CN116926542B - Copper-nickel-diamond composite material with low friction coefficient and preparation method thereof - Google Patents
Copper-nickel-diamond composite material with low friction coefficient and preparation method thereof Download PDFInfo
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- CN116926542B CN116926542B CN202310855656.0A CN202310855656A CN116926542B CN 116926542 B CN116926542 B CN 116926542B CN 202310855656 A CN202310855656 A CN 202310855656A CN 116926542 B CN116926542 B CN 116926542B
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 98
- 239000010432 diamond Substances 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 76
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052802 copper Inorganic materials 0.000 claims abstract description 50
- 239000010949 copper Substances 0.000 claims abstract description 50
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 25
- 229910000570 Cupronickel Inorganic materials 0.000 claims abstract description 24
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000005554 pickling Methods 0.000 claims abstract description 9
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 8
- 238000007747 plating Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000004544 sputter deposition Methods 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000010849 ion bombardment Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 3
- 238000005275 alloying Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 22
- 239000011159 matrix material Substances 0.000 description 5
- 230000003213 activating effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005271 boronizing Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005475 siliconizing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
-
- 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
- C23C24/00—Coating starting from inorganic powder
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
Abstract
The invention provides a copper-nickel-diamond composite material with a low friction coefficient and a preparation method thereof, comprising the following steps: forming a copper-nickel alloy layer with a surface hole structure by alloying the surface of pure copper; selecting and cleaning diamond powder, carrying out hydrogen microwave plasma hydrogenation or high-temperature pickling oxidation on the cleaned diamond powder to obtain hydrogenated/oxidized diamond powder with a hydrogen terminal or an oxygen terminal enriched on the surface, achieving the effect of dispersing the diamond powder, and uniformly dispersing the hydrogenated/oxidized diamond powder into holes on the surface of the copper-nickel alloy layer; and plating a metal copper film layer on the surface of the copper-nickel alloy layer containing hydrogenated/oxidized diamond powder inside to obtain the copper-nickel-diamond composite material with low friction coefficient. The method is simple, and the friction coefficient of the prepared composite material is far lower than that of pure copper.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a copper-nickel-diamond composite material with a low friction coefficient and a preparation method thereof.
Background
Pure copper is abundant in natural resources, has excellent properties such as excellent electrical conductivity, thermal conductivity, ductility, corrosion resistance, wear resistance and the like, is widely applied to fields such as electric power, electronics, energy, petrifaction, machinery, metallurgy, traffic, light industry, emerging industry and the like, but is soft metal, low in hardness and poor in wear resistance, and the wear loss can be rapidly increased in the use process, so that the friction coefficient is increased, the service life is shortened, and the application range is limited.
At present, a plurality of technologies for strengthening the surface of copper, such as plating chromium or cobalt on the surface of copper and then carrying out boronizing treatment, can form a wear-resistant layer with high hardness on the surface of copper so as to improve the wear resistance; thermal spray coating WC-C on copper surfaces o Composite coating and electrodepositing TiB on the surface of copper matrix 2 The coating can improve the surface strength of copper, but the coating and the matrix form mechanical combination, and the coating is easy to fall off, so that the application effect is poor. Siliconizing the surface of copper to form copper-silicon solid solution and copper-silicon compound on the surface layer, so that the wear resistance can be improved; the nickel and tantalum infiltration can be carried out on the surface of pure copper, so that the surface strength can be improved, the wear resistance can be enhanced, the plastic deformation can be reduced, and the friction coefficient is still larger.
Diamond has excellent thermal properties and high hardness, and can be compounded with a metal matrix to form various metal matrix composites, copper has a higher working temperature than aluminum and a lower price than silver, and copper-based diamond composites have received extensive research attention. The copper-diamond composite material can be prepared by a powder metallurgy method, has high heat conductivity, but the composite material obtained by the method has larger porosity and uneven internal structure, and influences the wear resistance; the spark plasma sintering method is a method for preparing the copper-diamond composite material based on a powder metallurgy method, and is more energy-saving compared with the powder metallurgy method, but the compactness of the obtained composite material is not high enough, and the wear resistance of a copper matrix cannot be effectively improved; the compact copper-diamond composite material can be prepared by adopting a high-temperature and high-pressure method, but the preparation method can damage the structure of the material to a certain extent and can not meet the requirement of high hardness.
Disclosure of Invention
Aiming at the problems of lower hardness, poorer wear resistance and higher friction coefficient of pure copper in the prior art, the invention provides a material for reducing the friction coefficient of copper by compounding nickel and diamond on copper and a preparation method thereof.
The invention provides the following technical scheme:
a method of making a low coefficient of friction copper-nickel-diamond composite comprising:
step S1, performing double-glow plasma nickel infiltration on pure copper to form a copper-nickel alloy layer with a surface hole structure;
s2, selecting and cleaning diamond powder, carrying out hydrogen microwave plasma hydrogenation or high-temperature pickling oxidation on the cleaned diamond powder to obtain hydrogenated/oxidized diamond powder with a surface enriched with hydrogen terminals or oxygen terminals, achieving the effect of dispersing the diamond powder, and uniformly dispersing the hydrogenated/oxidized diamond powder into holes on the surface of the copper-nickel alloy layer;
and S3, plating a metal copper film layer on the surface of the copper-nickel alloy layer containing the hydrogenated/oxidized diamond powder inside to obtain the copper-nickel-diamond composite material with low friction coefficient.
Further, step S1 includes:
s11, placing the cleaned pure copper workpiece on a sample table in a vacuum chamber, wherein a source electrode is a pure nickel plate, and the source electrode and the pure copper workpiece are discharged under the control of two different direct current power supplies;
s12, vacuumizing the vacuum chamber, and then filling a proper amount of argon gas to enable the vacuum chamber to reach the working pressure;
s13, starting a direct current power supply of the pure copper workpiece to ignite glow, bombarding the surface of the workpiece, wherein the pure copper workpiece can play a role in purifying and activating the surface, and the bombardment time of the purifying and activating the surface is 1-10min;
s14, turning on a source power supply, and forming a copper-nickel alloy layer with a surface hole structure under the bombardment of glow ions. This is because under glow ion bombardment, the source and the pure copper workpiece are rapidly heated to high temperatures, which enable the nickel element sputtered from the source to deposit on the surface of the pure copper workpiece and penetrate therein.
Optionally, step S2 includes:
step S21, selecting diamond powder, firstly carrying out acid washing on the diamond powder by using concentrated acid, then carrying out ultrasonic cleaning and water washing on the diamond powder, and drying under a protective atmosphere;
s22, preparing hydrogenated diamond powder with a surface enriched hydrogen terminal by using a hydrogen microwave plasma hydrogenation technology or preparing diamond powder with a surface enriched oxygen terminal by using a high-temperature pickling oxidation technology;
step S23, uniformly dispersing the hydrogenated/oxidized diamond powder into the copper-nickel alloy layer by using ultrasonic waves.
Optionally, step S3 includes:
the magnetron sputtering copper plating process is adopted, pure copper is used as a magnetron sputtering target, a vacuum chamber is vacuumized, argon with certain flow is introduced, a direct current power supply is started, and a metal copper film layer is plated on the surface of a copper-nickel alloy layer containing hydrogenated/oxidized diamond powder.
Optionally, in the step S1, the distance between the source electrode and the pure copper workpiece is 15-20mm, the inflow rate of argon is 25-50sccm, the working air pressure is 25-30Pa, the source electrode voltage is 700-900V, the workpiece voltage is 400-600V, the bombardment time of glow ions is 1-3h, and the reaction temperature is strictly limited to 800-900 ℃.
Optionally, in step S21, the micron and nano diamond powder may be selected, preferably nano powder with particle size below 2 μm, the concentrated acid may be selected from concentrated sulfuric acid and concentrated nitric acid mixed solution, and the solution is pickled at high temperature for 30 minutes to remove the surfactant; ultrasonic cleaning the diamond powder with acetone or ethanol (preferably acetone) for 20 min after acid washing; after ultrasonic cleaning, deionized water was used to clean the diamond powder and dried under nitrogen atmosphere.
Optionally, in step S22, when the hydrogen microwave plasma hydrogenates the diamond powder, the pressure is 5.3-5.7kPa, the temperature is 650-750 ℃, the working time is 5-10min, and the hydrogen-rich atmosphere is maintained for more than half an hour after the plasma hydrogenation is finished, so as to obtain the hydrogenated diamond powder with the surface enriched with hydrogen terminals. After the diamond powder forms a hydrogen termination surface, the vicinity of the carbon atoms is negatively charged, the vicinity of the hydrogen atoms is positively charged, and the hydrogen atoms exposed to the outside repel each other, forming a dispersed hydrogenated diamond powder.
Optionally, in step S22, the diamond powder is directly placed in HNO while the diamond powder is oxidized by high-temperature pickling 3 /H 2 SO 4 The volume ratio is 1:4, heating to 240-290 ℃ in the mixed concentrated acid solution, and preserving heat for more than 1 hour to obtain the oxidized diamond powder with the surface enriched with oxygen terminals, thereby achieving the effect of dispersing the diamond powder.
Optionally, in the magnetron sputtering coating process in the step S3, the target base distance is 50-70mm, the air inlet flow of argon is 20-50sccm, the working air pressure is 0.5-0.8Pa, the sputtering power is 80-100W, and the sputtering coating time is 1-4h.
Further, the invention also provides a copper-nickel-diamond composite material with a low friction coefficient.
The key of the implementation process of the invention is as follows:
(1) Alloying the pure copper surface by using a double-glow plasma nickel-penetrating technology to form a copper-nickel alloy layer with a surface hole structure.
(2) And (3) carrying out hydrogen microwave plasma hydrogenation or high-temperature pickling oxidation on the cleaned diamond powder to enrich hydrogen terminals or oxygen terminals on the surface, thereby obtaining the dispersed diamond powder.
(3) And plating a metal copper film layer on the surface of the alloy layer by using a magnetron sputtering coating process, and packaging diamond powder.
The technical scheme provided by the invention has the beneficial effects that at least:
1) The diamond powder is hydrogenated by hydrogen microwave plasma or oxidized by high-temperature acid washing to form a hydrogen terminal or oxygen terminal surface, so as to obtain the dispersed diamond powder.
2) The copper-nickel-diamond composite material has high hardness and good wear resistance, and prolongs the service life of the material.
3) The friction coefficient of the composite material prepared by the invention is far lower than that of pure copper.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an SEM image of a copper-nickel alloy layer prepared according to example 1 of the invention;
FIG. 3 is an SEM image of the diamond powder prepared in example 1 of the present invention after being uniformly dispersed in the pores of the copper-nickel alloy layer;
fig. 4 is a graph showing the friction coefficient of the copper-nickel-diamond composite material prepared in example 1 according to the present invention compared with that of a pure copper control experiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
Placing the cleaned pure copper workpiece on a sample table in a vacuum chamber, wherein a source electrode is a pure nickel plate, vacuumizing the vacuum chamber to the limit, and filling argon with the air inlet flow of 25sccm to reach the working air pressure of 25 Pa. And (3) starting a direct current power supply of the workpiece, wherein the voltage is 550V, igniting glow, bombarding the surface of the workpiece for about 5min, and purifying and activating the surface. And (3) starting a source power supply, wherein the voltage is 750V, and the source and the workpiece are rapidly heated to high temperature under the bombardment of glow ions. At 850 deg.c, the glow ion bombard for 2.5 hr to deposit nickel element on the surface of workpiece and penetrate into the workpiece to form copper-nickel alloy layer (see fig. 2). Selecting diamond powder with the particle size of 500nm, pickling the diamond powder with concentrated acid to remove a surfactant, ultrasonically cleaning the diamond powder with an acetone solution, then washing the diamond powder with deionized water, and drying the diamond powder in a nitrogen atmosphere. Putting the diamond powder into a microwave device, introducing microwaves, and hydrogenating the diamond powder with hydrogen microwave plasma for 8min under the condition that the pressure is 5.55kPa and the temperature is 700 ℃ to obtain the diamond powder with the surface enriched with hydrogen terminals and dispersed. Ultrasonic separation of diamond powderInto the copper-nickel alloy layer to form a copper-nickel alloy layer containing diamond powder therein (see fig. 3). Pure copper (purity of 99.99%) is used as a magnetron sputtering target, a workpiece is used as a substrate, the target base distance is 60mm, and a vacuum chamber is pumped to 5 multiplied by 10 -3 And (3) Pa, introducing argon with the flow of 40sccm, starting a direct current power supply at the working air pressure of 0.6Pa, sputtering power of 100W, and sputtering and coating for 3 hours, and coating a copper film layer on the surface of the workpiece, thereby obtaining the copper-nickel-diamond composite material. The average coefficient of friction of the copper-nickel-diamond composite is 0.26, which is much lower than 6.1 of the pure copper matrix (see fig. 4).
Example 2
Placing the cleaned pure copper workpiece on a sample table in a vacuum chamber, wherein a source electrode is a pure nickel plate, vacuumizing the vacuum chamber to the limit, and filling argon with the air inlet flow of 50sccm to reach the working air pressure of 25 Pa. And (3) starting a direct current power supply of the workpiece, wherein the voltage is 450V, igniting glow, bombarding the surface of the workpiece for about 5min, and purifying and activating the surface. And (3) starting a source power supply, wherein the voltage is 700V, and the source and the workpiece are rapidly heated to high temperature under the bombardment of glow ions. And bombarding the glow ion for 2.5 hours at the temperature of 800 ℃, and depositing nickel elements sputtered from the source on the surface of the workpiece and penetrating the nickel elements into the workpiece to form a copper-nickel alloy layer. Selecting diamond powder with the particle size of 500nm, pickling the diamond powder with concentrated acid to remove a surfactant, ultrasonically cleaning the diamond powder with an acetone solution, then washing the diamond powder with deionized water, and drying the diamond powder in a nitrogen atmosphere. Directly placing diamond powder into HNO 3 /H 2 SO 4 The volume ratio is 1:4, heating to 260 ℃ in the mixed concentrated acid solution, and preserving the temperature for 70 minutes to obtain the diamond powder with the surface enriched with oxygen terminals and dispersed. The diamond powder is dispersed into the copper-nickel alloy layer by ultrasonic wave to form the copper-nickel alloy layer containing the diamond powder inside. Pure copper (purity of 99.99%) is used as a magnetron sputtering target, a workpiece is used as a substrate, the target base distance is 60mm, and a vacuum chamber is pumped to 5 multiplied by 10 -3 Pa, introducing argon with the flow of 40sccm, operating air pressure of 0.6Pa, starting a direct current power supply, sputtering power of 100W, sputtering and coating for 3 hours, and coating a copper film layer on the surface of a workpiece to obtain copper-nickel-goldA diamond composite material. The average coefficient of friction is about 0.28.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (4)
1. A method of making a low coefficient of friction copper-nickel-diamond composite comprising:
step S1, performing double-glow plasma nickel infiltration on pure copper to form a copper-nickel alloy layer with a surface hole structure;
s2, selecting and cleaning diamond powder, carrying out hydrogen microwave plasma hydrogenation or high-temperature pickling oxidation on the cleaned diamond powder to obtain hydrogenated/oxidized diamond powder with a surface enriched with hydrogen terminals or oxygen terminals, achieving the effect of dispersing the diamond powder, and uniformly dispersing the hydrogenated/oxidized diamond powder into holes on the surface of the copper-nickel alloy layer;
s3, plating a metal copper film layer on the surface of the copper-nickel alloy layer containing hydrogenated/oxidized diamond powder inside to obtain a copper-nickel-diamond composite material with a low friction coefficient;
the step S1 comprises the following steps:
s11, placing the cleaned pure copper workpiece on a sample table in a vacuum chamber, wherein a source electrode is a pure nickel plate, and the source electrode and the pure copper workpiece are discharged under the control of two different direct current power supplies;
s12, vacuumizing the vacuum chamber, and then filling a proper amount of argon gas to enable the vacuum chamber to reach the working pressure;
s13, starting a direct current power supply of the pure copper workpiece to ignite glow, and bombarding the surface of the workpiece;
s14, starting a source power supply, and forming a copper-nickel alloy layer with a surface hole structure under the bombardment of glow ions;
the distance between the source electrode and the pure copper workpiece is 15-20mm, the air inlet flow rate of argon is 25-50sccm, the working air pressure is 25-30Pa, the source electrode voltage is 700-900V, the workpiece voltage is 400-600V, the time of glow ion bombardment is 1-3h, and the reaction temperature is 800-900 ℃;
the step S2 comprises the following steps:
step S21, selecting diamond powder, firstly carrying out acid washing on the diamond powder by using concentrated acid, then carrying out ultrasonic cleaning and water washing on the diamond powder, and drying under a protective atmosphere;
s22, preparing hydrogenated diamond powder with a surface enriched hydrogen terminal by using a hydrogen microwave plasma hydrogenation technology or preparing oxidized diamond powder with a surface enriched oxygen terminal by using a high-temperature pickling oxidation technology;
step S23, uniformly dispersing hydrogenated/oxidized diamond powder into the copper-nickel alloy layer by using ultrasonic waves;
in step S21, diamond powder with the diameter of less than 2 mu m is selected, and the concentrated acid is a mixed solution of concentrated sulfuric acid and concentrated nitric acid; washing diamond powder with acetone or methanol after acid washing; after ultrasonic cleaning, cleaning diamond powder by using deionized water and drying in a nitrogen atmosphere;
in the step S22, when the hydrogen microwave plasma hydrogenates the diamond powder, the pressure is 5.3-5.7kPa, the temperature is 650-750 ℃, the working time is 5-10min, and the hydrogen-rich atmosphere is maintained for more than half an hour after the plasma hydrogenation is finished, so that the hydrogenated diamond powder with the surface enriched with hydrogen terminals is obtained, and the effect of dispersing the diamond powder is achieved; alternatively, when the diamond powder is oxidized by high-temperature acid washing, the diamond powder is directly placed in HNO 3 /H 2 SO 4 Heating to 240-290 ℃ in a mixed concentrated acid solution with the volume ratio of 1:4, and preserving heat for more than 1 hour to obtain the oxidized diamond powder with the surface enriched with oxygen terminals.
2. The method according to claim 1, wherein step S3 comprises:
the magnetron sputtering copper plating process is adopted, pure copper is used as a magnetron sputtering target, a vacuum chamber is vacuumized, argon is introduced, a direct current power supply is started, and a metal copper film layer is plated on the surface of a copper-nickel alloy layer containing hydrogenated/oxidized diamond powder.
3. The method according to claim 2, wherein in the magnetron sputtering coating process in the step S3, the target base distance is 50-70mm, the inflow rate of argon is 20-50sccm, the working air pressure is 0.5-0.8Pa, the sputtering power is 80-100W, and the sputtering coating time is 1-4h.
4. A low coefficient of friction copper-nickel-diamond composite prepared by the method of any one of claims 1-3.
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