CN105331941A - Micro-arc oxidation method for surfaces of copper, copper alloy, zinc and zinc alloy - Google Patents
Micro-arc oxidation method for surfaces of copper, copper alloy, zinc and zinc alloy Download PDFInfo
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- CN105331941A CN105331941A CN201510647800.7A CN201510647800A CN105331941A CN 105331941 A CN105331941 A CN 105331941A CN 201510647800 A CN201510647800 A CN 201510647800A CN 105331941 A CN105331941 A CN 105331941A
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- zinc
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
-
- 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
- C25D11/024—Anodisation under pulsed or modulated current or potential
-
- 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
-
- 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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
Abstract
The invention discloses a micro-arc oxidation method for surfaces of copper, copper alloy, zinc and zinc alloy. The method includes the steps that aluminum films are manufactured on the surfaces of the copper or the copper alloy or the zinc or the zinc alloy through a magnetron sputtering method, the aluminum films are then treated through a micro-arc oxidation method, and therefore aluminum oxide ceramic films are obtained. Due to the fact that non-valve metal subjected to magnetron sputtering treatment is then subjected to micro-arc oxidation, the aluminum oxide ceramic films are obtained, abrasion resistance is improved by more than 10 times, and corrosion resistance is enhanced greatly; and the technical problem that the ceramic films cannot be manufactured for the non-valve metal through the micro-arc oxidation method or the performance of the manufactured ceramic films is quite poor is solved.
Description
Technical field
The present invention relates to a kind of at copper, copper alloy, zinc and zinc alloy surface differential arc oxidation method, belong to electrochemical field.
Background technology
As everyone knows, only have valve metal (aluminium, magnesium, zirconium, titanium etc.) directly could carry out differential arc oxidation process on surface, and the non-valve metals such as copper, iron, zinc directly can not carry out differential arc oxidation on surface, need to carry out secondary treatment, but the differential arc oxidation film layer carried out again after most of secondary treatment all can come across matrix attachment loosely, rete such as to wear no resistance at the feature.
Because Cu-base composites has very high conduction, heat conductivility, be expected to be used in requirement and have both highly conc and wear resistance field, Cu-base composites often will carry out sliding contact with various material as conducting element in actual applications, it is the major issue merited attention that the wearing and tearing of material comprise matrix material self with the wearing and tearing of pairing couple, it directly has influence on the normal work of whole slip electric contact-system, so these parts often require that material has high electrical conductivity, while thermal conductivity, also to possess excellent wear resistance, therefore, the friction and wear behavior of such matrix material is furtherd investigate there is important theory and realistic meaning.Equally, for zinc and zinc alloy material, its wear-resisting and corrosion resistance nature also needs further raising.
Summary of the invention
The technical problem that the present invention solves prepares alumina ceramic membrane by the method for differential arc oxidation at copper, copper alloy, zinc and zinc alloy surface, improves wear resistance and the erosion resistance of these metals.
Technical scheme of the present invention is, there is provided a kind of at copper, copper alloy, zinc and zinc alloy surface differential arc oxidation method, first prepare aluminium film with magnetron sputtering method at copper, copper alloy, zinc or zinc alloy surface, then with micro-arc oxidation, described aluminium film is processed, obtain alumina ceramic membrane.
Further, the thickness of described aluminium film is 6-200 micron.
Further, the thickness of described aluminium film is 40-60 micron.
Further, the design parameter of described micro-arc oxidation is: make anode to prepare the copper after having aluminium film, copper alloy, zinc or zinc alloy, negative electrode made by steel plate; The concentration of electrolytic solution is 10-70g/L, temperature 20-30 DEG C; Power parameter is set to: positive current is 2-10A/dm
2, negative current is 1-9A/dm
2, positive negative duty is 10%-30%, and frequency is 1000-3000Hz.
Further, described electrolytic solution is the aluminate of 12-60g/L, the potassium hydroxide of phosphoric acid salt or silicate and 1-5g/L forms.
Further, described aluminate, phosphoric acid salt and silicate are sodium salt.
Differential arc oxidization technique is as the process for treating surface of the very strong rising in recent years of sticking power at matrix surface growth in situ, effect highly significant in the wear-resisting and rotproofness improving aluminium alloy and zirconium alloy thereof, but copper, zinc and alloy thereof can not carry out conventional differential arc oxidation process.
One deck aluminium film was plated at copper, zinc and alloy surface thereof before differential arc oxidation, film coating method is a lot, have spraying, hot dipping cross, but the film of these methods plating and matrix adhesive force not firm, even if also not obvious to the raising of the wear resistance of copper, zinc or its alloy, erosion resistance after differential arc oxidation.
Magnetron sputtering of the present invention is as a kind of method of sputter coating, film and the matrix adhesive force of sputtering are firm, and the advantage of sputtered film thickness can be controlled, the very strong alumina ceramic membrane of one deck sticking power can be obtained after differential arc oxidation process, the wear resistance of rete can be strengthened greatly.
The method of the magnetron sputtering first that we adopt first after matrix surface sputters one deck pure aluminium film again the method for differential arc oxidation can strengthen the wear resisting property of non-valve metal greatly, the work-ing life of material can be extended to a great extent, save material.
In order to improve film performance, we devise following technical scheme, and concrete steps are as follows:
1, copper, copper alloy, zinc or zinc alloy sample respectively with the SiC sand papering of 60# to 5000#, then use polishing cloth polishing, and with alcohol, deionized water rinsing.
2, the copper after polishing, copper alloy, zinc or zinc alloy sample are carried out magnetron sputtering, the fine aluminium film of one deck 6 to 200 microns can be sputtered as requested, specifically use the rete of which kind of thickness according to purposes.
3, the sample epoxy sealing after magnetron sputtering, the area being coated with aluminium film is exposed.
4, electrolytic solution is prepared: the mixed solution of aluminate (12-60g/L) and potassium hydroxide (1-5g/L).Electrolytic solution is placed in circulating cooling groove keeps electrolyte temperature at (20-30) DEG C.
5, arrange mao power source parameter, positive current is (2-10) A/dm
2, negative current is set to (1-9) A/dm
2, positive negative duty is set to 10%-30%, frequency maintains (1000-3000) Hz.
6, copper, copper alloy, zinc or zinc alloy sample are done anode, steel plate does negative electrode, opening power reaction (4-10) min.
7, take out sample, rinse with clear water, then use deionized water rinsing, dry.The alumina ceramic membrane of one deck high abrasion is now just defined at copper, iron, zinc and alloy surface thereof.
The invention has the beneficial effects as follows, the copper after magnetron sputtering process, copper alloy, zinc or zinc alloy carry out the alumina ceramic membrane that differential arc oxidation obtains again, and wear resistance improves more than 10 times, and erosion resistance also greatly enhances; Solving copper, copper alloy, zinc and zinc alloy can not use micro-arc oxidation to prepare the technical problem of the ceramic membrane poor performance of ceramic membrane or preparation.
Accompanying drawing explanation
Fig. 1 represents that the brass base of the Brass sample that embodiment 1 obtains and comparative example 1 rubs the Wear track depth comparison diagram formed after 30min respectively under the load of 50N and 10N.
Fig. 2 represents the polarization curve comparison diagram of brass base respectively in the NaCl electrolytic solution of 3.5% of the Brass sample that embodiment 1 obtains and comparative example 1.
Embodiment
Below respectively for copper, copper alloy, zinc and zinc alloy, carry out differential arc oxidation process, technique effect of the present invention is described further.
Embodiment 1: the fine aluminium film forming one deck 40 microns after brass polishing through magnetron sputtering, after epoxy sealing, it is that 32g/L sodium aluminate adds in 1g potassium hydroxide that brass is placed on concentration, and arranging electrolytic parameter is positive current 0.6A/cm
2negative current is 0.5A/cm
2, positive negative duty is 20%, and frequency is 1000Hz.Do anode with brass after sputtering fine aluminium film, steel plate does negative electrode, and reaction 5min, just can form the abradability aluminium oxide ceramics film of one deck densification, obtain Brass sample in brass surfaces.
Brass sample embodiment 1 obtained carries out wear resistance and erosion resistance test, and its main testing tool is as follows:
TT260 carries out layer thickness tester: Beijing Time Zhifeng Science Co., Ltd.Can be used to the thickness measuring rete;
MIS800 type ionic fluid magnetron sputtering composite coating equipment: Ke You vacuum technique institute of Shenyang City;
X-ray diffractometer: (place of production Japan, model is RigakuD/MAX2500).Detect the composition of rete phase;
CETRUMT-3 frictiograph: adopt the fast formula rub(bing)test of ball-film, detects sample wear resistance;
Optical profilometer (WykoNT9100, VEECOInstrumentsInc.): detect Wear track depth;
CHI660 electrochemical workstation (Shanghai Chen Hua instrument company): the erosion resistance detecting film.
Comparative example 1: at identical conditions, tests as a comparison with brass base (namely not carrying out the brass processed).As depicted in figs. 1 and 2, rub under the 50N brass base of polishing scratch figure that 30min obtains and comparative example 1 of the Brass sample that the embodiment 1 that Fig. 1 represents obtains rubs the polishing scratch figure comparison diagram that 30min obtains experimental result under 10N.
As can be seen from the figure, under this kind of optimum configurations, the Wear track depth of embodiment 1 under 50N is 15.6 microns, and is being only 34.5 microns with the Wear track depth of the comparative example 1 of the 30min that rubs under 10N, thinks that its wear resistance improves 11 times through simple conversion.
Fig. 2 represents the polarization curve comparison diagram of the brass base of the Brass sample that embodiment 1 obtains and comparative example 1 in the NaCl electrolytic solution of 3.5%.The erosion resistance electric current of embodiment 1 decreases 2 orders of magnitude compared with the erosion resistance electric current of the brass base of comparative example 1, and curve is more past to move to left, and represent that erosion resistance is better, current density is also less.
Embodiment 2: carry out differential arc oxidation process of the present invention to copper by the condition of embodiment 1, the aluminium film thickness wherein first prepared through magnetron sputtering is 60 microns.Contrast wear resistance with corresponding undressed copper and about improve 17 times, erosion resistance electric current is compared and is decreased about 3 orders of magnitude.
Embodiment 3: carry out differential arc oxidation process of the present invention to zinc by the condition of embodiment 1, the aluminium film thickness wherein first prepared through magnetron sputtering is 45 microns.Contrast wear resistance with corresponding undressed zinc and about improve 12 times, erosion resistance electric current is compared and is decreased about 2 orders of magnitude.
Embodiment 4: carry out differential arc oxidation process of the present invention to zinc alloy by the condition of embodiment 1, the aluminium film thickness wherein first prepared through magnetron sputtering is 50 microns.Contrast wear resistance with corresponding undressed zinc alloy and about improve 15 times, erosion resistance electric current is compared and is decreased about 2.5 orders of magnitude.
Although aluminium film prepared by magnetron sputtering reaches 6 microns can carry out differential arc oxidation, the present invention find aluminium film reach 40-60 micron time, wear-resisting and corrosion resistance nature both can reach better level, though can continue the thickness increasing aluminium film, can increase process costs.
Claims (6)
1. one kind at copper, copper alloy, zinc and zinc alloy surface differential arc oxidation method, it is characterized in that, first prepare aluminium film with magnetron sputtering method at copper, copper alloy, zinc or zinc alloy surface, then with micro-arc oxidation, described aluminium film is processed, obtain alumina ceramic membrane.
2. the method for claim 1, is characterized in that, the thickness of described aluminium film is 6-200 micron.
3. the method for claim 1, is characterized in that, the thickness of described aluminium film is 40-60 micron.
4. the method for claim 1, is characterized in that, the design parameter of described micro-arc oxidation is: make anode to prepare the copper after having aluminium film, copper alloy, zinc or zinc alloy, negative electrode made by steel plate; The concentration of electrolytic solution is 10-70g/L, temperature 20-30 DEG C; Power parameter is set to: positive current is 2-10A/dm
2, negative current is 1-9A/dm
2, positive negative duty is 10%-30%, and frequency is 1000-3000Hz.
5. method as claimed in claim 4, is characterized in that, described electrolytic solution is the aluminate of 12-60g/L, the potassium hydroxide of phosphoric acid salt or silicate and 1-5g/L forms.
6. method as claimed in claim 5, it is characterized in that, described aluminate, phosphoric acid salt and silicate are sodium salt.
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| CN201510647800.7A CN105331941B (en) | 2015-10-09 | 2015-10-09 | One kind is in copper, copper alloy, zinc and zinc alloy surface differential arc oxidation method |
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| CN201510647800.7A CN105331941B (en) | 2015-10-09 | 2015-10-09 | One kind is in copper, copper alloy, zinc and zinc alloy surface differential arc oxidation method |
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| CN105331941A true CN105331941A (en) | 2016-02-17 |
| CN105331941B CN105331941B (en) | 2017-12-08 |
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Cited By (8)
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|---|---|---|---|---|
| CN110016708A (en) * | 2019-04-16 | 2019-07-16 | 湖南大学 | Suitable for copper and its micro-arc oxidization surface processing method and product of alloy |
| CN110952104A (en) * | 2019-08-19 | 2020-04-03 | 西南交通大学 | Method for preparing deep narrow gap consumable electrode gas shielded welding contact tip |
| CN111394771A (en) * | 2020-04-22 | 2020-07-10 | 哈尔滨工业大学 | Method for preparing coating on surface of copper and copper alloy and copper product |
| CN111705287A (en) * | 2020-07-10 | 2020-09-25 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C4F7N etching method |
| CN111763898A (en) * | 2020-06-01 | 2020-10-13 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C5F10O gas etching method |
| CN112226768A (en) * | 2020-10-13 | 2021-01-15 | 辽宁科技大学 | Composite preparation method of micro-arc oxidation CrAlN coating |
| CN112813392A (en) * | 2020-12-31 | 2021-05-18 | 中国科学院宁波材料技术与工程研究所 | Solid-liquid compound wear-resistant antibacterial material based on capillary action, preparation method and application |
| CN115233157A (en) * | 2022-06-14 | 2022-10-25 | 沈阳大学 | Method for preparing copper film on surface of zinc and zinc alloy through magnetron sputtering |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016708A (en) * | 2019-04-16 | 2019-07-16 | 湖南大学 | Suitable for copper and its micro-arc oxidization surface processing method and product of alloy |
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| CN110952104A (en) * | 2019-08-19 | 2020-04-03 | 西南交通大学 | Method for preparing deep narrow gap consumable electrode gas shielded welding contact tip |
| CN111394771A (en) * | 2020-04-22 | 2020-07-10 | 哈尔滨工业大学 | Method for preparing coating on surface of copper and copper alloy and copper product |
| CN111394771B (en) * | 2020-04-22 | 2021-05-04 | 哈尔滨工业大学 | Method for preparing coating on surface of copper and copper alloy and copper product |
| CN111763898A (en) * | 2020-06-01 | 2020-10-13 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C5F10O gas etching method |
| CN111763898B (en) * | 2020-06-01 | 2021-10-01 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C5F10O gas etching method |
| CN111705287A (en) * | 2020-07-10 | 2020-09-25 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C4F7N etching method |
| CN111705287B (en) * | 2020-07-10 | 2021-07-30 | 武汉大学 | Metal surface treatment for electrical insulation equipment for preventing C4F7N etching method |
| CN112226768A (en) * | 2020-10-13 | 2021-01-15 | 辽宁科技大学 | Composite preparation method of micro-arc oxidation CrAlN coating |
| CN112813392A (en) * | 2020-12-31 | 2021-05-18 | 中国科学院宁波材料技术与工程研究所 | Solid-liquid compound wear-resistant antibacterial material based on capillary action, preparation method and application |
| CN115233157A (en) * | 2022-06-14 | 2022-10-25 | 沈阳大学 | Method for preparing copper film on surface of zinc and zinc alloy through magnetron sputtering |
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