit for the current density and the anodizing time. Concerning the treatment of aluminum piston head, anodic oxidation is usually performed by an immersion of minutes for oxide layers 60 to 90 pm thick. That is why we developed a specific process where the aim was to retain the same properties for the oxide film while significantly reducing the operating time. Description of the process - Characterization of the samples Figure 2 : Voltage vs time for Hard Anodizing time + General orincble The process, as shown in Figure 3, is based on a concentric circulation of the electrolyte on the piston surface, allowing quick removal of the heat produced by the treatment. Electrolyte circulation is performed by a centrifugal pump. The acid is injected through a counter-electrode specially designed for that purpose. The jet strikes perpendicularly the piston head, then is recycled into the tank by a curved-shape baffle. A cooling system is used to maintain the electrolyte at low temperature. This system does not require a piston masking operation prior to anodizing treatment. piston I counter-electrode & 9, I-, AI Figure 3 : fast Anodizing process

3 &- Several sets of samples have been tested on this pilot device : - thermal fatigue test pieces, - pistons with and without a precombustion chamber. (Figure 4) Hardness : microhardness measurements have been performed on cross-sections in order to avoid any influence of the substrate. Micro-indentations were conducted with a KNOOP diamond tool under a load of 10 g during 15 seconds (Figure 5) Operation 4 * diameter = 45mm (1.77 in) Piston 1I3 i \ J \ c anodic film \ chamber Figure 4 : Example of samples Each type of sample needed a specific setting in order to obtain a uniform thickness of the coating, particularly for pistons with a deep combustion chamber. However, each setting can easily be modified simply by changing the counter-electrode configuration. Characterization of the samdles Three properties have been studied : the oxide thickness and hardness and the resistance of the piston to thermal fatigue. Thickness : the oxide thickness has been controlled by Eddy current measurements. However, for non-flat parts of the piston, cross sections have been made followed by Scanning Electron Microscopy observations. It should be pointed out that measurement of voltage versus time allows a good control of the oxide thickness as well as the detection of burning phenomenon. Figure 5 : Micro-indentation with a Knoop diamond tool Thermal fatigue : this property has been controlled by a piston manufacturer, with following conditions for one thermal cycle : - temperature step from 20 to 350 "C (70 to 660 OF) in 15 seconds, - air cooling during 15 seconds, - water cooling during 15 seconds, - air drying during 15 seconds. Trials have been achieved during cycles maximum. Results and discussion Optimization of the process has been performed on thermal fatigue pieces. Initially, the following goals had to be achieved : - minimal thickness of 60 pm, - microhardness of 400 _+ 50 HV 3 271

4 .. eof- When mixed with sulfuric acid, oxalic acid is said to increase film hardness as well as coating abrasion- resistance '. Figure 6 clearly shows the result of an oxalic acid addition to the sulfuric acid solution on on the loss of thickness as a result of abrasive wear ' A 0 / 'IL A / O / x / a./$ A / 100 zoo 300 coo S O ~ Humber of double movements Thicknesr reduction Lrm) x - 170g/l HISO, g/l H,SO, + 5 g/l oxalic acid = 170 gfi H, SO, + 10 g/l oxalic acid 0 = 170 g/l H, SO, + 15 g/1 oxalic acid Number of double movements -- Figure 6 : Thickness reduction as a result of abrasive wear in the abrasive wheel test with coatings produced in sulfuric acid electrolytes (24 OC, 1.5 Ndm2, 20 pm) with and without oxalic acid additions Two types of bath have been tested : - sulfuric acid 180 g/l - sulfuric acid 180 g/l + oxalic acid 15 g/l Figure 7 shows that the oxalic acid gives a significant increase of the oxide microhardness, but is still far from the objective (400 HV). On the other hand, the thickness was quite uniform in both cases (60 to 70 pm). Figure 7 : Micro-hardness of oxide layers obtained in sulfuric acid 180 g/l (A) and sulfuric acid 180 g/l + oxalic acid 15 g/i(b) (temperature c 5 "C, current density 50 Ndm2) Influence of the electrolytic temperature Two temperature conditions were tested :. 1 OC<t<2OC(34"F<t<36OF). 4 C<t<50C(390F<t<41 OF) with a sulfuric-oxalic acid electrolyte at 50 Ndm2. No particular effect has been detected in this range of temperature on the oxide microhardness. Moreover, we had a strong dispersion of experimental values, probably due to the high current density as is explained in the following section. Oxide thickness was correct in both cases (> 60 pm). jnfluence of cu rrent densitv Hard anodizing is usually conducted at constant current density. The oxidation time will depend on the final voltage, fixed here at V. The samples were treated in the following conditions : - electrolyte : sulfuric + oxalic acids - temperature : 2 OC < t < 5 "C(36 OF < t < 41 OF) - current density : between 20 and 50 Ndm2 (between 186 and 465 Nft2) Duration of the anodizing process was calculated to give an oxide thickness of pm. Figure 8 shows that the higher the current density, the lower the microhardness. This can be explained as follows : higher current densities induce more intense heating in the bottom of the oxide pores. 272 A

5 Increased chemical dissolution of the pore walls occurs, leading to a higher overall porosity of the oxide and here resulting to a lower hardness of the coating. The growth of the oxide at higher speed and temperature will probably change its structure as well the oxide layer thickness varies from 60 to 80 pm, - silicon precipitates are included in the oxide, with a mean size of 10 pm, - some micro-cracks are present on the oxide surface but they only affect the external part of the layer. No structural defect has been detected which could prevent the thermal barrier effect of the layer. z n > m 0 C? ; *0? - E current denslty (Aldm2) Figure 8 : microhardness vs current density electrolyte : sulfuric acid ( ) + oxalic acid temperature : - 2 "C c t c 0 "C, oxide mean thickness : pm I Figure 9 : Cross-section of the oxide layer For a lower current density (19 Ndm2-175 A/ft2), a microhardness of 450 HV is reached, fulfilling the objective. ORtimization of the oderatina conditions To make the process profitable, a compromise had to be found between mechanical properties of oxide and anodizing time. That is why we eventually chose to test the thermal fatigue of samples treated with following operating conditions : - electrolyte composition : sulfuric acid (180 g/i) + oxalic acid (1 5 s/) - bath temperature : 2 to 5 "C (28 to 41 OF) - current density : 22 Ndm2 (205 Mt2) - treating time : 6 to 7 min After cycles, no defect was detected on the thermal fatigue pieces. After cycles, cracks depth was not exceeding 2 mm which was acceptable according to our industrial partner. Oxide mecp hology Scanning Electron Microscopy observations of cross-sections (Figure 9) and of the piston head surface (Figure 10) show that : figure 10 : Surface of the oxide layer Trials on pistons Once the process operating conditions had been defined, some pistons have been treated by fast anodizing, then tested by the piston manufacturer in terms of thermal fatigue. Results after cycles are presented in Table

6 ~ ~ Type of treatment Not treated Industrial standard treatment (40 min) Crack length (" Crack depth (") Simplification of the process due to the lack of piston masking, etching and desmutting and reduction of the anodizing time result in a cost reduction for each piston produced. Moreover, if we consider an existing industrial unit, the production capacity can be increased. On the other hand, for a new installation with a fixed capacity, the area occupied by a production unit can be dramatically reduced. PECHINEY treatment (7 min) References 1. Bharat Bhushan, Gupta B.K., Handbook of Tribology, 15-34, Mc Graw-Hill Inc. (1991) Table 1 They clearly show that compared with the classical treatment the fast anodizing process gives a higher crack length while the crack depth is slightly lower. According to the industrial piston manufacturer, these differences were not significant and the overall quality of the coating was good. Conclusion A new fast anodizing process for piston heads has been developed. It has been patented in Europe, USA and Brazil 5-7. In less than 7 min (against min for the classical treatment) the piston can be anodized. The resulting oxide layer properties are as required : microhardness of 400 k 50 HV, thickness greater than 60 pm, thermal fatigue similar to the standard process. 2. Brace A.W. and Sheasby P.G., The Technology of Anodizing Aluminium, 2nd Edition, 129, Technicopy Ltd (1 979) 3. Wernick S. Pinner R. and Sheasby P.G., The Surface Treatment and Finishing of Aluminium and its Alloys, 5th Edition, Vol 1, Gimenez P., Unpublished results 5. Bommier C., Gimenez P., Laslaz G., Pechiney, US Patent no Bommier C., Gimenez P., Laslaz G., Pechiney, European Patent no Bommier C. Gimenez P. Laslaz G., Pechiney, Brasilian Patent

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