CN1306070C - Self-lubricating treatment method of porou anode aluminium oxide film - Google Patents
Self-lubricating treatment method of porou anode aluminium oxide film Download PDFInfo
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- CN1306070C CN1306070C CNB2003101193234A CN200310119323A CN1306070C CN 1306070 C CN1306070 C CN 1306070C CN B2003101193234 A CNB2003101193234 A CN B2003101193234A CN 200310119323 A CN200310119323 A CN 200310119323A CN 1306070 C CN1306070 C CN 1306070C
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Abstract
The present invention discloses a self-lubricating process method for a porous anodised aluminum film, which comprises the following steps that an aluminum piece which is processed makes the secondary anodisation in an electrolyte with oxalic acid; an anodised aluminum / aluminum composite film with nanometer holes of which the diameters are identical are uniformly distributed on the surface, polymer nanometer fiber can be compounded in a nanometer hole channel of anode coating by a chemical aggregation method, and the self-lubricating anodised aluminum filled with carbon fiber can be obtained through heat treatment at a certain temperature. The present invention has the characteristics of good pellumina uniformity, easy film thickness control, simple preparation process, easy operation, and favorable performance for antifriction and friction resistance of the self-lubricating pellumina; the self-lubricating anodised aluminum film has fine antifriction and friction resistance performance from a friction experiment, solves the problems of high friction coefficient for a hard anodised aluminum film and brittleness, and can become an effective means in the modification on the surface of aluminum materials in future.
Description
Technical field
The present invention relates to a kind of self-lubrication treatment method of aluminium porous surface anodic alumina films.
Background technology
Alumina is that a class is only second to iron and steel and the metallic substance that extensively adopted by mechanical industry etc.Because its high specific tenacity and excellent solidity to corrosion make that alumina has obtained using very widely in such as automobile, aerospace industry and other hi-tech industry.Yet as tribological material, the serious weakness of alumina is that matter is soft, frictional coefficient is high, wearing and tearing are pulled greatly, easily and is difficult to lubricate, limited its application in tribological field.
Numerous scholars has carried out the research of the tribology surface modification of aluminium.Many new surface modifying methods, as PVD, CVD, three beam modifyings, thermosprays etc. are by improving surface hardness, change surface chemistry state and introducing oilness material reduce abrasive wear and adhesive wear and reduce frictional coefficient, and have obtained good effect, but its equipment is but very expensive.
Anodic oxidation is the most traditional and the surface modifying method of effective aluminium, it can greatly improve the hardness on aluminum products surface, improve its chemical stability, thereby greatly improved its wear-resistant anti scuffing and anti-corrosion capability, but, anode oxide film is brittle ceramic membrane, and its frictional coefficient is very high, in higher speed, load and be with the next rapid inefficacy of ballistic working condition.Utilize the porous structure of anodic oxide coating, but in porous matter anodised aluminium micropore, deposit oilness the material both high rigidity and the wear resistance of holding anode oxide film by means of chemistry, physics or electrochemical method, the oilness of giving material again simultaneously, extremely people's the attention recently of this technology.People such as the stone standing grain of Japan and husband [lubricated ア Le マ イ ト exploitation. rattan storehouse electric wire skill newspaper, clear and 58 years, 65:49-54] work that deposits molybdenumdisulphide with chemical and electrochemical method in anodised aluminium of invention once was described as a revolution of alumina surface modification, but weak point is the loading level deficiency and the MoS of molybdenumdisulphide in the micropore
2Conversion need comparatively high temps.One of improved method is to utilize nano pore inwall in the anodic oxidation aluminium oxide layers to be rich in the characteristics of hydroxyl, makes polymer cation be adsorbed onto the content that the duct inwall can increase oilness material in the micropore.Simultaneously, along with the increase of the oilness substances content of filling, the fragility of anodic oxide coating also is improved.
Summary of the invention
The object of the present invention is to provide a kind of self-lubrication treatment method of porous anodic alumina films, solved the very high and fragility problem of hard anodizing aluminium film frictional coefficient.
Self-lubrication treatment method of the present invention comprises A and two steps of B successively:
A. the preparation of porous hard anodic alumina films
At first, through cleaning scrubbing, the alkali removing oxide layer after the electrochemical polishing treatment, carries out the secondary hard anodizing in the 0.2-0.4mol/L oxalic acid solution with the aluminium flake specimen surface, makes its surface form the porous hard anodized film; Afterwards porous oxide coatings being carried out reaming in the 3-5% phosphoric acid solution handles.
B. the preparation of self-lubricating anodic alumina films
Multiaperture pellumina after the reaming processing is immersed in the acrylonitrile monemer solution of 1.0-1.4mol/L, in the presence of initiator ammonium persulfate, carry out the composite membrane that initiated polymerization obtains containing in the zone of oxidation duct polymer nanofiber, reach proceed step by step thermal treatment under the 500-700 ℃ of argon gas atmosphere under the 240-260 ℃ of air atmosphere respectively afterwards, obtaining being filled with in the duct self-lubricating anodised aluminum compound film of carbon nanofiber.
Porous anodic alumina films of the present invention is to be made of the porous layer that the surface is uniform-distribution with about 80 nanometers of diameter, wherein the nano aperture in the porous layer is parallel to each other and perpendicular to the oxide film surface, arrange by being close to accurate six side's imporositys, the porosity of film reaches 1 * 10
10More than, its thickness between 5～100 microns, preferred 10～50 microns.Through after the self-lubrication treatment, the composite bed that the surface forms is to be made of hard porous anode oxide film and the solid lubricant that is filled in wherein, solid lubricant is a carbon nanofiber, this surface reforming layer controllable thickness is between 5～100 microns, and the characteristics of tool high rigidity, wear-resisting, anti-corrosion and low friction simultaneously.So this law can be carried out the tribology surface modification to various aluminium matter workpiece, has solved the very high problem of hard anodizing aluminium film frictional coefficient, has great importance in the aluminum material surface modification.
Friction-wear test is carried out on the static and dynamic friction coefficient determinator that Nippon Union K. K produces.Sliding velocity 90mmmin
-1, unidirectional sliding stroke is 5mm, the normal direction load is 3N.The idol part is selected the GCr15 steel ball of φ 3 for use.Under room temperature and relative humidity RH=40%～45% condition, measure.Friction and wear test results shows, GCr15 steel ball and pure hard anodizing aluminium surface be the frictional coefficient height when rubbing, and its value is for being 0.88, and the friction track on the alumina surface is coarse, and as seen seriously ruptures and peel off sign.Be reduced to 0.23 through frictional coefficient after the self-lubrication treatment, the friction smooth trajectory on the self-lubricating alumina surface, and abrasive dust is few.Along with the increase of slip number of times, frictional coefficient tends towards stability.
Above coefficient of friction data shows that self-lubricating anodic alumina films involved in the present invention has tangible antifriction and abrasion resistance, and friction pair is had the certain protection effect.This law can be carried out the tribology surface modification to various aluminium matter workpiece.
Embodiment
For a better understanding of the present invention, describe by example
Embodiment 1:
With the fine aluminium sheet through cleaning scrubbing, the alkali removing oxide layer, at 0 ℃, constant voltage anodic oxidation 3h under the 60V volts DS condition in the 0.3mol/L oxalic acid solution removed after the zone of oxidation under the same terms anodic oxidation 5 hours with phosphoric acid-chromic acid mixture then behind the electrochemical etching.With 5% phosphoric acid solution carry out after the reaming careful clean standby.The thickness of the anode oxide film of gained is about 40 μ m, about 80 nanometers of surface micropore aperture.
Aluminium flake after the anodic oxidation is immersed in the acrylonitrile solution of 26mL 1.3mol/L, add the NaHSO of 13ml 20mM then
3Solution, 12ml15mM (NH4)
2S
2O
8Solution and a 0.5mol/L H
2SO
4, 40 ℃ of constant temperature promptly obtain being filled with in the nano pore composite membrane of polyacrylonitrile nano fiber after 2 hours, through the thermal treatment one hour under 600 ℃ of argon gas atmosphere again after one hour of thermal treatment under 250 ℃ of air atmospheres, obtain the self-lubricating anodised aluminum compound film.
Embodiment 2:
With the fine aluminium sheet through cleaning scrubbing, the alkali removing oxide layer, at 0 ℃, constant voltage anodic oxidation 3h under the 60V volts DS condition in the 0.3mol/L oxalic acid solution removed after the zone of oxidation under the same terms anodic oxidation 6 hours with phosphoric acid-chromic acid mixture behind the electrochemical etching.With 5% phosphoric acid solution carry out after the reaming careful clean standby.The thickness of the anode oxide film of gained is about 50 μ m, about 80 nanometers of surface micropore aperture.
Aluminium flake after the anodic oxidation is immersed in the acrylonitrile solution of 26mL 1.3mol/L, add 13ml 20mM NaHSO then
3Solution, 12ml 15mM (NH4)
2S
2O
8Solution and a 0.5mol/L H
2SO
4, 40 ℃ of constant temperature promptly obtain being filled with in the nano pore composite membrane of polyacrylonitrile nano fiber after 2 hours, through the thermal treatment one hour under 700 ℃ of argon gas atmosphere again after one hour of thermal treatment under 250 ℃ of air atmospheres, obtain the self-lubricating anodised aluminum compound film.
Claims (1)
1. the self-lubrication treatment method of an aluminium porous surface anodic alumina films, its feature may further comprise the steps successively in this method:
A. the preparation of porous hard anodic alumina films
At first, through cleaning scrubbing, the alkali removing oxide layer after the electrochemical polishing treatment, carries out the secondary hard anodizing in the 0.2-0.4mol/L oxalic acid solution with the aluminium flake specimen surface, makes its surface form the porous hard anodized film; Afterwards porous oxide coatings being carried out reaming in the 3-5% phosphoric acid solution handles;
B. the preparation of self-lubricating anodic alumina films
Multiaperture pellumina after the reaming processing is immersed in the acrylonitrile monemer solution of 1.0-1.4mol/L, in the presence of initiator ammonium persulfate, carry out the composite membrane that initiated polymerization obtains containing in the zone of oxidation duct polymer nanofiber, reach proceed step by step thermal treatment under the 500-700 ℃ of argon gas atmosphere under the 240-260 ℃ of air atmosphere respectively afterwards, obtaining being filled with in the duct self-lubricating anodised aluminum compound film of carbon nanofiber.
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| CNB2003101193234A CN1306070C (en) | 2003-12-04 | 2003-12-04 | Self-lubricating treatment method of porou anode aluminium oxide film |
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| CNB2003101193234A CN1306070C (en) | 2003-12-04 | 2003-12-04 | Self-lubricating treatment method of porou anode aluminium oxide film |
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| CN1306070C true CN1306070C (en) | 2007-03-21 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101240440B (en) * | 2007-11-16 | 2011-02-16 | 苏州有色金属研究院有限公司 | Technique for preparing high-hardness large-aperture thick film by mixed acid anode oxidation |
| CN102199784B (en) * | 2010-03-22 | 2013-04-10 | 河北师范大学 | Preparation method of porous alumina membrane with two layers communicated with each other |
| CN108531958B (en) * | 2017-03-01 | 2019-12-20 | 比亚迪股份有限公司 | Mobile phone shell and preparation method thereof |
| CN109986742A (en) * | 2017-12-29 | 2019-07-09 | 比亚迪股份有限公司 | Waterproof dyes mobile phone shell and preparation method thereof |
| CN109811397B (en) * | 2019-04-03 | 2021-06-18 | 上海电力学院 | Method for modifying surface of aluminum alloy bipolar plate by using polyacrylonitrile film |
| CN113355712A (en) * | 2021-05-14 | 2021-09-07 | 张健 | Preparation method of corrosion-resistant aluminum alloy |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11256357A (en) * | 1998-03-06 | 1999-09-21 | Nippon Parkerizing Co Ltd | Formation of self-lubricating film on surface of metallic material |
| JP2000045096A (en) * | 1998-05-22 | 2000-02-15 | Mitsubishi Heavy Ind Ltd | Production of self-lubricative anodized aluminum film |
| CN1403632A (en) * | 2002-10-10 | 2003-03-19 | 上海交通大学 | Macroporous thick-film process for anode oxidization of phosphoric acid |
| CN1403633A (en) * | 2002-10-10 | 2003-03-19 | 上海交通大学 | Ultrasonic prepn process of self-lubricating surface composite material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11256357A (en) * | 1998-03-06 | 1999-09-21 | Nippon Parkerizing Co Ltd | Formation of self-lubricating film on surface of metallic material |
| JP2000045096A (en) * | 1998-05-22 | 2000-02-15 | Mitsubishi Heavy Ind Ltd | Production of self-lubricative anodized aluminum film |
| CN1403632A (en) * | 2002-10-10 | 2003-03-19 | 上海交通大学 | Macroporous thick-film process for anode oxidization of phosphoric acid |
| CN1403633A (en) * | 2002-10-10 | 2003-03-19 | 上海交通大学 | Ultrasonic prepn process of self-lubricating surface composite material |
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