CN101372731A - Anodized aluminum alloy material having both durability and low polluting property - Google Patents
Anodized aluminum alloy material having both durability and low polluting property Download PDFInfo
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- CN101372731A CN101372731A CNA2008101357595A CN200810135759A CN101372731A CN 101372731 A CN101372731 A CN 101372731A CN A2008101357595 A CNA2008101357595 A CN A2008101357595A CN 200810135759 A CN200810135759 A CN 200810135759A CN 101372731 A CN101372731 A CN 101372731A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
- C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/047—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/05—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
Abstract
The objective of the invention is to provide an anodized aluminum alloy having a long durability and low polluting property even under a high hardness. An anodisation processing aluminum alloy has the following aluminum alloy and an anodic oxide film on the surface of the aluminum alloy. As the alloy contents, the aluminum alloy contains a Mg content between 0.1 and 2.0% (''%'' signifies ''mass %'' herein unless otherwise specified), a Si content between 0.1 and 2.0%, a Mn content between 0.1 and 2.0%, and an Fe, a Cr and a Cu content of 0.03% or below and containing Al and unavoidable impurities as other components. Parts of the anodic oxide film at different positions with respect to thickness of the anodic oxide film have different hardnesses, respectively, and the difference in Vickers hardness between a part having the highest hardness and a part having the lowest hardness is Hv 5 or above.
Description
Technical field
The present invention relates to aluminium alloy, particularly relate to the semi-conductor of CVD device, PVD device, ion implantation apparatus, sputter equipment, dry-etching device etc. and liquid crystal manufacturing installation vacuum chamber member and be located at the employed anodized aluminum alloy of its inner member.
Background technology
Inside at the vacuum chamber of the semi-conductor of CVD device, PVD device, ion implantation apparatus, sputter equipment, dry-etching device etc. and liquid crystal manufacturing installation, be imported into as reactant gases, etching gas, purge gas owing to contain the corrosive gases of halogen, therefore require it erosion resistance (hereinafter referred to as gasproof body corrodibility) to be arranged for corrosive gases.In addition, among above-mentioned vacuum chamber, because the plasma body of halogen system is taken place, so also pay attention to patience (hereinafter referred to as plasma-resistance) (open the 2003-34894 communique with reference to the spy, the spy opens 2004-225113 communique etc.) for plasma body more.In addition in recent years, as the member light weight and the heat conductivity excellence of this vacuum chamber, therefore adopt aluminium and aluminium alloy.
Yet aluminium and aluminium alloy do not have sufficient gasproof body corrodibility and plasma-resistance, and therefore numerous and confused proposition is useful on the surfaction technology that these characteristics are improved., still insufficient for these characteristics, therefore expectation further improves.
In order to improve above-mentioned plasma-resistance, effectively make the anodic oxide coating of the surface formation high rigidity of aluminium and aluminium alloy.Trace it to its cause is because the anodic oxide coating of this high rigidity has patience for the abrasion of the member that the energy of the physical property of plasma body brings, and therefore can improve plasma-resistance (opening 2004-225113 communique etc. with reference to the spy).
Yet, only form high hard adopted anodic oxide coating on the surface of aluminium and aluminium alloy, even anti-plasma can improve, but crackle still takes place on the anodic oxide coating of high rigidity easily.In addition, when connecting anodic oxide coating in case crackle takes place, corrosive gases just can be invaded by the crackle (hereinafter referred to as through check) of this perforation, thereby aluminium and the such problem of corrosion of aluminium alloy as base material take place.
Therefore, just expectation not only has high rigidity, and has the anodic oxide coating of weather resistance (anti-crackle and gasproof body corrodibility).
In addition, from suppressing Fe,, then can form the poor anodic oxide coating of Fe really if reduce the content of the Fe in the aluminium alloy for semiconductor wafer and liquid crystal viewpoint with the pollution of the object being treated of glass substrate etc.But, so further hardening of anodic oxide coating meeting, anti-crackle and gasproof body corrodibility is deterioration more.Therefore, in this field, should guarantee low contaminative, expect the raising of stronger weather resistance (anti-crackle and gasproof body corrodibility) again.
[patent documentation 1] spy opens the 2003-34894 communique
[patent documentation 2] spy opens the 2004-225113 communique
Summary of the invention
The present invention does in view of this situation, and its purpose is, even a kind of high rigidity is provided, still has both durability and the anodized aluminum alloy of low contaminative.
In order to reach above-mentioned purpose, the described invention of claim 1 of the present invention, be a kind ofly to have following aluminium alloy and at the anodic oxidation treatment aluminium alloy of the surperficial formed anodic oxide coating of this aluminium alloy, as alloying constituent, this aluminium alloy contains Mg:0.1～2.0%, and (meaning of " quality % " is descended together.), Si:0.1～2.0%, Mn:0.1～2.0%, each content separate provision of Fe, Cr and Cu is below 0.03%, surplus is made of Al and unavoidable impurities, wherein, have the different position of hardness on the thickness direction of described anodic oxide coating, the difference at the position of the position of hardness maximum and minimum is counted more than 5 with Vickers' hardness.In view of the above, even high rigidity also can realize the anodic oxidation treatment aluminium alloy that weather resistance and low contaminative have both.
The described invention of claim 2 is to have following feature in the described invention of claim 1, and the Vickers' hardness at the position of described hardness minimum is more than 365.In view of the above, plasma-resistance improves.
As above, the present invention a kind ofly has following aluminium alloy and at the anodic oxidation treatment aluminium alloy of the surperficial formed anodic oxide coating of this aluminium alloy, as alloying constituent, this aluminium alloy contain Mg:0.1～2.0% (meaning of " quality % ", down with.), Si:0.1～2.0%, Mn:0.1～2.0%, each content separate provision of Fe, Cr and Cu is below 0.03%, surplus is made of Al and unavoidable impurities, because on the thickness direction of described anodic oxide coating, have the different position of hardness, the difference at the position of the position of hardness maximum and minimum is counted more than 5 with Vickers' hardness, even, still have both durability and the anodic oxidation treatment aluminium alloy of low contaminative so can provide to high rigidity.
Embodiment
Below, just illustrated embodiment limit, limit of the present invention is described in detail.
(formation of the anodized aluminum alloy that weather resistance of the present invention and low contaminative have both)
The anodic oxidation treatment aluminium alloy that weather resistance of the present invention and low contaminative have both, be to have following aluminium alloy and at the anodic oxidation treatment aluminium alloy of the surperficial formed anodic oxide coating of this aluminium alloy, as alloying constituent, this aluminium alloy contains Mg:0.1～2.0%, and (meaning of " quality % " is descended together.), Si:0.1～2.0%, Mn:0.1～2.0%, each content separate provision of Fe, Cr and Cu is below 0.03%, surplus is made of Al and unavoidable impurities, wherein, have the different position of hardness on the thickness direction of described anodic oxide coating, the difference at the position of the position of hardness maximum and minimum is counted more than 5 with Vickers' hardness.In view of the above, even can provide to high rigidity, still have both durability and the anodic oxidation treatment aluminium alloy of low contaminative.
Below, describe in detail for the reason that reaches above-mentioned formation.
Present inventors at first suppress Fe, the Cr in the aluminium alloy, the content of Cu, make it can not pollute the object being treated of semi-conductor etc.Particularly apply flexibly the anodic oxide coating hardening that makes generation by the content that suppresses Fe on one side energetically, thereby can guarantee this characteristic of plasma-resistance, study with keen determination just in case on the anodic oxide coating crackle takes place on one side, how not only this crackle is stretched over aluminium alloy itself.It found that, by preparing the formation condition of anodic oxide coating, make on the thickness direction of anodic oxide coating to have the different position of hardness, the difference at the position of hardness maximum and minimum position is counted more than 5 with Vickers' hardness, can make crackle can not be stretched over aluminium alloy itself.In view of the above, gas also is inhibited to the intrusion of aluminium alloy itself, and comprehensive weather resistance is guaranteed.Mention reason, become such structure and can to solve the detailed mechanism of above-mentioned problem still indeterminate.But,, think that the result is that crackle can not extend to aluminium alloy itself because the stretching, extension of crackle is absorbed by the little position of hardness or suppresses as one of mechanism.
The present invention below is described in detail in detail.
(composition in the aluminium alloy)
Be present in Mg, Si and Mn in the aluminium alloy, be combined into Mg
2Si, also have Al-Mn-Si compound or Al-Mn compound, though at length mechanism is not clear, supposition can make anodic oxide coating strengthen.
·Mg：0.1～2.0％
Mg forms Mg
2The needed element of Si compound is lower than at 0.1% o'clock, can form Mg hardly
2The Si compound, the weather resistance that therefore can not get the anodic oxide coating expectation improves effect.On the other hand, when surpassing 2.0%, Mg
2Thickization of Si compound hinders the formation of normal anodic oxide coating on the contrary.Therefore, the following of the content of Mg is limited to 0.1%, is limited to 2.0% on it.Be preferably 0.8%.
·Si：0.1～2.0％
Si and Mg form Mg
2The needed element of Si compound is lower than at 0.1% o'clock, can form Mg hardly
2The Si compound, the weather resistance that therefore can not get the anodic oxide coating expectation improves effect.On the other hand, when surpassing 2.0%, Mg
2Thickization of Si compound hinders the formation of normal anodic oxide coating on the contrary.Therefore, the following of the content of Si is limited to 0.1%, is limited to 2.0% on it.Be preferably 1.2%.
·Mn：0.1～2.0％
Mn forms Al-Mn-Si compound or the needed element of Al-Mn compound, is lower than at 0.1% o'clock, can form these compounds hardly, and the weather resistance that therefore can not get the anodic oxide coating expectation improves effect.On the other hand, when surpassing 2.0%, thickization of above-claimed cpd hinders the formation of normal anodic oxide coating on the contrary.Therefore, the following of the content of Mn is limited to 0.1%, is limited to 2.0% on it.Be preferably 1.6%.
Fe, Cr and Cu: respectively below 0.03%
Employed in the anodic oxidation treatment, be used to the ionization of aluminium and take place, therefore, become big if be used for the ratio of the electricity that oxygen takes place based on the electrolytic oxygen of water, the ratio that then is used for the Ionized electricity of aluminium alloy diminishes, and the efficient of the formation of oxidized aluminum alloy thing reduces and slows down film forming speed.If Fe, Cr, Cu are present in the aluminium alloy, then these elements become the starting point that oxygen takes place, and the ratio that causes being used for the electricity that oxygen takes place becomes big, and film forming speed is slack-off.In addition.If the content of Fe, Cr, Cu surpasses 0.03% respectively, then to gas, discharge from mother metal and anodic oxide coating, thus the object being treated of pollution semi-conductor etc.Therefore, each content of Fe, Cr and Cu is respectively below 0.03%, and preferred separate provision is below 0.01%.
Surplus Al and unavoidable impurities
Surplus has only Al in fact, but also allows the containing on a small quantity inevitably of impurity element of Ni, Zn, B, Ca, Na, K etc. beyond Fe, Cr, the Cu.But in order to realize lower pollutionization, preferably the summation with the impurity element (unavoidable impurities) beyond Fe, Cr, the Cu is defined in below 0.1%.
In addition, if the crystal grain of aluminium alloy is big, then manifest the crystallization grain pattern on anodic oxide coating, the tone heterogeneity that becomes therefore for it is prevented, also can contain Ti.Also have, if the content of Ti is very few, then can not get the control effect of crystal grain, if content is too much, then become the reason of pollution on the contrary, therefore Ti is contained sometimes, preferably be limited to 0.01% under it, more preferably 0.015%, preferably be limited to 0.03% on it, more preferably 0.025%.
(manufacture method of aluminium alloy)
Next, the manufacture method for aluminium alloy describes.
At first, suitable selection is Continuous casting process, semicontinuous casting method common fusion castings such as (DC castings) for example, makes the aluminium alloy cast ingot of adjusting in the mentioned component scope.Secondly, to the thermal treatment (also claiming " all thermal treatment ") of implementing to homogenize of this aluminium alloy cast ingot.This homogenization temperature (also claiming " treatment temp homogenizes " or " all thermal treatment temps ") is to carry out equal thermal treatment with the temperature more than 500 ℃, thereby obtain the anodic oxide coating of excellent in te pins of durability.But if implement to homogenize processing with the temperature that surpasses 600 ℃, then scaling loss generations such as (burning) has the situation that surface texture etc. goes wrong of causing.Therefore, the treatment temp that homogenizes is recommended as (more preferably above 550 ℃), the scope below 600 ℃ more than 500 ℃.Though how to concern the formation of the anodic oxide coating of high-durability about so equal thermal treatment temp do not distinguish as yet, as above-mentioned, think relevant with the formation of Al-Mn-Si compound or Al-Mn compound.
Then, the aluminium alloy cast ingot of having handled having implemented to homogenize such as is rolled, forges, extrudes at suitable plastic working, the aluminium alloy that obtains is thus carried out solution treatment, quenching, artificial aging handle (following only be called " ageing treatment ".) after, be machined into suitable shape, thereby make the base material of aluminium alloy.Perhaps, also above-mentioned aluminium alloy can be shaped be processed into the shape of regulation after, implement solution treatment, quenching, ageing treatment again, make the base material of aluminium alloy thus.As solution treatment, quenching, ageing treatment, for example can carry out 515～550 ℃ of solution treatment, water quenching, 170 ℃ * 8h of ageing treatment, 155～165 ℃ * 18h as common T6 processing.
(about anodic oxide coating)
Secondly, the surperficial formed anodic oxide coating for above-mentioned aluminium alloy base plate describes.As anodic scale formation method, it needs only suitable the selection and carries out electrolytic condition, and promptly the condition of the composition of electrolytic solution, concentration, electrolytic condition (voltage, current density, current-voltage waveform, temperature) etc. gets final product.About anode oxidation treatment liquid, need carry out electrolysis with the solution that contains the element more than a kind among C, S, N, P, the B, for example, use that to contain oxalic acid, formic acid, thionamic acid, phosphoric acid, phosphorous acid, boric acid, nitric acid or its compound, phthalandione or its compound aqueous solution more than a kind in this be effective.The thickness of anodic oxide coating is not particularly limited, but to be advisable about 0.1～200 μ m, is preferably about 0.5～70 μ m, more preferably about 1～50 μ m.
As described above, because have the different position of hardness on the thickness direction of anodic oxide coating, the difference at the position of the position of this hardness maximum and minimum is counted more than 5 with Vickers' hardness, so even this epithelium is a high rigidity, still can suppress the propagation of crackle, anti-crackle excellence.So, because anti-crackle is suppressed, so as a result of, gas also is suppressed to the intrusion of aluminium alloy itself, and weather resistance obtains guaranteeing comprehensively.With respect to this, the difference at the position of the position of hardness maximum and minimum is lower than at 5 o'clock with Vickers hardness tester, on the thickness direction of anodic oxide coating, can demonstrate the identical movement of situation with hardness homogeneous (equally) in fact, the propagation of crackle is difficult to be inhibited, and anti-crackle is bad.Therefore, gasproof body corrodibility is also poor.
In the present invention, the quantity at the position that hardness is different on the thickness direction of anodic oxide coating needs more than 2, but if more than 2, then the quantity at this position is not particularly limited.In addition, on the thickness direction of anodic oxide coating, hardness can change intermittently, perhaps also (obliquely) variation continuously.
In addition, from being suppressed at this viewpoint of propagation of the crackle that anodic oxide coating takes place, the Vickers' hardness at the position of consideration hardness minimum is advisable with as far as possible little aspect, but, if the abrasive patience that the physical energy for plasma body causes is also taken into account, is then preferably counted more than 365 with Vickers' hardness.
The aluminium alloy (hereinafter referred to as the anodic oxidation treatment aluminium alloy) that is applied with this anodic oxide coating is adapted at the various uses of use under the pyritous corrosive environment.Particularly be suitable as under hot environment and be exposed in etchant gas and the plasma body, require one side appended employed vacuum chamber of plasma processing apparatus that adds setting such as the semiconductor manufacturing facility of low pollutionizations of object being treated and the member of being located at its inner electrode etc.
In order on the thickness direction of anodic oxide coating, to make the changes in hardness of anodic oxide coating, employing intermittently or continuously makes the method for the temperature variation of anode oxidation treatment liquid in the way of anodic oxidation treatment, interrupt anodic oxidation treatment on the way, from anode oxidation treatment liquid, take out object being treated quickly, the method etc. of recovering anodic oxidation treatment in the anode oxidation treatment liquid that other liquid is formed and/or temperature is different gets final product, according to these methods, can make the changes in hardness of the thickness direction of anodic oxide coating.In addition, the side that the temperature of anode oxidation treatment liquid is low, the chemical dissolution of the anodic oxide coating in the anodic oxidation treatment is suppressed and hardening.
In addition as described above, consider processed pollution to semi-conductor etc., for example be suppressed at below 0.03% as if content with the Fe in the aluminium alloy, then the content of the Fe in the anodic oxide coating is suppressed in below the 500ppm, in addition, if just the content of the Fe in the aluminium alloy is suppressed at below 0.01%, then the content of the Fe in the anodic oxide coating is suppressed in below the 150ppm.
As described above, even above-mentioned anodic oxidation treatment aluminium alloy is a high rigidity, also can satisfy weather resistance (anti-crackle and gasproof body corrodibility) and low contaminative.
[embodiment]
Below, elaborate the present invention based on embodiment.But following embodiment does not limit the present invention, changes all being included in the technical scope of the present invention of enforcement in the scope that does not break away from the forward and backward aim of stating.
At first, melting has the described { embodiment (test portion No.1,2,4,5) of following table 1, comparative example (test portion No.3,6～14) } become the aluminium alloy cast ingot (size: wide 220mm * long 250mm * thick 100mm be grouped into, speed of cooling: 15～10 ℃/s), cut off this ingot casting and carry out face milling (size: wide 220mm * long 150mm * thick 60mm), implement equal thermal treatment (540 ℃ * 4h).All after the thermal treatment, former material 60mm is thick by hot rolling is rolled into the thick sheet material of 6mm, carry out solution treatment (510～520 ℃ * 30min) after, carry out shrend and fight and implement (160～180 ℃ * 8h), obtain of ageing treatment for the examination alloy sheets.From this alloy sheets cut 25mm * 35mm (rolling direction) thick * test film of 3mm, face milling is carried out on its surface processes surfaceness into Ra1.6.
Secondly, above-mentioned each test film is flooded 2 minutes after washings in 60 ℃-10% NaOH aqueous solution, again at 30 ℃-20% HNO
3Dipping by the treatment and purification surface of washing, is implemented anodic oxidation treatment by the order of the 1st layer (aluminum alloy base material side), the 2nd layer (layer that forms again on the 1st layer) after 2 minutes afterwards in the aqueous solution.As the condition of anodizing, as described in above-mentioned table 1, layers 1 and 2 all is that treatment solution is 25g/L (is the meaning that rises at this " L ") oxalic acid, and electrolysis voltage is fixed as 60V, and the thickness that makes the anodic oxide coating of formation is 15 μ m.As the condition of the anodic oxidation treatment of layers 1 and 2, different is the temperature of above-mentioned treatment solution, and a side of the 1st layer of temperature when forming is than the 2nd layer of temperature height when the formation.
Anodic oxidation treatment aluminium alloy test portion sheet (the following test portion sheet that only is called) for as above making like this carries out Fe, the Cr in the anodic oxide coating, the Determination on content of Cu, the mensuration of the hardness of anodic oxide coating, the test of the weather resistance of anodic oxide coating.
(Determination on content of the Fe in the anodic oxide coating, Cr, Cu)
In order to estimate the stain resistance of test portion sheet, (at this " mL " is the meaning of milliliter to make anodic oxide coating be dissolved in 7% hydrochloric acid 100mL under the degree of not exposing aluminium alloy base plate.) in, calculate the meltage W (g) of anodic oxide coating according to the changes in weight of the hydrochloric acid before and after the dissolving.Secondly, this hydrochloric acid soln is carried out icp analysis, try to achieve Fe, the Cr in the hydrochloric acid, each concentration of Cu, calculate and be dissolved in Fe, the Cr in the 100mL hydrochloric acid, each weight W of Cu
Fe, W
Cr, W
Cu(g), according to W
Fe/ W, W
Cr/ W, W
Cu/ W tries to achieve Fe, Cr, each concentration of Cu in the anodic oxide coating.Then, with the concentration of the Fe in the anodic oxide coating, Cr, Cu, according to following benchmark evaluation stain resistance (evaluation result is presented in the above-mentioned table 1).
The stain resistance metewand
◎: whole elements is all below 300ppm, and zero: at least a kind of element surpasses 300ppm below 500ppm, other elements below 300ppm, *: at least a kind of element surpasses 500ppm
The stain resistance evaluation result
Shown in above-mentioned table 1, comparative example (test portion No.12～14), though the content of any one element in the anodic oxide coating surpasses 500ppm, embodiment (test portion No.1,2,4,5) and comparative example (test portion No.3,6～11) are all good results below 500ppm of whole elements.In addition, embodiment (test portion No.1,2) and comparative example (test portion No.3,6～11) are shown in above-mentioned table 1, and the content that is the whole element in the anodic oxide coating is the following fabulous result of 300ppm.
(mensuration of the hardness of anodic oxide coating)
Along cross-wise direction (making anodic oxide coating cross section and aluminum alloy base material cross section become abrasive surface) the test portion sheet is imbedded resin, after grinding, press the method for JIS Z2244 (1998) for the anodic oxide coating cross section and measure hardness.
Measurement result
Shown in above-mentioned table 1, embodiment (test portion No.1,2,4,5) and comparative example (test portion No.3,6～14) all are that the 2nd layer the hardness of the anodic oxide coating of a side than the 1st layer of hardness of anodic oxide coating is hard.This be because, the temperature of the treatment solution the during shaping of the anodic oxide coating of temperature than the 1st layer of the treatment solution of the 2nd layer anodic oxide coating when forming is low.In addition, the hardness of the anodic oxide coating of the 2nd layer of embodiment (test portion No.2) and the 1st layer poor counts 5 with Vickers' hardness.This anodic oxide coating temperature when forming that is based on the 2nd layer is 5 ℃, and the temperature of the treatment solution of the 1st layer anodic oxide coating when forming is 8 ℃.In addition, the hardness of the anodic oxide coating of the 2nd layer of embodiment (test portion No.3) and the 1st layer poor counts 4 with Vickers' hardness.This anodic oxide coating temperature when forming that is based on the 2nd layer is 5 ℃, and the temperature of the treatment solution of the 1st layer anodic oxide coating when forming is 7 ℃.The hardness of the anodic oxide coating of embodiment (test portion No.1,4,5) beyond these and comparative example (test portion No.6～14) the 2nd layer and the 1st layer poor counts 10 with Vickers' hardness.This anodic oxide coating temperature when forming that is based on the 2nd layer is 5 ℃, and the temperature of the treatment solution of the 1st layer anodic oxide coating when forming is 10 ℃.So, by the temperature of the treatment solution of control anodic oxide coating when forming, can set the hardness of anodic oxide coating arbitrarily.In addition, the hardness of above-mentioned anodic oxide coating is removed comparative example (test portion No.12) shown in above-mentioned table 1, is more than 365 with Vickers hardness tester, therefore except that comparative example (test portion No.12), all can guarantee plasma-resistance.
(test of the weather resistance of anodic oxide coating)
The test of weather resistance was made of 2 stages of following this anti-crackle test and gasproof body corrosion test.At first, at first the test portion sheet is arranged on (atmosphere is in the atmosphere) in the test chamber, is heated to 450 ℃ and kept 1 hour, from test chamber, take out the test portion sheet thereafter, be immersed in chilling (anti-crackle test) in 27 ℃ the water.After this test, the test portion sheet is rested on 5% Cl
2After (400 ℃) 4 hours (as 1 cycle), append a cycle again under the-Ar gas atmosphere, implement to add up to 2 cycles (gasproof body corrosion test).Afterwards, take out the test portion sheet, calculate the corrosion generation area occupation ratio (corroded area/test portion sheet area * 100) on test portion sheet surface, estimate (evaluation result is presented in the above-mentioned table 1) according to following benchmark.
The durability evaluation benchmark
◎: area occupation ratio 0%, zero takes place in corrosion: corrosion take place area occupation ratio surpass 9%, below 3%, *: area occupation ratio takes place and surpasses 3% in corrosion
Durability evaluation result
Shown in above-mentioned table 1, though comparative example (test portion No.3,6～11) is defective, embodiment (test portion No.1,2,4,5) and comparative example (test portion No.12～14) are good result.In addition, embodiment (test portion No.1) and comparative example (test portion No.12～14) are extremely good results shown in above-mentioned table 1.
As above, if Fe, Cr in the comprehensive judgement anodic oxide coating, the Determination on content result of Cu, the test-results of the measurement result of the hardness of anodic oxide coating and the weather resistance of anodic oxide coating, that then can satisfy whole benchmark has only embodiment (test portion No.1,2,4,5).The embodiment (test portion No.1,2,4,5) that satisfies whole benchmark still has both durability and low contaminative even be high rigidity.
Claims (2)
1. one kind has both durability and the anodized aluminum alloy of low contaminative, it is characterized in that, be to have the aluminium alloy of following formation and the anodic oxidation treatment aluminium alloy of the anodic oxide coating that forms on the surface of this aluminium alloy, this aluminium alloy contains Mg:0.1～2.0% as alloying constituent in quality %, Si:0.1～2.0%, Mn:0.1～2.0%, Fe, each content of Cr and Cu is each defined in below 0.03%, surplus is made of A1 and unavoidable impurities, wherein, have the different position of hardness on the thickness direction of described anodic oxide coating, the difference at the position of the position of hardness maximum and minimum is counted more than 5 with Vickers' hardness.
2. anodized aluminum alloy according to claim 1 is characterized in that, the Vickers' hardness at the position of described hardness minimum is more than 365.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007216239A JP5064935B2 (en) | 2007-08-22 | 2007-08-22 | Anodized aluminum alloy that combines durability and low contamination |
| JP2007216239 | 2007-08-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101372731A true CN101372731A (en) | 2009-02-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CNA2008101357595A Pending CN101372731A (en) | 2007-08-22 | 2008-07-11 | Anodized aluminum alloy material having both durability and low polluting property |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US20090050485A1 (en) |
| JP (1) | JP5064935B2 (en) |
| KR (1) | KR20090020496A (en) |
| CN (1) | CN101372731A (en) |
| DE (1) | DE102008037271A1 (en) |
| SG (1) | SG150438A1 (en) |
| TW (1) | TW200914627A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420555A (en) * | 2015-11-11 | 2016-03-23 | 苏州三基铸造装备股份有限公司 | Cast aluminum alloy capable of being anodized and preparation method thereof |
| CN110402296B (en) * | 2017-03-10 | 2021-04-20 | 伊苏瓦尔肯联铝业 | High temperature stable aluminum alloy vacuum chamber element |
| CN115698355A (en) * | 2020-06-10 | 2023-02-03 | 爱励轧制产品德国有限责任公司 | Method for manufacturing aluminum alloy sheet for vacuum chamber member |
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| JP4168066B2 (en) | 2006-08-11 | 2008-10-22 | 株式会社神戸製鋼所 | Aluminum alloy for anodizing treatment used in plasma processing apparatus and manufacturing method thereof, aluminum alloy member having anodized film, and plasma processing apparatus |
| KR101657722B1 (en) * | 2008-07-30 | 2016-09-19 | 고쿠리츠 다이가쿠 호진 도호쿠 다이가쿠 | Al ALLOY MEMBER, ELECTRONIC DEVICE MANUFACTURING DEVICE, AND MANUFACTURING METHOD FOR Al ALLOY MEMBER WITH ANODIC OXIDE FILM |
| JP5284740B2 (en) * | 2008-09-25 | 2013-09-11 | 株式会社神戸製鋼所 | Method for forming anodized film and aluminum alloy member using the same |
| FR2955336B1 (en) | 2010-01-20 | 2013-02-15 | Alcan Rhenalu | PROCESS FOR MANUFACTURING 6XXX ALLOY PRODUCTS FOR VACUUM CHAMBER |
| WO2012148370A1 (en) * | 2011-04-27 | 2012-11-01 | Axcelis Technologies, Inc. | Substantially non-oxidizing plasma treatment devices and processes |
| JP5648660B2 (en) * | 2012-09-10 | 2015-01-07 | 株式会社デンソー | Method of anodizing aluminum |
| FR2996857B1 (en) | 2012-10-17 | 2015-02-27 | Constellium France | ELEMENTS OF ALUMINUM ALLOY VACUUM CHAMBERS |
| US9850591B2 (en) | 2013-03-14 | 2017-12-26 | Applied Materials, Inc. | High purity aluminum top coat on substrate |
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| US9869030B2 (en) | 2014-08-29 | 2018-01-16 | Apple Inc. | Process to mitigate spallation of anodic oxide coatings from high strength substrate alloys |
| EP3042983A1 (en) * | 2015-01-09 | 2016-07-13 | Apple Inc. | Processes to reduce interfacial enrichment of alloying elements under anodic oxide films and improve anodized appearance of heat treatable alloys |
| WO2016111693A1 (en) | 2015-01-09 | 2016-07-14 | Apple Inc. | Processes to reduce interfacial enrichment of alloying elements under anodic oxide films and improve anodized appearance of heat treatable alloys |
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| US10174436B2 (en) | 2016-04-06 | 2019-01-08 | Apple Inc. | Process for enhanced corrosion protection of anodized aluminum |
| US11352708B2 (en) | 2016-08-10 | 2022-06-07 | Apple Inc. | Colored multilayer oxide coatings |
| US11242614B2 (en) | 2017-02-17 | 2022-02-08 | Apple Inc. | Oxide coatings for providing corrosion resistance on parts with edges and convex features |
| US11549191B2 (en) | 2018-09-10 | 2023-01-10 | Apple Inc. | Corrosion resistance for anodized parts having convex surface features |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5431802A (en) * | 1985-05-10 | 1995-07-11 | Showa Aluminum Corporation | Cylinder tube and process for producing same |
| JPH06330386A (en) * | 1993-05-20 | 1994-11-29 | Fujikura Ltd | Formation of hard anodic oxide film and aluminum alloy for forming the film |
| US5775892A (en) * | 1995-03-24 | 1998-07-07 | Honda Giken Kogyo Kabushiki Kaisha | Process for anodizing aluminum materials and application members thereof |
| DE59704202D1 (en) * | 1996-04-03 | 2001-09-06 | Alusuisse Tech & Man Ag | COATING SUBSTRATE |
| JP4194143B2 (en) * | 1998-10-09 | 2008-12-10 | 株式会社神戸製鋼所 | Aluminum alloy material with excellent gas and plasma corrosion resistance |
| JP2003034894A (en) | 2001-07-25 | 2003-02-07 | Kobe Steel Ltd | Al ALLOY MEMBER SUPERIOR IN CORROSION RESISTANCE |
| JP2004225113A (en) | 2003-01-23 | 2004-08-12 | Kobe Steel Ltd | Al alloy member excellent in corrosion resistance and plasma resistance |
| JP4796464B2 (en) * | 2005-11-17 | 2011-10-19 | 株式会社神戸製鋼所 | Aluminum alloy member with excellent corrosion resistance |
-
2007
- 2007-08-22 JP JP2007216239A patent/JP5064935B2/en not_active Expired - Fee Related
-
2008
- 2008-07-11 CN CNA2008101357595A patent/CN101372731A/en active Pending
- 2008-07-17 US US12/174,845 patent/US20090050485A1/en not_active Abandoned
- 2008-07-25 SG SG200805547-7A patent/SG150438A1/en unknown
- 2008-08-06 TW TW097129844A patent/TW200914627A/en unknown
- 2008-08-11 DE DE102008037271A patent/DE102008037271A1/en not_active Ceased
- 2008-08-21 KR KR1020080081628A patent/KR20090020496A/en not_active Application Discontinuation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420555A (en) * | 2015-11-11 | 2016-03-23 | 苏州三基铸造装备股份有限公司 | Cast aluminum alloy capable of being anodized and preparation method thereof |
| CN110402296B (en) * | 2017-03-10 | 2021-04-20 | 伊苏瓦尔肯联铝业 | High temperature stable aluminum alloy vacuum chamber element |
| CN115698355A (en) * | 2020-06-10 | 2023-02-03 | 爱励轧制产品德国有限责任公司 | Method for manufacturing aluminum alloy sheet for vacuum chamber member |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20090020496A (en) | 2009-02-26 |
| JP5064935B2 (en) | 2012-10-31 |
| SG150438A1 (en) | 2009-03-30 |
| TW200914627A (en) | 2009-04-01 |
| JP2009046747A (en) | 2009-03-05 |
| DE102008037271A1 (en) | 2009-02-26 |
| US20090050485A1 (en) | 2009-02-26 |
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