CN102925727A - Preparation method for high-performance Zn@W-Cu heat composite - Google Patents
Preparation method for high-performance Zn@W-Cu heat composite Download PDFInfo
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Abstract
The invention provides a preparation method for high-performance Zn@W-Cu heat composite. The preparation method for the high-performance Zn@W-Cu heat composite is characterized by utilizing a magnetron sputtering method. Zinc blocks serve as target materials, or the surface of tungstenic powder is covered by a layer of high-purity zinc film with zinc powder with the purity of 99.9 % by utilizing a vacuum hot-dip coating process, so that Zn@W powder is obtained, the Zn@W powder and copper powder are evenly mixed in a ball-milling mode according to the volume percentage that W=70.0 %-90.0 % and Cu=10.0 %-30.0 %, an isostatic cool pressing operation is carried out on the evenly mixed powder at the pressure of 100-400 M Pa to obtain a green body, and the green body is sintered in an atmosphere mode after placed into a hydrogen furnace to obtain the Zn@W-Cu heat composite. The preparation method for the high-performance Zn@W-Cu heat composite is capable of obtaining the W-Cu composite which is high in density, strong in combination capacity between tungsten and copper, and good in heat conductivity and electric conductively at a relatively low sintering temperature, and has the advantages of being controllable in the W-Cu composite, small in adding amount of zinc, capable of achieving directional covering, and the like.
Description
Technical field
The present invention relates to the W-Cu field of compound material, particularly relate to a kind of high-performance Zn@W-Cu heat with the low temperature preparation method of matrix material, so-called high-performance Zn@W-Cu heat with matrix material refer to have density up to more than 96.0%, thermal conductivity is about 200W/mK, resistivity is lower than 1.7 * 10
-7The Zn@W-Cu heat matrix material of Ω m.
Background technology
The false alloy material that the W-Cu matrix material is comprised of the copper of the tungsten of high-melting-point, low thermal coefficient of expansion and high conductivity, high heat conductance and good plasticity.Because tungsten, copper do not dissolve each other in solid phase and liquid phase, so the W-Cu matrix material combines the advantage of simple substance tungsten and copper, has high-density, high strength, good ductility, good electroconductibility and the good characteristics such as thermal conductivity.Owing to having numerous premium propertiess, the W-Cu matrix material just is being widely used in the electronic package material of electrical contact material, electrospark machining and electrode materials, rocket nozzle, large-scale integrated circuit and the heat sink material of microelectronic device etc. at present.
At present in the W-Cu matrix material is used, require all higher to its density, the density that for example is used as the W-Cu matrix material of electrical spark will reach more than 95%, W-Cu matrix material as electronic package material and heat sink material then has higher resistance to air loss and intensity, and density will reach more than 97%.Because tungsten and copper do not dissolve each other, the two formation be a kind of typical false alloy, so powder metallurgy is one of effective ways of this metal composite of acquisition, but its complete densification is the problem of fine solution of failing always.The traditional method of the W-Cu matrix material of preparation high-compactness mainly contains high-temperature liquid-phase sintering, infiltration etc. at present.Bhalla etc. adopt the explosive compaction legal system for the W-Cu matrix material of high W content, utilize explosive power to realize the high-temperature liquid-phase sintering, have obtained comparatively fine and close W-Cu matrix material; The people such as Liang Ronghai inquire into the infiltration mechanism of high Tungsten Contact Alloys, have obtained high-quality W-Cu matrix material infiltration goods.Although these traditional preparation methods can obtain the higher W-Cu matrix material of density, they all are easy to cause the distortion of specimen shape, composition deviation and consumptive material consuming time etc.For this reason, vast researcher has developed mechanical alloying method, has used some novel preparation methods such as nanometer powder method and activated sintering method.J. interpolation transition element Pd, Ni, Co, the Fe such as L. Johnson carries out activated sintering to the W-Cu matrix material, reaches W-Cu matrix material more than 95.0% obtaining relative density more than the 1100oC; The people such as Dae-Gun Kim are by mechanical ball milling W powder and CuO mixed powder, then at H
2Under the atmosphere, when 1200oC, prepared fully dense W-Cu matrix material.Wherein, because the activated sintering method can reduce under the prerequisite of the performances such as thermoelectricity of sample in little amplitude, the decrease sintering temperature, improve the performance of sample integral body and be subject to paying attention to more and more widely, such as Chen Pingan etc. take Zn as sintering aid under the temperature of 850oC sintering prepared the W-Cu matrix material of density as 97.0%.Although densification temperature that can decrease W-Cu matrix material take Zn as sintering aid, but join the skewness that is easy to cause Zn and W, Cu in the W-Cu powder with powder type, produce the reunion of Zn and the preferential reaction of Zn and Cu, thereby reduced the effect of Zn as sintering aid.
Show according to the domestic and international patent of consulting and the result of document: also do not coat Zn at the W particle surface at present, then prepare at low temperatures the report of fine and close W-Cu matrix material by pressureless sintering.
Summary of the invention
Technical problem to be solved by this invention is: for existing preparation technology's deficiency, coat W with Zn, a kind of W-Cu composite material and preparation method thereof for preparing at low temperatures higher-density is provided, the method sintering temperature is low, technique is controlled, it is high that prepared W-Cu matrix material has density, the characteristics of heat conduction, good conductivity.
The present invention solves its technical problem and adopts following technical scheme:
The low temperature preparation method of W-Cu matrix material provided by the invention, specifically: the method that adopts magnetron sputtering take the Zn piece as target, perhaps adopt the Vacuum Heat depositing process to coat the high-purity Zn film of one deck on W powder surface take the Zn powder of purity as 99.9%, obtain Zn@W powder, again with Zn@W powder, the Cu powder is W=70.0% ~ 90.0% according to volume percent, Cu=10.0% ~ 30.0% carries out ball milling and mixes, then will mix powder and under 100-400MPa, carry out isostatic cool pressing acquisition base substrate, at last base substrate is put into hydrogen furnace and carry out atmosphere sintering, obtain Zn@W-Cu heat matrix material.
The technique of described magnetron sputtering is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, power are 50-120W, and sputtering time is 5-15min, and temperature is 90-200oC.Described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 400-700oC, soaking time is 30-60min.Described atmosphere sintering technique is: sintering temperature is 800oC ~ 1000oC, and soaking time is 30min ~ 90min, H
2In the atmosphere.
Described Zn piece target, its purity is 99.99%.
Described high-purity Zn powder, its purity is 99.9%.
Described W powder, its purity are 99.9%, and particle diameter is 2 ~ 10 μ m.
Described Cu powder, its purity are 99.9%, and particle diameter is 1 ~ 10 μ m.
The present invention compared with prior art has advantages of following main:
Employing coats the W particle with Zn, and control non-pressure sintering technology system (sintering temperature, soaking time) is prepared density high (greater than 96.0%), thermal conductivity high (about 200W/mK), resistivity low by (1.7 * 10
-7About Ω m) the W-Cu matrix material, the density of this matrix material is up to more than 96.0%.
Sintering temperature of the present invention is compared low with the bibliographical information result, only be 800-1000oC, insulation 30min ~ 90min, and the raw material and the ball mill mixing mode that adopt industry easily to obtain, burn till behind product composition and the batch mixing and the goodness of fit of design mix high; The advantage such as therefore have that technique is controlled, preparation time is short, cost low (energy consumption is low), density are high, calorifics, electric property are good.
Description of drawings
Fig. 1 is W-Cu composite manufacture process flow sheet.
Fig. 2-Fig. 8 is the microstructure picture of prepared W-Cu matrix material.
Embodiment
In order to understand better the present invention, be described further below in conjunction with embodiment.
Embodiment 1:
Take magnetron sputtering as example, to place through W powder after the surface treatment sample table of magnetron sputtering, take the Zn block as target, at first coat the high-purity Zn film of one deck on W powder particles surface, again the long-pending per-cent of Zn W particle and Cu powder being carried out ball milling according to W:Cu=70:30% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then the powder that mixes is carried out carrying out isostatic cool pressing and obtain base substrate under 400MPa, wherein the W powder directly is 5 μ m, and the Cu powder directly is 10 μ m; Put at last the hydrogen atmosphere stove, by specifying sintering process to carry out pressureless sintering, sintering process is 800oC-90min, specifically, is warming up to 800oC, at 800oC insulation 90min, naturally lowers the temperature with stove, obtains fine and close Zn@W-Cu matrix material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, power are 50W, and sputtering time is 15min, and temperature is 200oC.
The technique of described isostatic cool pressing is: pressure is 400MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this Zn@W-Cu matrix material is 16.15g/cm
3, density reaches 99.8%, and thermal conductivity is 230.5 W/mK, and resistivity is 0.85 * 10
-7Ω m.This matrix material microstructure as shown in Figure 2, as can be seen from Figure 2 Zn@W-Cu matrix material is very fine and close, does not have large hole, W powder, Cu powder are evenly distributed.
Embodiment 2:
Take magnetron sputtering as example, to place through W powder after the surface treatment sample table of magnetron sputtering, take the Zn block as target, at first coat the high-purity Zn film of one deck at the W particle surface, then with Zn@W powder, Cu powder volume ratio is carried out ball milling according to W:Cu=90:10% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill and is mixed, then powder is carried out under 100MPa, carrying out isostatic cool pressing and obtain base substrate, wherein the W particle diameter is 10 μ m, the Cu particle diameter is 50 μ m, then put into the hydrogen atmosphere stove, by specifying sintering process to carry out pressureless sintering, sintering process is 1000oC-30min, specifically, be warming up to 1000oC, at 1000oC insulation 30min, naturally lower the temperature with stove, obtain preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, power are 120W, and sputtering time is 5min, and temperature is 90oC.
The technique of described isostatic cool pressing is: pressure is 100MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 17.71g/cm
3, density reaches 97.0%, and thermal conductivity is 200.2 W/mK, and resistivity is 1.7 * 10
-7Ω m.This matrix material microstructure as shown in Figure 3, as can be seen from Figure 3 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Embodiment 3:
Take magnetron sputtering as example, to place through W powder after the surface treatment sample table of magnetron sputtering, take the Zn block as target, at first coat the high-purity Zn film of one deck at the W particle surface, then Zn W powder, Cu powder volume ratio being carried out ball milling according to W:Cu=80:20vol% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then powder is carried out carrying out isostatic cool pressing and obtain base substrate under 300MPa, wherein the W particle diameter is 10 μ m, and the Cu particle diameter is 10 μ m; Then put into the hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-60min, specifically, is warming up to 900oC, at 900oC insulation 60min, naturally lowers the temperature with stove, obtains preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, power are 100W, and sputtering time is 10min, and temperature is 150oC.
The technique of described isostatic cool pressing is: pressure is 300MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 16.90g/cm
3, density reaches 98.1%, and thermal conductivity is 210.1 W/mK, and resistivity is 1.58 * 10
-7Ω m.The microstructure of this matrix material as shown in Figure 4, as can be seen from Figure 4 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Embodiment 4:
Take the vacuum hot dip as example, to place vacuum oven through W powder after the surface treatment, take high-purity Zn powder as raw material, at first coat the high-purity Zn film of one deck at the W particle surface, then Zn W powder, Cu powder volume ratio being carried out ball milling according to W:Cu=80:20vol% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then powder is carried out carrying out isostatic cool pressing and obtain base substrate under 400MPa, wherein the W particle diameter is 10 μ m, and the Cu particle diameter is 10 μ m; Then put into the hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 800oC-90min, specifically, is warming up to 800oC, at 800oC insulation 90min, naturally lowers the temperature with stove, obtains preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 400oC, soaking time is 60min.
The technique of described isostatic cool pressing is: pressure is 400MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 16.95g/cm
3, density reaches 98.4%, and thermal conductivity is 205.1 W/mK, and resistivity is 1.5 * 10
-7Ω m.The microstructure of this matrix material as shown in Figure 5, as can be seen from Figure 5 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Embodiment 5:
Take the vacuum hot dip as example, to place vacuum oven through W powder after the surface treatment, take high-purity Zn powder as raw material, at first coat the high-purity Zn film of one deck at the W particle surface, then Zn W powder, Cu powder volume ratio being carried out ball milling according to W:Cu=70:30vol% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then powder is carried out carrying out isostatic cool pressing and obtain base substrate under 400MPa, wherein the W particle diameter is 10 μ m, and the Cu particle diameter is 10 μ m; Then put into the hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 1000oC-30min, specifically, is warming up to 1000oC, at 1000oC insulation 30min, naturally lowers the temperature with stove, obtains preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 700oC, soaking time is 30min.
The technique of described isostatic cool pressing is: pressure is 400MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 15.86g/cm
3, density reaches 98.0%, and thermal conductivity is 220.1 W/mK, and resistivity is 1.1 * 10
-7Ω m.The microstructure of this matrix material as shown in Figure 6, as can be seen from Figure 6 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Embodiment 6:
Take the vacuum hot dip as example, to place vacuum oven through W powder after the surface treatment, take high-purity Zn powder as raw material, at first coat the high-purity Zn film of one deck at the W particle surface, then Zn W powder, Cu powder volume ratio being carried out ball milling according to W:Cu=90:10vol% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then powder is carried out carrying out isostatic cool pressing and obtain base substrate under 100MPa, wherein the W particle diameter is 10 μ m, and the Cu particle diameter is 10 μ m; Then put into the hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-60min, specifically, is warming up to 900oC, at 900oC insulation 60min, naturally lowers the temperature with stove, obtains preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 500oC, soaking time is 40min.
The technique of described isostatic cool pressing is: pressure is 100MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 17.80g/cm
3, density reaches 97.5%, and thermal conductivity is 198.2 W/mK, and resistivity is 1.9 * 10
-7Ω m.The microstructure of this matrix material as shown in Figure 7, as can be seen from Figure 7 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Embodiment 7:
Take the vacuum hot dip as example, to place vacuum oven through W powder after the surface treatment, take high-purity Zn powder as raw material, at first coat the high-purity Zn film of one deck at the W particle surface, then Zn W powder, Cu powder volume ratio being carried out ball milling according to W:Cu=80:20vol% at QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill mixes, then powder is carried out carrying out isostatic cool pressing and obtain base substrate under 200MPa, wherein the W particle diameter is 10 μ m, and the Cu particle diameter is 10 μ m; Then put into the hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-90min, specifically, is warming up to 900oC, at 900oC insulation 90min, naturally lowers the temperature with stove, obtains preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in 17% hydrochloric acid, then with distilled water clean to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 500oC, soaking time is 60min.
The technique of described isostatic cool pressing is: pressure is 200MPa, pressurize 5min.
The density that adopts Archimedes's water discharge method to record this W-Cu matrix material is 16.87g/cm
3, density reaches 97.9%, and thermal conductivity is 205.4 W/mK, and resistivity is 1.5 * 10
-7Ω m.The microstructure of this matrix material as shown in Figure 8, as can be seen from Figure 8 the W-Cu matrix material is very fine and close, W, Cu are evenly distributed.
Claims (7)
1. Zn W-Cu heat composite manufacture method, it is characterized in that adopting take the Zn piece as target the method for magnetron sputtering, perhaps adopt the Vacuum Heat depositing process to coat the high-purity Zn film of one deck on W powder surface take the Zn powder of purity as 99.9%, obtain Zn@W powder, again with Zn@W powder, the Cu powder is W=70.0% ~ 90.0% according to volume percent, Cu=10.0% ~ 30.0% carries out ball milling and mixes, then will mix powder and under 100-400MPa, carry out isostatic cool pressing acquisition base substrate, at last base substrate is put into hydrogen furnace and carry out atmosphere sintering, obtain Zn@W-Cu heat matrix material.
2. Zn@W-Cu heat according to claim 1 is used the composite manufacture method, and it is characterized in that the technique of described magnetron sputtering is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, power are 50-120W, and sputtering time is 5-15min, and temperature is 90-200oC.
3. Zn@W-Cu heat according to claim 1 is used the composite manufacture method, and it is characterized in that described Vacuum Heat depositing process is: vacuum tightness is 1 * 10
-3~ 1 * 10
-4Pa, temperature is 400-700oC, soaking time is 30-60min.
4. the low temperature preparation method of Zn@W-Cu matrix material according to claim 1, it is characterized in that described atmosphere sintering technique is: sintering temperature is 800oC ~ 1000oC, and soaking time is 30min ~ 90min, H
2In the atmosphere.
5. Zn@W-Cu heat according to claim 1 is used the composite manufacture method, and the purity that it is characterized in that described Zn target is 99.99%.
6. Zn@W-Cu heat according to claim 1 is used the composite manufacture method, and the purity that it is characterized in that described W powder is 99.9%, and particle diameter is 2 ~ 10 μ m.
7. Zn@W-Cu according to claim 1 heat is with the low temperature preparation method of matrix material, and the purity that it is characterized in that described Cu powder is 99.9%, and particle diameter is 1 ~ 10 μ m.
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| CN106978586A (en) * | 2017-04-01 | 2017-07-25 | 西安交通大学 | A kind of overlay coating processing method of arc-chutes copper tungsten electrical contact material |
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| CN103464742B (en) * | 2013-09-18 | 2016-01-20 | 武汉理工大学 | The compound coating raw powder's production technology of the coated tungsten of a kind of copper clad silver |
| 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 |
| CN106978586A (en) * | 2017-04-01 | 2017-07-25 | 西安交通大学 | A kind of overlay coating processing method of arc-chutes copper tungsten electrical contact material |
| CN106978586B (en) * | 2017-04-01 | 2018-12-07 | 西安交通大学 | A kind of overlay coating processing method of arc-chutes copper tungsten electrical contact material |
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