CN105349941A - Modification method for obtaining high-harness and high-wear-resistance gradient layer on surface of copper alloy - Google Patents
Modification method for obtaining high-harness and high-wear-resistance gradient layer on surface of copper alloy Download PDFInfo
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- CN105349941A CN105349941A CN201510785955.7A CN201510785955A CN105349941A CN 105349941 A CN105349941 A CN 105349941A CN 201510785955 A CN201510785955 A CN 201510785955A CN 105349941 A CN105349941 A CN 105349941A
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
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Abstract
The invention relates to a modification method, in particular to a modification method for obtaining a high-harness and high-wear-resistance gradient layer on the surface of copper alloy. The modification method aims to solve the problems that copper alloy is low in surface hardness, poor in wear resistance and poor in binding force with a base. The modification method comprises the specific steps that firstly, the surface of copper alloy is coated with a CuxTi(1-x) film through non-balance magnetron sputtering coating; and secondly, the surface, coated with the film, of the copper alloy is subjected to plasma nitriding treatment. The modification method is used for the field of modification of the surface of copper alloy.
Description
Technical field
The present invention relates to a kind of method of modifying, be specifically related to a kind of method of modifying obtaining high rigidity, high-wearing feature gradient layer at copper alloy surface, belong to copper alloy surface modification field.
Background technology
Copper alloy has excellent conduction, heat conductivility has good mechanical property concurrently, is thus widely used in the field of engineering technology such as electronics, automobile, boats and ships, Aeronautics and Astronautics.But there is the shortcomings such as hardness is low, intensity is low, wear resistance is poor in copper alloy, makes it be restricted in friction field range of application.Application surface modification technology can prepare the multiple functional rete with excellent properties on differing materials surface.Current copper alloy surface modification technology comprises: ion implantation, laser modified, thermospray, magnetron sputtering plating etc.After above-mentioned surface modification treatment, copper alloy surface hardness and wear resistance obtain certain raising, but still there is the application of some problems restriction process for modifying surface on copper alloy product.Ion implanted layer is thinner, and thickness is generally no more than 1 μm, and copper alloy product friction and wear behavior cannot be made to effectively improve.Laser surface modification crack problem, the thermal conductivity that copper alloy is good and the specific absorption low to laser cause Laser Surface Modification of Copper Alloy to become difficult point.Copper alloy surface thermospray or surface sputtering plating ganoine thin film, rete differs greatly with Copper substrate linear expansivity, and there is larger stress in interface, lower with the bonding strength of matrix, coating easily comes off.Therefore, copper alloy surface obtains high rigidity, super-high wear-resistant layer, still difficult realization.
The Design & preparation of gradient film be solve that copper alloy surface hardness is low, wear resistance and the effective way of bonding force difference between rete and matrix.The technical requirements that copper alloy surface prepares gradient film is that rete and copper alloy matrix realize metallurgical binding, and prepared copper alloy wearing layer surface hardness is high, section hardness distribution gradient.What ganoine thin film was most widely used in suitability for industrialized production is Ti-N film, its hardness value wide range, effectively can improve the life-span of friction and wear behavior and product.In addition, metallurgical binding can be realized between Cu and Ti.Therefore, Cu will be plated
xti
(1-x)film combines with plasma nitridation technology, to obtaining high rigidity, super-high wear-resistant gradient modified layer at copper alloy surface.
Summary of the invention
The present invention be solve copper alloy surface hardness low, wear no resistance and basic between the problem of bonding force difference, and then a kind of method of modifying obtaining high rigidity, high-wearing feature gradient layer at copper alloy surface is proposed.
The present invention is the technical scheme taked that solves the problem: concrete steps of the present invention are as follows:
Step one, employing non-balance magnetically controlled sputter plated film carry out plating Cu to copper alloy surface
xti
(1-x)film;
Step 2, plasma nitridation process is carried out to the copper alloy surface after plated film.
The invention has the beneficial effects as follows: the invention solves between copper alloy matrix and high rigidity rete in conjunction with hypodynamic problem.Surface hardness significantly improves compared to untreated copper alloy substrate, is up to 1000HV
0.01.Modified layer has excellent wear resistance, and wear rate is compared untreated copper alloy and reduced more than 90%.Improve the problems such as copper alloy surface hardness in prior art, wear resistance be poor.The service life of effective raising copper alloy and stability, have very high engineer applied and be worth.
Accompanying drawing explanation
Fig. 1 a is 6.3 μm of Ti films/C17200 berylliumbronze nitriding 4h curve figure, Fig. 1 b is 6.3 μm of Ti films/C17200 berylliumbronze nitriding 4h matrix and modified layer wear rate comparing result figure, Fig. 2 a is 6.3 μm of Ti films/C61900 xantal tufftridy 4h curve figure, Fig. 2 b is 6.3 μm of Ti films/C61900 xantal tufftridy 4h matrix and modified layer wear rate comparing result figure.
Embodiment
Embodiment one: composition graphs 1 and Fig. 2 illustrate present embodiment, described in present embodiment, a kind of method of modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer realizes as follows:
Step one, employing non-balance magnetically controlled sputter plated film carry out plating Cu to copper alloy surface
xti
(1-x)film;
Step 2, plasma nitridation process is carried out to the copper alloy surface after plated film.
The step one of present embodiment can also adopt the technology such as sputter coating, ion film plating, vapour deposition to carry out plated film to copper alloy surface; In step 2 to the copper alloy surface after plated film can also using plasma carburizing, ooze the method such as oxygen, metallic cementation and process.
Embodiment two: composition graphs 1 and Fig. 2 illustrate present embodiment, described in present embodiment, a kind of specific operation process of step one of the method for modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer is as follows:
Steps A, by copper alloy surface polishing, then copper alloy surface plating Cu
xti
(1-x)film, wherein 0≤x<1;
Step B, membranous layer ingredient are by the power regulation of sputtering target;
Step C, thicknesses of layers are regulated and controled by sputtering time;
Step D, use argon gas are as the sputter gas of non-balance magnetically controlled sputter method.
Other composition and annexation identical with embodiment one.
Embodiment three: composition graphs 1 and Fig. 2 illustrate present embodiment, in the step B of a kind of method of modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer described in present embodiment, Cu target power output is 0 ~ 1kW, Ti target power output is 0.5 ~ 3kW.Other composition and annexation identical with embodiment two.
Embodiment four: composition graphs 1 and Fig. 2 illustrate present embodiment, in the step C of a kind of method of modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer described in present embodiment, the regulation and control time is 2-8h.Other composition and annexation identical with embodiment two.
Embodiment five: composition graphs 1 and Fig. 2 illustrate present embodiment, in the step D of a kind of method of modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer described in present embodiment, the dividing potential drop of argon gas is 3.7 × 10
-2torr, magnetron voltage is 400V, and substrate bias is 70V, and in coating process, vacuum chamber temperature is 20 ~ 200 DEG C.Other composition and annexation identical with embodiment two.
Embodiment six: composition graphs 1 and Fig. 2 illustrate present embodiment, described in present embodiment a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying step 2 in use atmosphere to be hydrogen and nitrogen mixed gas, plasma nitridation temperature is 600 ~ 800 DEG C, soaking time is 0.5 ~ 4h, and flow is respectively 0.1L/min, 0 ~ 0.3L/min.Other composition and annexation identical with embodiment one.
Embodiment seven: composition graphs 1 and Fig. 2 illustrate present embodiment; described in present embodiment a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying step 2 in copper alloy nitriding terminate after under nitrogen or argon; cool to room temperature with the furnace from nitriding temperature, avoid surface oxidation.Other composition and annexation identical with embodiment one.
Embodiment one:
Step one, C17200 berylliumbronze after 790 DEG C of solution treatment 15min, shrend, linear cutter becomes the thin slice of 5mm, sand papering, is polished to minute surface, cleans, cold air drying with acetone;
Non-balance magnetically controlled sputter equipment put into by step 2, copper alloy sample step one obtained, and Cu target power output is 0kW, Ti target power output is 2.8kW, and depositing time is 5h, obtains 6.3 μm of Ti films;
Pulsed plasma multiple permeation stove put into by step 3, copper alloy sample step 2 obtained, and hollow cathode is auxiliary is warming up to 650 ± 5 DEG C, and in stove, atmosphere flow is respectively hydrogen 0.1L/min, nitrogen 0.1L/min, and soaking time is be cooled to room temperature after 4h;
Step 4, modified layer carried out to micro-hardness testing and friction and wear behavior test, hardness test condition: adopt HV-1000 type micro Vickers, load is 10g, loading time is 15s, and friction and wear behavior test condition is: adopting Pin-On-Disk-1-AUTO type friction wear testing machine, is diameter 5mmWC ball to abrading-ball, test is carried out under DRY SLIDING, positive pressure 4N, rotating speed is 200r/min, and test period is 1800s.
The modified layer surface hardness of the present embodiment reaches 982.68HV
0.01, wear rate reduces 96.28%, and wear resistance is greatly improved
Embodiment two:
Step one, C17200 berylliumbronze after 790 DEG C of solution treatment 15min, shrend, linear cutter becomes the thin slice of 5mm, sand papering, is polished to minute surface, cleans, cold air drying with acetone;
Non-balance magnetically controlled sputter equipment put into by step 2, copper alloy sample step one obtained, and Cu target power output is 0kW, Ti target power output is 2.8kW, and depositing time is 5h, obtains 6.3 μm of Ti films;
Pulsed plasma multiple permeation stove put into by step 3, copper alloy sample step 2 obtained, and hollow cathode is auxiliary is warming up to 750 ± 5 DEG C, and in stove, atmosphere flow is respectively hydrogen 0.1L/min, nitrogen 0.1L/min, and soaking time is be cooled to room temperature after 4h;
Step 4, modified layer carried out to micro-hardness testing and friction and wear behavior test, hardness test condition: adopt HV-1000 type micro Vickers, load is 10g, loading time is 15s, and friction and wear behavior test condition is: adopting Pin-On-Disk-1-AUTO type friction wear testing machine, is diameter 5mmWC ball to abrading-ball, test is carried out under DRY SLIDING, positive pressure 4N, rotating speed is 200r/min, and test period is 1800s.
In the present embodiment, modified layer surface hardness reaches 825.47HV
0.01, wear rate reduces 90.73%.
Embodiment three:
Step one, C17200 berylliumbronze after 790 DEG C of solution treatment 15min, shrend, linear cutter becomes the thin slice of 5mm, sand papering, is polished to minute surface, cleans, cold air drying with acetone;
Non-balance magnetically controlled sputter equipment put into by step 2, copper alloy sample step one obtained, and Cu target initial power is 1kW, with the rate reduction of 50W/10min to 50W; Ti target initial power is 100W, is increased to 2.8KW with the speed of 150W/10min, and depositing time is 4h, obtains 5 μm of Cu-Ti films;
Pulsed plasma multiple permeation stove put into by step 3, copper alloy sample step 2 obtained, hollow cathode is auxiliary is warming up to 650 ± 5 DEG C, in stove, atmosphere flow is respectively hydrogen 0.1L/min, nitrogen 0.1L/min, and soaking time is be cooled to room temperature after 0.5h;
Step 4, modified layer carried out to micro-hardness testing and friction and wear behavior test, hardness test condition: adopt HV-1000 type micro Vickers, load is 10g, loading time is 15s, and friction and wear behavior test condition is: adopting Pin-On-Disk-1-AUTO type friction wear testing machine, is diameter 5mmWC ball to abrading-ball, test is carried out under DRY SLIDING, positive pressure 4N, rotating speed is 200r/min, and test period is 1800s.
In the present embodiment, modified layer surface hardness reaches 406.73HV
0.01, wear rate reduces 96.31%.
Embodiment four:
Step one, C61900 xantal after 930 DEG C of solution treatment 120min, shrend, linear cutter becomes the thin slice of 5mm, sand papering, is polished to minute surface, cleans, cold air drying with acetone;
Non-balance magnetically controlled sputter equipment put into by step 2, copper alloy sample step one obtained, and Cu target power output is 0kW, Ti target power output is 2.8kW, and depositing time is 5h, obtains 6.3 μm of Ti films;
Pulsed plasma multiple permeation stove put into by step 3, copper alloy sample step 2 obtained, hollow cathode is auxiliary is warming up to 650 ± 5 DEG C, nitriding atmosphere is that hydrogen 0.1L/min is incubated 2h, then atmosphere is adjusted to hydrogen 0.1L/min, nitrogen 0.1L/min, and soaking time is be cooled to room temperature after 2h;
Step 4, modified layer carried out to micro-hardness testing and friction and wear behavior test, hardness test condition: adopt HV-1000 type micro Vickers, load is 10g, loading time is 15s, and friction and wear behavior test condition is: adopting Pin-On-Disk-1-AUTO type friction wear testing machine, is diameter 5mmGCr15 ball to abrading-ball, test is carried out under DRY SLIDING, positive pressure 4N, rotating speed is 200r/min, and test period is 1800s.
In the present embodiment, modified layer surface hardness reaches 711.39HV
0.01, wear rate reduces 95.64%.
Embodiment five:
Step one, C61900 xantal after 930 DEG C of solution treatment 120min, shrend, linear cutter becomes the thin slice of 5mm, sand papering, is polished to minute surface, cleans, cold air drying with acetone;
Non-balance magnetically controlled sputter equipment put into by step 2, copper alloy sample step one obtained, and Cu target power output is 0kW, Ti target power output is 2.8kW, and depositing time is 7h, obtains 8.8 μm of Ti films;
Pulsed plasma multiple permeation stove put into by step 3, copper alloy sample step 2 obtained, and hollow cathode is auxiliary is warming up to 650 ± 5 DEG C, and in stove, atmosphere flow is respectively hydrogen 0.1L/min, nitrogen 0.1L/min, and soaking time is be cooled to room temperature after 4h;
Step 4, modified layer carried out to micro-hardness testing and friction and wear behavior test.Hardness test condition: adopt HV-1000 type micro Vickers, load is 10g, loading time is 15s, friction and wear behavior test condition is: adopt Pin-On-Disk-1-AUTO type friction wear testing machine, be diameter 5mmWC ball to abrading-ball, test and carry out under DRY SLIDING, positive pressure 4N, rotating speed is 200r/min, and test period is 1800s.
In the present embodiment, modified layer surface hardness reaches 721.87HV
0.01, wear rate reduces 96.04%.
Claims (9)
1. obtain a method of modifying for high rigidity, high-wearing feature gradient layer at copper alloy surface, it is characterized in that: described a kind of method of modifying at copper alloy surface acquisition high rigidity, high-wearing feature gradient layer realizes as follows:
Step one, employing non-balance magnetically controlled sputter plated film carry out plating Cu to copper alloy surface
xti
(1-x)film;
Step 2, plasma nitridation process is carried out to the copper alloy surface after plated film.
2. according to claim 1 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: step one is not limited to non-balance magnetically controlled sputter coating technique, sputter coating, ion film plating, gas-phase deposition coating technology can be adopted.
3. according to claim 1 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: step 2 is not limited to plasma nitridation treatment process, can using plasma carburizing, ooze oxygen, metallic cementation method.
4. according to claim 1 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: the specific operation process of step one is as follows:
Steps A, by copper alloy surface polishing, then copper alloy surface plating Cu
xti
(1-x)film, wherein 0≤x<1;
Step B, membranous layer ingredient are by the power regulation of sputtering target;
Step C, thicknesses of layers are regulated and controled by sputtering time;
Step D, use argon gas are as the sputter gas of non-balance magnetically controlled sputter method.
5. according to claim 4 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: in step B, Cu target power output is 0 ~ 1kW, Ti target power output is 0.5 ~ 3kW.
6. according to claim 4 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: in step C, the regulation and control time is 2-8h.
7. according to claim 4 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: in step D, the dividing potential drop of argon gas is 3.7 × 10
-2torr, magnetron voltage is 400V, and substrate bias is 70V, and in coating process, vacuum chamber temperature is 20 ~ 200 DEG C.
8. according to claim 1 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying, it is characterized in that: in step 2, use the mixed gas that atmosphere is hydrogen and nitrogen, plasma nitridation temperature is 600 ~ 800 DEG C, soaking time is 0.5 ~ 4h, and flow is respectively 0.1L/min, 0 ~ 0.3L/min.
9. according to claim 1 a kind of copper alloy surface obtain high rigidity, high-wearing feature gradient layer method of modifying; it is characterized in that: in step 2 copper alloy nitriding after terminating under nitrogen or argon; cool to room temperature with the furnace from nitriding temperature, avoid surface oxidation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107632509A (en) * | 2016-07-19 | 2018-01-26 | 尼瓦洛克斯-法尔股份有限公司 | Component for watch and clock movement |
| CN114807845A (en) * | 2021-01-28 | 2022-07-29 | 山东大学 | Titanium copper nitride coating with gradually increased nitrogen content gradient |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805996A (en) * | 2014-01-16 | 2014-05-21 | 中国科学院金属研究所 | Composite treating method for nitriding surface of metal material after coating |
-
2015
- 2015-11-16 CN CN201510785955.7A patent/CN105349941A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805996A (en) * | 2014-01-16 | 2014-05-21 | 中国科学院金属研究所 | Composite treating method for nitriding surface of metal material after coating |
Non-Patent Citations (1)
| Title |
|---|
| 杨林: "C17200铜合金表面镀钛渗氮复合改性研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107632509A (en) * | 2016-07-19 | 2018-01-26 | 尼瓦洛克斯-法尔股份有限公司 | Component for watch and clock movement |
| CN114807845A (en) * | 2021-01-28 | 2022-07-29 | 山东大学 | Titanium copper nitride coating with gradually increased nitrogen content gradient |
| CN114807845B (en) * | 2021-01-28 | 2024-02-27 | 山东大学 | Titanium copper nitride coating with gradient increasing nitrogen content |
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Application publication date: 20160224 |