CN104213009A - Method for cladding copper on surface of infiltration sintered tungsten-copper composite material - Google Patents
Method for cladding copper on surface of infiltration sintered tungsten-copper composite material Download PDFInfo
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Abstract
The invention discloses a method for cladding copper on a surface of an infiltration sintered tungsten-copper composite material. The method comprises the following steps: a mixture of tungsten powder and copper powder is prepared, wherein the content of the tungsten powder is 65-85 weight%, and the content of the copper powder is 15-35 weight%; after the prepared mixture is added to forming agent, and is dried for pelletizing through spraying, the prepared mixture is compressed for forming in a mold to obtain a tungsten skeleton pressing blank, wherein the pressing pressure is 150-400 MPa; oxygen-free copper is pressed into a copper bar serving as sintering infiltration agent; the sintering infiltration agent is stacked on the tungsten skeleton pressing blank, then the sintering infiltration agent and the tungsten skeleton pressing blank are put in a graphite mold, and are sintered in a vacuum furnace to obtain the tungsten-copper composite material; the tungsten-copper composite material consists of a tungsten-copper alloy layer and a copper layer; and the copper layer covers the surface of the tungsten-copper alloy. The infiltration density of the tungsten-copper composite material is raised to more than 99% to totally satisfy the requirements of some special equipment parts, so that the service life of the special equipment is greatly prolonged.
Description
Technical field
The present invention relates to a kind of preparation method of tungsten-copper composite material, particularly relate to a kind of method of being produced tungsten-copper composite material by melting infiltration sintering method.
Background technology
The metallurgical matrix material of tungsten copper powder is by high-melting-point, the tungsten of high rigidity and high connductivity, the pseudoalloy that the copper of high thermal conductivity is formed, because it has good resistance to arc erosion, resistance fusion welding and high strength, the advantages such as high rigidity, be widely used as electrical contact material at present, resistance welding, electrospark machining and plasma electrode material, electrical heating alloys and heavy metal, the military project material of special purpose is (as rocket nozzle, aircraft larynx serves as a contrast), and computer central processing system, the lead frame of large-scale integrated circuit, the heat sink substrate of the electron devices such as solid state microwave pipe.
Publication number is CN1995438, publication date is that the Chinese invention patent application on July 11st, 2007 discloses one to prepare copper be 25wt% ~ 40wt%, surplus is the method for the high copper content tungsten-copper alloy of tungsten, adopt 5wt% ~ 20wt%, purity >=99.5%, granularity is the copper powder of 15 μm ~ 20 μm, and with the tungsten in described tungsten-copper alloy, there is equal in quality per-cent, purity >=99%, granularity is 3 ~ 6 μm of tungsten powders, compression molding after Homogeneous phase mixing, the pressed compact presintering that porosity λ controls 35% ± 2% obtains tungsten-copper alloy skeleton, copper amount is oozed in calculating, by purity >=99.5%, the copper powder of granularity <76um is molded into the copper sheet measure-alike with skeleton surface and is placed on tungsten-copper alloy skeleton, load in plumbago crucible, carry out intensification after adopting aluminum oxide landfill and ooze copper, the high copper content tungsten-copper alloy obtained, conductive performance is excellent, is suitable for electrical contact and electrode materials, electronic package material, high temperature transpiring material etc.
Publication number is CN103409676A, publication date is that the Chinese invention patent application on November 27th, 2013 discloses a kind of method improving heat conductivity of tungsten copper alloy, comprise the steps: step, adopt tungsten-copper alloy prepared by powder metallurgic method, wherein the massfraction of tungsten is 80-85%, and all the other are copper; Step 2, tungsten-copper alloy powder metallurgic method prepared carries out ultra-high voltage thermal treatment, and the pressure of ultra-high voltage is 3.0-5.0GPa, and under ultra-high voltage, Heating temperature is 820-900 DEG C, insulation 20-30min, and naturally cools to room temperature under ultra-high voltage; Step 3, is heated to 450-550 DEG C, ageing treatment 90-120min by the normal pressure resistance furnace that nitrogen protection put into by the alloy material after above-mentioned ultra-high voltage thermal treatment, naturally cools to room temperature.The problem that tungsten-copper alloy density is not high, heat conductivility is lower that this invention is prepared for powder metallurgic method, main employing ultra-high voltage thermal treatment process, exploitativeness is strong, and technique is simple, and steady quality, can improve heat conductivity of tungsten copper alloy by a relatively large margin.
But the tungsten-copper alloy infiltration density that foregoing invention patent application is produced is generally 97% ~ 98% of theoretical density, can not more than 98% be reached, and tungsten-copper alloy infiltration density is higher, its performance is more superior, during especially for rocket nozzle or aircraft larynx lining, need the tungsten-copper alloy of higher infiltration density, the space that infiltration density is also improved.
Above-mentioned production technique needs ultra-high voltage and needs nitrogen protection, and make whole production technique wayward, and production cost is higher, consuming time longer, production efficiency is lower.
The tungsten-copper alloy produced is because the content of tungsten is higher than the content of copper, and when welding, its welding property is poor.
Summary of the invention
In order to overcome the defect that above-mentioned existing tungsten-copper alloy infiltration density can not reach more than 98%, the invention provides the method that copper is covered on a kind of melting infiltration sintering tungsten-copper composite material surface, the present invention by covering the method for copper on melting infiltration sintering tungsten-copper composite material, the infiltration density of tungsten-copper composite material is brought up to more than 99%, meet the requirement of some specific installation parts (such as rocket nozzle or aircraft larynx serve as a contrast) completely, greatly extend the work-ing life of these specific installations.
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, it is characterized in that: comprise following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 65-85%, and the content of copper powder is 15-35%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 150 ~ 400MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1000 DEG C-1500 DEG C, and sintering time is 50min-75min, and the thickness of the layers of copper obtained is 0.3 ~ 5mm.
In step 4, the temperature of vacuum oven is 1250 DEG C, and sintering time is 60min, and the thickness of the layers of copper obtained is 0.3 ~ 5mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.The add-on of polyvinyl alcohol is the wt10% of tungsten powder, refers to be the weight of the polyvinyl alcohol added be 10% of tungsten powder weight.
Compared with prior art, the present invention has following beneficial effect:
The present invention includes following processing step: tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 65-85%, and the content of copper powder is 15-35%; After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 150 ~ 400MPa, obtains W skeleton pressed compact; Oxygen free copper is struck out copper bar as sintering and infiltration agent; Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.Anaerobic copper bar is placed on W skeleton pressed compact as sintering and infiltration agent by the present invention, during sintering, oxygen free copper melts slowly as sintering and infiltration agent, then by the kapillary infiltration in W skeleton pressed compact in W skeleton pressed compact, when infiltration, have enough infiltration of copper in W skeleton pressed compact, and in W skeleton pressed compact, the content of tungsten powder is 65-85%, the content of copper powder is 15-35%, is convenient to the infiltration of copper by the W skeleton pressed compact formed after the compacting of 150 ~ 400MPa pressure.Oxygen free copper part infiltration is to W skeleton pressed compact, and another part covers on W skeleton pressed compact, and after sintering, do not have the anaerobic copper bar melted to cover on W skeleton pressed compact firmly, the layers of copper of formation can increase welding property.
The present invention is in step 4, and the temperature of vacuum oven is 1000 DEG C-1500 DEG C, and sintering time is 50min-75min, and the thickness of the layers of copper obtained is 0.3 ~ 5mm.To the control of vacuum oven temperature and time, mainly in order to fully ensure copper can infiltration in W skeleton pressed compact, improve the infiltration density of tungsten-copper composite material, and the major cause that the present invention can allow the infiltration density of tungsten-copper composite material reach more than 99% is also to allow copper fully in W skeleton pressed compact, can also strengthen the welding property of tungsten-copper composite material by infiltration simultaneously.
Embodiment
Embodiment 1
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, comprises following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 65%, and the content of copper powder is 35%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 320MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1200 DEG C, and sintering time is 55min, and the thickness of the layers of copper obtained is 0.8mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.
Sinter and cover copper and once complete, the relative density of product reaches 99% after testing.
Embodiment 2
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, comprises following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 70%, and the content of copper powder is 30%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 150MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1000 DEG C, and sintering time is 60min, and the thickness of the layers of copper obtained is 1.2mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.
Sinter and cover copper and once complete, the relative density of product reaches 99.5% after testing.
Embodiment 3
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, comprises following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 75%, and the content of copper powder is 25%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 400MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1500 DEG C, and sintering time is 50min, and the thickness of the layers of copper obtained is 1.4mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.
Sinter and cover copper and once complete, the relative density of product reaches 99% after testing.
Embodiment 4
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, comprises following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 80%, and the content of copper powder is 20%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 300MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1250 DEG C, and sintering time is 60min, and the thickness of the layers of copper obtained is 2.3mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.
Sinter and cover copper and once complete, the relative density of product reaches 99.8% after testing.
Embodiment 5
A method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, comprises following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 85%, and the content of copper powder is 15%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 380MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
In step 4, the temperature of vacuum oven is 1500 DEG C, and sintering time is 75min, and the thickness of the layers of copper obtained is 1.0mm.
Described binder is polyvinyl alcohol, and the add-on of polyvinyl alcohol is the wt10% of tungsten powder.
Sinter and cover copper and once complete, the relative density of product reaches 99.2% after testing.
Claims (4)
1. a method for copper is covered on melting infiltration sintering tungsten-copper composite material surface, it is characterized in that: comprise following processing step:
Step one, the compound of preparation tungsten powder and copper powder
Tungsten powder and copper powder are mixed, in the compound obtained, by weight percentage, wherein the content of tungsten powder is 65-85%, and the content of copper powder is 15-35%;
Step 2, prepares W skeleton pressed compact
After the compound that step one is obtained is added the spray-dried granulation of binder, press forming in a mold, pressing pressure 150 ~ 400MPa, obtains W skeleton pressed compact;
Step 3, prepares sintering and infiltration agent
Oxygen free copper is struck out copper bar as sintering and infiltration agent;
Step 4, sintering
Sintering and infiltration agent overlayed after above W skeleton pressed compact and put into graphite jig, then sinter in a vacuum furnace, obtain tungsten-copper composite material, this tungsten-copper composite material is made up of tungsten-copper alloy layer and layers of copper, and layers of copper covers on the surface of tungsten-copper alloy.
2. the method for copper is covered on a kind of melting infiltration sintering tungsten-copper composite material surface according to claim 1, it is characterized in that: in step 4, the temperature of vacuum oven is 1000 DEG C-1500 DEG C, and sintering time is 50min-75min, and the thickness of the layers of copper obtained is 0.3 ~ 5mm.
3. the method for copper is covered on a kind of melting infiltration sintering tungsten-copper composite material surface according to claim 1, and it is characterized in that: in step 4, the temperature of vacuum oven is 1250 DEG C, and sintering time is 60min, and the thickness of the layers of copper obtained is 0.3 ~ 5mm.
4. the method for copper is covered on a kind of melting infiltration sintering tungsten-copper composite material surface according to claim 1,2 or 3, and it is characterized in that: described binder is polyvinyl alcohol, the add-on of polyvinyl alcohol is the wt10% of tungsten powder; The add-on of polyvinyl alcohol is the wt10% of tungsten powder, refers to be the weight of the polyvinyl alcohol added be 10% of tungsten powder weight.
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| CN105568209A (en) * | 2016-03-04 | 2016-05-11 | 西安理工大学 | In-situ formation preparation method for gradient WC-strengthened CuW composite material |
| CN106180654A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for infiltration copper-chromium contact material |
| CN106180653A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for copper tungsten contact material |
| CN107498047A (en) * | 2017-09-01 | 2017-12-22 | 西北有色金属研究院 | A kind of tungsten-copper composite material and preparation method thereof |
| KR20180086629A (en) * | 2017-01-23 | 2018-08-01 | (주)메탈라이프 | Manufacturing method of tungsten-copper clad alloy and clad alloy using the same |
| CN109371356A (en) * | 2018-12-14 | 2019-02-22 | 北京九土科技有限公司 | A kind of infiltration copper product seeping process for copper and its preparation and application |
| CN109609792A (en) * | 2018-12-17 | 2019-04-12 | 河源市凯源硬质合金有限公司 | A method of preparing tungsten-copper alloy |
| CN111250720A (en) * | 2020-03-02 | 2020-06-09 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111299594A (en) * | 2019-11-29 | 2020-06-19 | 安徽恒均粉末冶金科技股份有限公司 | Preparation method of copper-tungsten petal contact |
| CN111889674A (en) * | 2020-08-13 | 2020-11-06 | 山东威尔斯通钨业有限公司 | Preparation method for one-step sintering molding of tungsten copper and copper combined part |
| CN112872356A (en) * | 2021-05-06 | 2021-06-01 | 陕西斯瑞新材料股份有限公司 | Method for improving strength of copper-tungsten and copper bonding surface |
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| CN113921310A (en) * | 2021-11-01 | 2022-01-11 | 西安西电高压开关有限责任公司 | Process manufacturing method of high-performance arc contact |
| CN114000023A (en) * | 2021-09-18 | 2022-02-01 | 西安理工大学 | Method for preparing molybdenum-copper composite material by using gas pressure infiltration sintering |
| CN114231812A (en) * | 2021-12-21 | 2022-03-25 | 合肥工业大学 | AlN-W-Cu composite material and preparation method thereof |
| CN115522090A (en) * | 2021-10-29 | 2022-12-27 | 山东威尔斯通钨业有限公司 | Method and treatment equipment for coating copper on surface of tungsten carbide copper composite material |
| CN116475422A (en) * | 2023-05-19 | 2023-07-25 | 福建国福中亚电气机械有限公司 | Preparation method and equipment of copper-tungsten alloy electrical contact |
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| CN105568209A (en) * | 2016-03-04 | 2016-05-11 | 西安理工大学 | In-situ formation preparation method for gradient WC-strengthened CuW composite material |
| CN106180654A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for infiltration copper-chromium contact material |
| CN106180653A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for copper tungsten contact material |
| CN106180653B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares copper tungsten contact material |
| CN106180654B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares infiltration copper-chromium contact material |
| KR101890396B1 (en) * | 2017-01-23 | 2018-08-21 | (주)메탈라이프 | Manufacturing method of tungsten-copper clad alloy and clad alloy using the same |
| KR20180086629A (en) * | 2017-01-23 | 2018-08-01 | (주)메탈라이프 | Manufacturing method of tungsten-copper clad alloy and clad alloy using the same |
| CN107498047A (en) * | 2017-09-01 | 2017-12-22 | 西北有色金属研究院 | A kind of tungsten-copper composite material and preparation method thereof |
| CN109371356A (en) * | 2018-12-14 | 2019-02-22 | 北京九土科技有限公司 | A kind of infiltration copper product seeping process for copper and its preparation and application |
| CN109609792A (en) * | 2018-12-17 | 2019-04-12 | 河源市凯源硬质合金有限公司 | A method of preparing tungsten-copper alloy |
| CN111299594A (en) * | 2019-11-29 | 2020-06-19 | 安徽恒均粉末冶金科技股份有限公司 | Preparation method of copper-tungsten petal contact |
| CN111250720A (en) * | 2020-03-02 | 2020-06-09 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111250720B (en) * | 2020-03-02 | 2023-02-28 | 合肥尚德新材料有限公司 | Method for preparing tungsten-copper composite material |
| CN111889674A (en) * | 2020-08-13 | 2020-11-06 | 山东威尔斯通钨业有限公司 | Preparation method for one-step sintering molding of tungsten copper and copper combined part |
| CN112872356B (en) * | 2021-05-06 | 2021-07-23 | 陕西斯瑞新材料股份有限公司 | Method for improving strength of copper-tungsten and copper bonding surface |
| CN112872356A (en) * | 2021-05-06 | 2021-06-01 | 陕西斯瑞新材料股份有限公司 | Method for improving strength of copper-tungsten and copper bonding surface |
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| CN114000023A (en) * | 2021-09-18 | 2022-02-01 | 西安理工大学 | Method for preparing molybdenum-copper composite material by using gas pressure infiltration sintering |
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