CN107236876B - A kind of preparation method of high compactness high thermal conductivity Tungsten-copper Composites - Google Patents
A kind of preparation method of high compactness high thermal conductivity Tungsten-copper Composites Download PDFInfo
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- CN107236876B CN107236876B CN201710404443.0A CN201710404443A CN107236876B CN 107236876 B CN107236876 B CN 107236876B CN 201710404443 A CN201710404443 A CN 201710404443A CN 107236876 B CN107236876 B CN 107236876B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1031—Alloys containing non-metals starting from gaseous compounds or vapours of at least one of the constituents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1094—Alloys containing non-metals comprising an after-treatment
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Abstract
The invention discloses a kind of preparation methods of high compactness high thermal conductivity Tungsten-copper Composites, comprising: one, tungsten powder is placed in hydrogen furnace restores；Two, using copper target as sputtering target material, magnetron sputtering is carried out to the tungsten powder after reduction, obtains composite material；Three, composite material is placed in hot pressed sintering and then natural cooling in hot pressing furnace, obtains presoma；Four, precursor is placed in chemical vapor deposition stove, using the mixed gas of methane and vapor as reaction gas, chemical vapor deposition is carried out to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites.The thermal conductivity for the Tungsten-copper Composites for using the method for the present invention to prepare is 220W/mK~300W/mK, and compactness is greater than 98%, and tensile strength is 680MPa~692MPa, and thermal expansion coefficient is 4.3 × 10‑6/ K~4.7 × 10‑6/ K, hardness are 180HV~186HV.
Description
Technical field
The invention belongs to tungsten-copper composite material preparation technical fields, and in particular to a kind of high compactness high thermal conductivity Tungsten-copper Composites
Preparation method.
Background technique
Tungsten-copper composite material by tungsten and high-ductility, electric-conductivity heat-conductivity high with high-melting-point, high rigidity metallic copper
It is formed；Since tungsten copper two-phase is immiscible, therefore the two belongs to pseudo-alloy again.This, which makes it both, has the characteristics that tungsten and copper respectively,
As having high-intensitive and hardness, high electrical and thermal conductivity, good electrical erosion resistance, good ray absorption capacity (ratio at high temperature
High 30%~40%) of lead, low thermal expansion coefficient (only the 1/2~1/3 of steel and iron) and certain plasticity (15%) etc.；And
Its mechanical and physical property can also be changed, by changing the relative amount of tungsten copper two-phase in composite material to reach required zero
The specific requirement of part.In addition to this, it also have two be combined and the new performance that generates, such as in the sufficiently high environment of temperature
In, the copper in composite material, which is met, to be generated evaporation and absorbs heat, and part can be produced from cooling effect.Therefore, it can be used extensively
In various industries such as aerospace, defence and military, electronic information, metallurgy and machinings, occupy in national economy very heavy
The status wanted.
The high-compactness of material is the premise for guaranteeing its excellent properties, but since tungsten copper two-phase is immiscible, formation is
A kind of typical pseudo-alloy, therefore the preparation of this composite material can only pass through the method for powder metallurgy.But pass through traditional powder
The consistency of composite material obtained by last sintering method is relatively low (95% or less).By the unremitting effort of various countries researcher,
The method for having invented the fine and close tungsten-copper composite material of a variety of preparations, such as: the molten infiltration method of liquid phase, lqiuid phase sintering method activate liquid-phase sintering
Method.Although solving compactness defect to a certain degree, since liquid copper is in the intergranular poor fluidity of tungsten,
The compactness of tungsten-copper alloy is not still high, causes its mechanicalness and thermal conductivity lower.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing, a kind of high compactness is high
The preparation method of thermally conductive Tungsten-copper Composites.This method uses copper target magnetron sputtering tungsten powder, obtains the tungsten powder of copper clad, hot pressed sintering at
Chemical vapor deposition is carried out after presoma, strong using the mobility of gas, reaction gas can be flow in the hole of presoma
And it is cracked to form carbon nanotube, so that the compactness and thermal conductivity of composite material are increased, the tungsten copper material prepared using this method
The thermal conductivity of material is 220W/mK~300W/mK, and compactness is greater than 98%, and tensile strength is 680MPa~692MPa, and heat is swollen
Swollen coefficient is 4.3 × 10-6/ K~4.7 × 10-6/ K, hardness are 180HV~186HV.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of high compactness high thermal conductivity Tungsten-copper Composites
Preparation method, which is characterized in that the high compactness refer to Tungsten-copper Composites compactness be greater than 98%, the high thermal conductivity refers to
The thermal conductivity of Tungsten-copper Composites is 220W/mK~300W/mK；
The preparation method comprises the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 1.0Pa~9.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, magnetic
Induction is 0.2T~0.3T, and the time of magnetron sputtering is 30min~60min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1500 DEG C~
1600 DEG C, pressure is hot pressed sintering 30min~60min under conditions of 10 tons~15 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites.
The preparation method of above-mentioned a kind of high compactness high thermal conductivity Tungsten-copper Composites, which is characterized in that described in step 1 also
Former temperature is 1200 DEG C~1500 DEG C, and the time is 30min~90min, and hydrogen flowing quantity is 30cc/min~50cc/min.
A kind of preparation method of above-mentioned high compactness high thermal conductivity Tungsten-copper Composites, which is characterized in that argon described in step 2
The volumn concentration of argon gas is 80%~90% in the mixed gas of gas and hydrogen chloride, and surplus is hydrogen chloride gas.
A kind of preparation method of above-mentioned high compactness high thermal conductivity Tungsten-copper Composites, which is characterized in that first described in step 4
The volumn concentration of methane is 70%~90% in the mixed gas of alkane and vapor, and surplus is vapor, and gas flow is
60cc/min~90cc/min, the temperature of chemical vapor deposition are 600 DEG C~800 DEG C, and the time is 10min~30min.
Compared with the prior art, the present invention has the following advantages:
1, the present invention uses copper target magnetron sputtering tungsten powder, the tungsten powder of copper clad is obtained, after then hot pressed sintering is at presoma
Chemical vapor deposition is carried out, strong using the mobility of gas, reaction gas can flow in the hole of presoma and crack life
At carbon nanotube, the theoretical thermal conductivity of carbon nanotube can achieve 3600W/mK, and thermal expansion coefficient is 5.4 × l0-6/ K, from
And increase the compactness and thermal conductivity of composite material.
2, the compactness of the Tungsten-copper Composites prepared using method of the invention is greater than 98%, thermal conductivity be 220W/mK~
300W/mK, thermal expansion coefficient are 4.3 × 10-6/ K~4.7 × 10-6/ K, tensile strength are 680MPa~692MPa, and hardness is
180HV~186HV.
Below by embodiment, technical scheme of the present invention will be described in further detail.
Specific embodiment
Embodiment 1
The preparation method of the Tungsten-copper Composites of the present embodiment, comprising the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；The temperature of the reduction is
1200 DEG C, time 30min, hydrogen flowing quantity 30cc/min；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 1.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, mixed gas
The volumn concentration of middle argon gas is 80%, and surplus is hydrogen chloride gas, and the magnetic induction intensity of magnetron sputtering is 0.2T, and the time is
30min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1500 DEG C,
Pressure is hot pressed sintering 30min under conditions of 10 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and
The volumn concentration of methane is 70% in the mixed gas of vapor, and surplus is vapor, and gas flow 60cc/min changes
The temperature for learning vapor deposition is 600 DEG C, time 10min.
The compactness of Tungsten-copper Composites manufactured in the present embodiment is 98.4%, thermal conductivity 220W/mK, and thermal expansion coefficient is
4.3×10-6/ K, tensile strength 680MPa, hardness 180HV.
Embodiment 2
The preparation method of the Tungsten-copper Composites of the present embodiment, comprising the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；The temperature of the reduction is
1300 DEG C, time 60min, hydrogen flowing quantity 40cc/min；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 3.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, mixed gas
The volumn concentration of middle argon gas is 85%, and surplus is hydrogen chloride gas, and the magnetic induction intensity of magnetron sputtering is 0.25T, time
For 40min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1550 DEG C,
Pressure is hot pressed sintering 40min under conditions of 12 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and
The volumn concentration of methane is 80% in the mixed gas of vapor, and surplus is vapor, and gas flow 70cc/min changes
The temperature for learning vapor deposition is 700 DEG C, time 20min.
The compactness of Tungsten-copper Composites manufactured in the present embodiment is 98.3%, thermal conductivity 260W/mK, and thermal expansion coefficient is
4.7×10-6/ K, tensile strength 692MPa, hardness 182HV.
Embodiment 3
The preparation method of the Tungsten-copper Composites of the present embodiment, comprising the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；The temperature of the reduction is
1500 DEG C, time 90min, hydrogen flowing quantity 50cc/min；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 9.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, mixed gas
The volumn concentration of middle argon gas is 90%, and surplus is hydrogen chloride gas, and the magnetic induction intensity of magnetron sputtering is 0.3T, and the time is
60min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1600 DEG C,
Pressure is hot pressed sintering 60min under conditions of 15 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and
The volumn concentration of methane is 90% in the mixed gas of vapor, and surplus is vapor, and gas flow 90cc/min changes
The temperature for learning vapor deposition is 800 DEG C, time 30min.
The compactness of Tungsten-copper Composites manufactured in the present embodiment is 98.8%, thermal conductivity 300W/mK, and thermal expansion coefficient is
4.3×10-6/ K, tensile strength 690MPa, hardness 186HV.
Embodiment 4
The preparation method of the Tungsten-copper Composites of the present embodiment, comprising the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；The temperature of the reduction is
1400 DEG C, time 70min, hydrogen flowing quantity 35cc/min；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 5.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, mixed gas
The volumn concentration of middle argon gas is 80%, and surplus is hydrogen chloride gas, and the magnetic induction intensity of magnetron sputtering is 0.3T, and the time is
50min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1600 DEG C,
Pressure is hot pressed sintering 50min under conditions of 13 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and
The volumn concentration of methane is 70% in the mixed gas of vapor, and surplus is vapor, and gas flow 80cc/min changes
The temperature for learning vapor deposition is 650 DEG C, time 20min.
The compactness of Tungsten-copper Composites manufactured in the present embodiment is 99.1%, thermal conductivity 280W/mK, and thermal expansion coefficient is
4.5×10-6/ K, tensile strength 685MPa, hardness 185HV.
Embodiment 5
The preparation method of the Tungsten-copper Composites of the present embodiment, comprising the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；The temperature of the reduction is
1500 DEG C, time 30min, hydrogen flowing quantity 40cc/min；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite wood
Material；The pressure in vacuum tank of the magnetron sputtering is 1.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, mixed gas
The volumn concentration of middle argon gas is 90%, and surplus is hydrogen chloride gas, and the magnetic induction intensity of magnetron sputtering is 0.3T, and the time is
30min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1500 DEG C,
Pressure is hot pressed sintering 30min under conditions of 15 tons, and then natural cooling, obtains presoma；
Step 4: precursor described in step 3 is placed in chemical vapor deposition stove, with the mixing of methane and vapor
Gas is reaction gas, carries out chemical vapor deposition to precursor, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and
The volumn concentration of methane is 85% in the mixed gas of vapor, and surplus is vapor, and gas flow 75cc/min changes
The temperature for learning vapor deposition is 750 DEG C, time 30min.
The compactness of Tungsten-copper Composites manufactured in the present embodiment is 99.3%, thermal conductivity 245W/mK, and thermal expansion coefficient is
4.6×10-6/ K, tensile strength 690MPa, hardness 183HV.
The above is only presently preferred embodiments of the present invention, not does any restrictions to the present invention, all according to invention skill
Art any simple modification substantially to the above embodiments, change and equivalent structural changes, still fall within the technology of the present invention
In the protection scope of scheme.
Claims (3)
1. a kind of preparation method of high compactness high thermal conductivity Tungsten-copper Composites, which is characterized in that the high compactness refers to tungsten copper material
The compactness of material is greater than 98%, and the high thermal conductivity refers to that the thermal conductivity of Tungsten-copper Composites is 220W/mK~300W/mK；
The preparation method comprises the following steps:
It restores Step 1: tungsten powder is placed in hydrogen furnace to remove the oxide layer on surface；
Step 2: carrying out magnetron sputtering using copper target as sputtering target material to the tungsten powder after restoring in step 1, obtaining composite material；
The pressure in vacuum tank of the magnetron sputtering is 1.0Pa~9.0Pa, and protective gas is the mixed gas of argon gas and hydrogen chloride, magnetic strength
Answering intensity is 0.2T~0.3T, and the time of magnetron sputtering is 30min~60min；
Step 3: composite material described in step 2 is placed in hot pressing furnace, under protection of argon gas, temperature is 1500 DEG C~1600
DEG C, pressure is hot pressed sintering 30min~60min under conditions of 10 tons~15 tons, and then natural cooling, obtains presoma；
Step 4: presoma described in step 3 is placed in chemical vapor deposition stove, with the mixed gas of methane and vapor
For reaction gas, chemical vapor deposition is carried out to presoma, obtains high compactness high thermal conductivity Tungsten-copper Composites；The methane and water
The volumn concentration of methane is 70%~90% in the mixed gas of steam, and surplus is vapor, gas flow 60cc/
Min~90cc/min, the temperature of chemical vapor deposition are 600 DEG C~800 DEG C, and the time is 10min~30min.
2. a kind of preparation method of high compactness high thermal conductivity Tungsten-copper Composites according to claim 1, which is characterized in that step
The temperature of reduction described in one be 1200 DEG C~1500 DEG C, the time be 30min~90min, hydrogen flowing quantity be 30cc/min~
50cc/min。
3. a kind of preparation method of high compactness high thermal conductivity Tungsten-copper Composites according to claim 1, which is characterized in that step
The volumn concentration of argon gas is 80%~90% in the mixed gas of argon gas described in two and hydrogen chloride, and surplus is hydrogen chloride gas
Body.
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| CN103079714A (en) * | 2010-09-02 | 2013-05-01 | 应用奈米结构公司 | Metal substrates having carbon nanotubes grown thereon and methods for production thereof |
| CN103589884A (en) * | 2013-11-25 | 2014-02-19 | 武汉理工大学 | Low-temperature preparation method of high-performance tungsten copper composite material |
| CN103849824A (en) * | 2014-03-11 | 2014-06-11 | 武汉理工大学 | Preparation method for CNT (Carbon Nanotube)-enhanced W-Cu thermal composite material |
| CN105755307A (en) * | 2016-03-21 | 2016-07-13 | 中南大学 | Reinforced composite adopting honeycomb structure and preparation method |
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2017
- 2017-06-01 CN CN201710404443.0A patent/CN107236876B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103079714A (en) * | 2010-09-02 | 2013-05-01 | 应用奈米结构公司 | Metal substrates having carbon nanotubes grown thereon and methods for production thereof |
| CN103589884A (en) * | 2013-11-25 | 2014-02-19 | 武汉理工大学 | Low-temperature preparation method of high-performance tungsten copper composite material |
| CN103849824A (en) * | 2014-03-11 | 2014-06-11 | 武汉理工大学 | Preparation method for CNT (Carbon Nanotube)-enhanced W-Cu thermal composite material |
| CN105755307A (en) * | 2016-03-21 | 2016-07-13 | 中南大学 | Reinforced composite adopting honeycomb structure and preparation method |
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