CN103643075A - Nano-particle reinforced copper-based composite material and preparation method thereof - Google Patents
Nano-particle reinforced copper-based composite material and preparation method thereof Download PDFInfo
- Publication number
- CN103643075A CN103643075A CN201310632642.9A CN201310632642A CN103643075A CN 103643075 A CN103643075 A CN 103643075A CN 201310632642 A CN201310632642 A CN 201310632642A CN 103643075 A CN103643075 A CN 103643075A
- Authority
- CN
- China
- Prior art keywords
- nano
- base composites
- copper
- preparation
- molybdenum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a nano-particle reinforced copper-based composite material and a preparation method thereof. The size of a copper matrix grain is smaller than 20 microns in the copper-based composite material; the nano-particle reinforced phase is molybdenum carbide, or molybdenum carbide and molybdenum, or molybdenum carbide and carbon; the particle size of the nano-particle reinforced phase is smaller than 200nm; the mass percent of Mo in the copper-based composite material is 0.1-15%; the mass percent of C is smaller than 1%. The nano-particle reinforced copper-based composite material disclosed by the invention is prepared by adopting an electronic beam physical vapor deposition process. The nano-particle reinforced copper-molybdenum-carbon composite material prepared by the method has excellent mechanical property and electrical property, and adopted electronic beam physical vapor deposition process is simple, low in cost and easy to control.
Description
Technical field
The present invention relates to Cu-base composites of a kind of nano-particle reinforcement and preparation method thereof, be specifically related to a kind of copper-molybdenum-carbon composite and preparation method of nano-particle reinforcement.
Background technology
Copper and Cu alloy material are a kind of important nonferrous materialss, owing to having excellent physical and mechanical properties, in fields such as electronic industries, obtain a wide range of applications.But along with the fast development of science and technology (the especially fast development of microelectronics industry), traditional copper and alloy thereof can not be taken into account due to electrical property and intensity, can not meet the demands.It is to take the advanced composite material that nanoparticle is second-phase that nano dispersion reinforced copper closes, because nanoparticle can hinder dislocation motion and Grain Boundary Sliding effectively, the mechanical property of material is improved, simultaneously can obviously not reduce specific conductivity, thereby solve preferably the problem that electrical property and intensity can not be taken into account.At present, the enhancing particle in this material has oxide compound, carbide, boride, nitride and refractory metal etc.Prepare the method for this material mainly by internal oxidation, powder metallurgy process and Mechanical Alloying etc.Internal oxidation is to utilize under hypoxia condition in Cu-Al alloy Al that selective oxidation occurs to form Al
2o
3technique.This technique is at present for the preparation of Cu-Al
2o
3the main technique of dispersion strengthening composites, the material property of preparation is good, but this technique also exists complex procedures, the cycle is long, cost is high shortcoming.Powder metallurgic method be utilize copper powder with strengthen particle according to a certain ratio be dry mixed or wet mixing condition under; through the mechanically mixing uniform mixed powder of mix particles that can be enhanced; sintering under moulding, vacuum or protective atmosphere condition, multiple pressure, resintering are prepared the technique of material.Although this technique can be prepared the matrix material that various size strengthen particle distribution, also exist the shortcoming that poor mechanical property, operation are many, cost is high of the matrix material of preparation.Mechanical Alloying is after adopting high energy ball mill that copper powder and enhancing mix particles is even, sintering under moulding, vacuum or protective atmosphere condition, the technique of press again, resintering being prepared material.Equally, also there is poor mechanical property, operation is many, cost is high shortcoming in this technique.In a word, about preparing nano dispersion reinforced Cu-base composites, all there is the problem that operation is many, the cycle is long, cost is high at present.Therefore, under this background, inventing a kind of matrix material of high-strength highly-conductive electrical property and operation is simple, cost is low preparation technology has great importance.
Summary of the invention
The object of this invention is to provide Cu-base composites of a kind of nano-particle reinforcement with excellent mechanical property, electrical property and preparation method thereof.
For achieving the above object, the present invention adopts following technical scheme:
The invention provides a kind of Cu-base composites of nano-particle reinforcement, in described Cu-base composites, copper matrix grain size is less than 20 μ m, and nano-particle reinforcement is molybdenum carbide or molybdenum carbide and molybdenum or molybdenum carbide and carbon mutually, and the particle size of nano-particle reinforcement phase is below 200nm; In described Cu-base composites, the quality percentage composition of Mo is 0.1-15%, and the quality percentage composition of C is below 1%.
The performance index of described Cu-base composites are as follows: yield strength R
p0.2>=420MPa, tensile strength Rm>=480MPa, specific conductivity>=70%ICAS.
The present invention also provides a kind of preparation method of Cu-base composites of described nano-particle reinforcement, comprises the steps:
(1) a kind of in copper ingot material and molybdenum source, carbon source or two kinds are put in crucible respectively, and put isolating layer material on copper ingot material;
(2) vacuumize heated substrates;
(3) when vacuum tightness reaches 9 * 10
-2pa is following, substrate temperature reaches 500-800 ℃, opens substrate rotating device, makes substrate rotation, layer deposited isolating;
(4) open baffle plate, start deposition material;
(5) deposited, after substrate is cooling, taken off substrate, separation obtains settled layer material, is the Cu-base composites of nano-particle reinforcement.
In described step (1), molybdenum source or carbon source can be made into corresponding ingot and are placed in respectively crucible, or carbon is made to ingot, put molybdenum raw material be placed in same crucible at this above ingot.
Further, described carbon source is carbon target, or carbon dust, or anthracene powder.
Further, isolating layer material is selected from CaF
2or ZrO
2.
Further, in deposition process, substrate rotating speed is controlled at 3-20rev/min.
In described step (4), those skilled in the art can be according to actual needs by controlling the line size of electron beam gun and composition and the thickness that depositing time is controlled deposition material.
Compared with prior art, the invention has the beneficial effects as follows:
(1) copper-molybdenum-carbon composite of the nano-particle reinforcement that the present invention makes has excellent mechanical property and electrical property, its yield strength R
p0.2>=420MPa, tensile strength Rm>=480MPa, specific conductivity>=70%IACS, and the room temperature yield strength of fine copper is 33MPa, tensile strength is 209MPa;
(2) the electro beam physics vapour deposition technique that the present invention adopts is simple, and cost is low, is easy to control.Particularly, at present the sedimentation rate of copper can reach 20 μ m/min, i.e. sedimentation diameter 1m, and the sheet material that thickness is 2mm only need deposit 100min.And same internal oxidation is prepared nano dispersion reinforced Cu-base composites, in light, oxidising process just needs 4-60h, and carries out hot pressed sintering at reducing atmosphere condition, and required operation is many, and the time is long.
Accompanying drawing explanation
Fig. 1 is copper-molybdenum-carbon material surface SEM photo of embodiment 1 preparation.
Fig. 2 is copper-molybdenum-carbon material TEM photo of embodiment 1 preparation.
Embodiment
Below by preferred embodiment, technical scheme of the present invention is described further, but should not be understood as limiting the scope of the invention.
Embodiment 1:
Copper ingot material and graphite ingot are put into crucible, and put 200g molybdenum on graphite ingot, on copper ingot material, put 5g CaF
2; Shut vacuum chamber, start to vacuumize; Start wheelwork substrate is rotated with the speed of 6rpm, and open substrate heating equipment, heated substrates temperature makes it to be stabilized in 650 ℃; When vacuum tightness reaches 3 * 10
-2during Pa, open baffle plate, electron beam gun, layer deposited isolating CaF
2; With line size 1.5A Heated Copper ingot, with line size 1.5A heating graphite ingot, start deposition material, after deposition 50min, close electron beam gun, pull on baffle plate, close heating unit, close substrate rotating device; When substrate temperature drops to below 200 ℃, close vacuum system, take off substrate, separated thickness 0.26mm, the sheet material of diameter 520mm of obtaining.Preparation sheet material composition be Cu-Mo1.3wt%-C0.086wt%, according to standard GB/T/T228.1-2010 to the finished product are carried out to Mechanics Performance Testing, its yield strength R
p0.2=426MPa, tensile strength Rm=480MPa.With four probe method, the specific conductivity of material is detected, its specific conductivity is 82%IACS.Copper-molybdenum carbon composite copper matrix grain of preparation is of a size of 5-10 μ m(and sees Fig. 1), second-phase is Mo
2c, mean sizes is about 5nm(and sees Fig. 2).
Embodiment 2:
Copper ingot material, molybdenum ingot and anthracene powder are put into respectively to crucible, and put 5g CaF on copper ingot material
2; Shut vacuum chamber, start to vacuumize; Start wheelwork substrate is rotated with the speed of 15rpm, and open substrate heating equipment, heated substrates temperature makes it to be stabilized in 750 ℃; When vacuum tightness reaches 3 * 10
-2during Pa, open baffle plate, electron beam gun, layer deposited isolating CaF
2; With line size 2.2A Heated Copper ingot, with line size 2.6A heating molybdenum ingot, with line size 0.6A heating anthracene powder, start deposition material, after deposition 30min, close electron beam gun, pull on baffle plate, close heating unit, close substrate rotating device; When substrate temperature drops to below 200 ℃, close vacuum system, take off substrate, separated thickness 0.3mm, the sheet material of diameter 520mm of obtaining.Preparation sheet material composition be Cu-Mo15wt%-C0.2wt%, according to standard GB/T/T228.1-2010 to the finished product are carried out to Mechanics Performance Testing, its yield strength R
p0.2=540MPa, tensile strength Rm=600MPa.With four probe method, the specific conductivity of material is detected, its specific conductivity is 70%IACS.Preparation state material matrix grain-size is 1-5 μ m, and Second Phase Particle is that Mo(mean sizes is 180nm), Mo
2c(mean sizes is 20nm).
Embodiment 3:
Copper ingot material, molybdenum ingot and anthracene powder are put into respectively to crucible, and put 5g ZrO on copper ingot material
2; Shut vacuum chamber, start to vacuumize; Start wheelwork substrate is rotated with the speed of 8rpm, and open substrate heating equipment, heated substrates temperature makes it to be stabilized in 650 ℃; When vacuum tightness reaches 3 * 10
-2during Pa, open baffle plate, electron beam gun, layer deposited isolating ZrO
2; With line size 2.2A Heated Copper ingot, with line size 2.0A heating molybdenum ingot, with line size 1A heating anthracene powder, start deposition material, after deposition 40min, close electron beam gun, pull on baffle plate, close heating unit, close substrate rotating device; When substrate temperature drops to below 200 ℃, close vacuum system, take off substrate, separated thickness 0.38mm, the sheet material of diameter 520mm of obtaining.The sheet material composition of preparation is Cu-Mo0.2wt%-C1wt%, according to standard GB/T/T228.1-2010, the finished product is carried out to Mechanics Performance Testing, its yield strength R
p0.2=440MPa, tensile strength Rm=500MPa.With four probe method, the specific conductivity of material is detected, its specific conductivity is 80%IACS.Preparation state material matrix grain-size is 1-5 μ m, and Second Phase Particle is that C(mean sizes is 16nm), Mo
2c(mean sizes is 20nm).
Claims (6)
1. the Cu-base composites of a nano-particle reinforcement, it is characterized in that: in described Cu-base composites, copper matrix grain size is less than 20 μ m, and nano-particle reinforcement is molybdenum carbide or molybdenum carbide and molybdenum or molybdenum carbide and carbon mutually, and the particle size of nano-particle reinforcement phase is below 200nm; In described Cu-base composites, the quality percentage composition of Mo is 0.1-15%, and the quality percentage composition of C is below 1%.
2. the Cu-base composites of nano-particle reinforcement according to claim 1, is characterized in that the performance index of described Cu-base composites are as follows: yield strength R
p0.2>=420MPa, tensile strength Rm>=480MPa, specific conductivity>=70%ICAS.
3. the preparation method of the Cu-base composites of nano-particle reinforcement according to claim 1, comprises the steps:
(1) a kind of in copper ingot material and molybdenum source, carbon source or two kinds are put in crucible respectively, and put isolating layer material on copper ingot material;
(2) vacuumize heated substrates;
(3) when vacuum tightness reaches 9 * 10
-2pa is following, substrate temperature reaches 500-800 ℃, opens substrate rotating device, makes substrate rotation, layer deposited isolating;
(4) open baffle plate, start deposition material;
(5) deposited, after substrate is cooling, taken off substrate, separation obtains settled layer material, is the Cu-base composites of nano-particle reinforcement.
4. the preparation method of the Cu-base composites of nano-particle reinforcement according to claim 3, is characterized in that: carbon source is carbon target, or carbon dust, or anthracene powder.
5. the preparation method of the Cu-base composites of nano-particle reinforcement according to claim 3, is characterized in that: isolating layer material is selected from CaF
2or ZrO
2.
6. the preparation method of the Cu-base composites of nano-particle reinforcement according to claim 6, is characterized in that: in deposition process, substrate rotating speed is controlled at 3-20rev/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310632642.9A CN103643075B (en) | 2013-11-29 | 2013-11-29 | Cu-base composites of nano-particle reinforcement and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310632642.9A CN103643075B (en) | 2013-11-29 | 2013-11-29 | Cu-base composites of nano-particle reinforcement and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103643075A true CN103643075A (en) | 2014-03-19 |
| CN103643075B CN103643075B (en) | 2016-01-20 |
Family
ID=50248355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310632642.9A Active CN103643075B (en) | 2013-11-29 | 2013-11-29 | Cu-base composites of nano-particle reinforcement and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103643075B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946923A (en) * | 2015-06-30 | 2015-09-30 | 浙江工业大学 | Copper-based composite material and preparation method thereof |
| CN112846570A (en) * | 2020-12-31 | 2021-05-28 | 松山湖材料实验室 | Nano welding flux and preparation method thereof, device and welding method |
| CN112846563A (en) * | 2020-12-31 | 2021-05-28 | 松山湖材料实验室 | Solder paste, method for preparing same, device and soldering method |
| CN114293051A (en) * | 2021-12-23 | 2022-04-08 | 北京科大京都高新技术有限公司 | Preparation method of high-temperature softening resistant high-strength high-conductivity copper-based composite material formed part |
| CN115612890A (en) * | 2022-11-03 | 2023-01-17 | 中南大学 | Mo 2 C particle reinforced CuCrZr composite material and preparation process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1150172A (en) * | 1997-07-29 | 1999-02-23 | Yazaki Corp | Carbide-dispersion strengthened copper alloy material |
| JP2008223091A (en) * | 2007-03-13 | 2008-09-25 | Komatsu Ltd | Electrode for welding, and method for producing the same |
| CN102400006A (en) * | 2010-09-16 | 2012-04-04 | 北京有色金属研究总院 | Foamy carbon/copper matrix or aluminum matrix composite material and preparation method thereof |
-
2013
- 2013-11-29 CN CN201310632642.9A patent/CN103643075B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1150172A (en) * | 1997-07-29 | 1999-02-23 | Yazaki Corp | Carbide-dispersion strengthened copper alloy material |
| JP2008223091A (en) * | 2007-03-13 | 2008-09-25 | Komatsu Ltd | Electrode for welding, and method for producing the same |
| CN102400006A (en) * | 2010-09-16 | 2012-04-04 | 北京有色金属研究总院 | Foamy carbon/copper matrix or aluminum matrix composite material and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946923A (en) * | 2015-06-30 | 2015-09-30 | 浙江工业大学 | Copper-based composite material and preparation method thereof |
| CN104946923B (en) * | 2015-06-30 | 2017-02-01 | 浙江工业大学 | Copper-based composite material and preparation method thereof |
| CN112846570A (en) * | 2020-12-31 | 2021-05-28 | 松山湖材料实验室 | Nano welding flux and preparation method thereof, device and welding method |
| CN112846563A (en) * | 2020-12-31 | 2021-05-28 | 松山湖材料实验室 | Solder paste, method for preparing same, device and soldering method |
| CN112846570B (en) * | 2020-12-31 | 2022-08-16 | 松山湖材料实验室 | Nano welding flux and preparation method thereof, device and welding method |
| CN114293051A (en) * | 2021-12-23 | 2022-04-08 | 北京科大京都高新技术有限公司 | Preparation method of high-temperature softening resistant high-strength high-conductivity copper-based composite material formed part |
| CN114293051B (en) * | 2021-12-23 | 2022-07-26 | 北京科大京都高新技术有限公司 | Preparation method of high-temperature softening resistant high-strength high-conductivity copper-based composite material formed part |
| CN115612890A (en) * | 2022-11-03 | 2023-01-17 | 中南大学 | Mo 2 C particle reinforced CuCrZr composite material and preparation process thereof |
| CN115612890B (en) * | 2022-11-03 | 2024-01-19 | 中南大学 | Mo (molybdenum) 2 C particle reinforced CuCrZr composite material and preparation process thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103643075B (en) | 2016-01-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103643075B (en) | Cu-base composites of nano-particle reinforcement and preparation method thereof | |
| Wang et al. | Enhanced thermal conductivity in Cu/diamond composites by tailoring the thickness of interfacial TiC layer | |
| JP5413540B2 (en) | MgO target for sputtering | |
| Mondin et al. | Metal deposition by electroless plating on polydopamine functionalized micro-and nanoparticles | |
| CN112553500B (en) | Method for simultaneously improving strength and conductivity of Cu-Cr-Nb alloy | |
| CN106735249B (en) | A kind of niobium based composites and preparation method | |
| Huang et al. | Effects of TiN nanoparticles on the microstructure and properties of W–30Cu composites prepared via electroless plating and powder metallurgy | |
| CN102965619A (en) | Preparation method of multi-metal doping hydrogen-free diamond carbon film | |
| CN113070471A (en) | Preparation method of titanium-graphene composite material with strong plasticity matching | |
| Luo et al. | Fabrication of W–Cu/La2O3 composite powder with a novel pretreatment prepared by electroless plating and its sintering characterization | |
| CN109811177A (en) | A kind of preparation method of highly conductive high-intensitive silver-graphene composite material | |
| CN114293158B (en) | Preparation method of tungsten-silicon alloy target | |
| WO2008071068A1 (en) | Cladding process of metal micro/nano-particle | |
| Zhan et al. | Preparation and mechanism of Cu/GO/Cu laminated composite foils with improved thermal conductivity and mechanical property by architectural design | |
| WO2018113717A1 (en) | Method for preparing neodymium-iron-boron permanent magnetic material | |
| CN109554564B (en) | Preparation method of amorphous alloy particle and carbon nano tube reinforced aluminum matrix composite material | |
| CN114054762A (en) | Graphene/metal matrix composite material preparation method based on graphene defect regulation | |
| CN108788134A (en) | A kind of preparation method of graphene-nanometer pltine core-shell structural conductive material | |
| CN104946923B (en) | Copper-based composite material and preparation method thereof | |
| Biyik | Effect of Y2O3 addition and milling time on the synthesis of nanocrystalline Ag–ZnO composite powder via mechanical alloying | |
| CN103628032A (en) | Method of preparing nano titanium nitride layer on conductive base body material | |
| CN113996782B (en) | Composite material of graphene coated copper powder and preparation method thereof | |
| Zhou et al. | The effect of surface coating treatment on the properties of carbon nanotube reinforced copper matrix composites | |
| Winnicki et al. | Microscopic examination of cold spray cermet Sn+ In2O3 coatings for sputtering target materials | |
| CN109468619B (en) | Carbon nanotube surface plating method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191225 Address after: No. 88, Yungang section, Dushan Port Town, Pinghu City, Jiaxing City, Zhejiang Province Patentee after: Pinghu xinchengfa Hardware Machinery Co.,Ltd. Address before: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee before: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Effective date of registration: 20191225 Address after: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee after: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Address before: 310014 Hangzhou city in the lower reaches of the city of Zhejiang Wang Road, No. 18 Patentee before: Zhejiang University of Technology |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210709 Address after: Room 503, building 3, No. 133, development avenue, Tongxiang Economic Development Zone, Tongxiang City, Jiaxing City, Zhejiang Province Patentee after: ZHEJIANG MAIZHI NETWORK TECHNOLOGY Co.,Ltd. Address before: 314200 No.88, Yungang section, dushangang Town, Pinghu City, Jiaxing City, Zhejiang Province Patentee before: Pinghu xinchengfa Hardware Machinery Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221230 Address after: No. 545, Xinxing Community, Puyuan Town, Tongxiang City, Jiaxing City, Zhejiang Province, 314500 Patentee after: Jiaxing Yanzhi Network Technology Co.,Ltd. Address before: Room 503, building 3, No. 133, development avenue, Tongxiang Economic Development Zone, Tongxiang City, Jiaxing City, Zhejiang Province Patentee before: ZHEJIANG MAIZHI NETWORK TECHNOLOGY CO.,LTD. |
|
| TR01 | Transfer of patent right |