CN102925727B - 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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- CN102925727B CN102925727B CN201210454292.7A CN201210454292A CN102925727B CN 102925727 B CN102925727 B CN 102925727B CN 201210454292 A CN201210454292 A CN 201210454292A CN 102925727 B CN102925727 B CN 102925727B
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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 W-Cu field of compound material, particularly relate to a kind of low temperature preparation method of high-performance Zn@W-Cu heat matrix material, so-called high-performance Zn@W-Cu heat matrix material refer to have density up to more than 96.0%, thermal conductivity is about 200W/mK, resistivity lower than 1.7 × 10
-7the Zn@W-Cu heat matrix material of Ω m.
Background technology
The false alloy material that W-Cu matrix material is made up of the tungsten of high-melting-point, low thermal coefficient of expansion and the copper of high conductivity, high heat conductance and good plasticity.Because tungsten, copper do not dissolve each other in solid phase and liquid phase, therefore W-Cu matrix material combines the advantage of simple substance tungsten and copper, has the features such as high-density, high strength, good ductility, good electroconductibility and good thermal conductivity.Owing to having numerous premium propertiess, current W-Cu matrix material is just being widely used in electrical contact material, electrospark machining and electrode materials, rocket nozzle, the electronic package material of large-scale integrated circuit and the heat sink material etc. of microelectronic device.
At present in the application of W-Cu matrix material, require all higher to its density, the density being such as used as the W-Cu matrix material of electrical spark will reach more than 95%, the W-Cu matrix material being used 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, what the two was formed is a kind of typical false alloy, and therefore powder metallurgy is one of effective ways obtaining this metal composite, but its complete densification is the problem failing to solve very well always.The traditional method preparing the W-Cu matrix material of high-compactness at present mainly contains high-temperature liquid-phase sintering, infiltration etc.Bhalla etc. adopt explosive compaction legal system for the W-Cu matrix material of high W content, utilize explosive power to realize high-temperature liquid-phase sintering, obtain comparatively fine and close W-Cu matrix material; The infiltration mechanism of the people such as Liang Ronghai to high Tungsten Contact Alloys is inquired into, and obtains high-quality W-Cu matrix material infiltration goods.Although these traditional preparation methods can obtain the higher W-Cu matrix material of density, they are all easy to the distortion causing specimen shape, composition tolerances 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. L. Johnson etc. add transition element Pd, Ni, Co, Fe and carry out activated sintering to W-Cu matrix material, obtain at more than 1100oC the W-Cu matrix material that relative density reaches more than 95.0%; The people such as Dae-Gun Kim pass through mechanical ball milling W powder and CuO mixed powder, then at H
2under atmosphere, prepare fully dense W-Cu matrix material when 1200oC.Wherein, because activated sintering method can under the prerequisite of the performances such as the thermoelectricity of little amplitude reduction sample, significantly reduce sintering temperature, improve the performance of sample entirety and be subject to paying attention to more and more widely, such as Chen Pingan etc. are that sintering aid sinters and prepared the W-Cu matrix material that density is 97.0% at the temperature of 850oC with Zn.Although take Zn as the densification temperature that sintering aid significantly can reduce W-Cu matrix material, but join in W-Cu powder the skewness being easy to cause Zn and W, Cu in powder form, produce the reunion of Zn and the preferential reaction of Zn and Cu, thus reduce the effect of Zn as sintering aid.
Result according to consulted domestic and international patent and document shows: at present also not at the coated Zn of W particle surface, then at low temperatures by the report of the W-Cu matrix material of pressureless sintering preparation densification.
Summary of the invention
Technical problem to be solved by this invention is: for the deficiency of existing preparation technology, with the coated W of Zn, a kind of W-Cu composite material and preparation method thereof preparing higher-density is at low temperatures provided, the method sintering temperature is low, technique is controlled, it is high that prepared W-Cu matrix material has density, the feature 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: with the method for Zn block for target employing magnetron sputtering, or the Zn powder being 99.9% with purity adopts Vacuum Heat depositing process at the high-purity Zn film of W powder Surface coating one deck, obtain Zn@W powder, again by Zn@W powder, 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 under 100-400MPa, carry out isostatic cool pressing acquisition base substrate, finally 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 is 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, and soaking time is 30-60min.Described atmosphere sintering technique is: sintering temperature is 800oC ~ 1000oC, and soaking time is 30min ~ 90min, H
2in atmosphere.
Described Zn block target, its purity is 99.99%.
Described high-purity Zn powder, its purity is 99.9%.
Described W powder, its purity is 99.9%, and particle diameter is 2 ~ 10 μm.
Described Cu powder, its purity is 99.9%, and particle diameter is 1 ~ 10 μm.
The present invention compared with prior art has following main advantage:
Adopt with the coated W particle of Zn, control non-pressure sintering technology system (sintering temperature, soaking time), prepare density high (being greater than 96.0%), thermal conductivity high (about 200W/mK), resistivity are low by (1.7 × 10
-7Ω about m) W-Cu matrix material, the density of this matrix material is up to more than 96.0%.
Sintering temperature of the present invention is low compared with bibliographical information result, is only 800-1000oC, insulation 30min ~ 90min, and the raw material adopting industry easily to obtain and ball mill mixing mode, after burning till product composition and batch mixing and the goodness of fit of design mix high; Therefore there is the advantages such as technique is controlled, preparation time is short, cost low (energy consumption is low), density is high, calorifics, electric property are good.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of W-Cu matrix material.
Fig. 2-Fig. 8 is the microstructure picture of prepared W-Cu matrix material.
Embodiment
In order to understand the present invention better, be described further below in conjunction with embodiment.
Embodiment 1:
For magnetron sputtering, W powder after surface treatment is placed in the sample table of magnetron sputtering, with Zn block for target, first at the high-purity Zn film of W powder particles Surface coating one deck, again Zn W particle is carried out ball milling according to W:Cu=70:30% with Cu powder volume percent on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill to mix, then the powder mixed is carried out under 400MPa, carry out isostatic cool pressing and obtain base substrate, wherein W powder footpath is 5 μm, and Cu powder footpath is 10 μm; Finally put into hydrogen atmosphere stove, carry out pressureless sintering by appointment sintering process, sintering process is 800oC-90min, specifically, is warming up to 800oC, is incubated 90min, with stove Temperature fall, obtains fine and close Zn@W-Cu matrix material at 800oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, power is 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 adopting 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.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 for this matrix material microstructure, and W powder, Cu powder are evenly distributed.
Embodiment 2:
For magnetron sputtering, W powder after surface treatment is placed in the sample table of magnetron sputtering, with Zn block for target, first at the high-purity Zn film of the coated one deck of W particle surface, then by Zn@W powder, Cu powder volume ratio is carried out ball milling according to W:Cu=90:10% and is mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 100MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, Cu particle diameter is 50 μm, then hydrogen atmosphere stove is put into, pressureless sintering is carried out by appointment sintering process, sintering process is 1000oC-30min, specifically, be warming up to 1000oC, 30min is incubated at 1000oC, with stove Temperature fall, obtain preparing compact W-Cu composite material.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, power is 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 adopting 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.As shown in Figure 3, as can be seen from Figure 3 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for this matrix material microstructure.
Embodiment 3:
For magnetron sputtering, W powder after surface treatment is placed in the sample table of magnetron sputtering, with Zn block for target, first at the high-purity Zn film of the coated one deck of W particle surface, then Zn W powder, Cu powder volume ratio are carried out ball milling according to W:Cu=80:20vol% and mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 300MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, and Cu particle diameter is 10 μm; Then put into hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-60min, specifically, is warming up to 900oC, is incubated 60min, with stove Temperature fall, obtains preparing compact W-Cu composite material at 900oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
The technique of described magnetron sputtering is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, power is 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 adopting 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.As shown in Figure 4, as can be seen from Figure 4 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for the microstructure of this matrix material.
Embodiment 4:
For vacuum hot dip, vacuum oven will be placed in by W powder after surface treatment, with high-purity Zn powder for raw material, first at the high-purity Zn film of the coated one deck of W particle surface, then Zn W powder, Cu powder volume ratio are carried out ball milling according to W:Cu=80:20vol% and mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 400MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, and Cu particle diameter is 10 μm; Then put into hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 800oC-90min, specifically, is warming up to 800oC, is incubated 90min, with stove Temperature fall, obtains preparing compact W-Cu composite material at 800oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, temperature is 400oC, and soaking time is 60min.
The technique of described isostatic cool pressing is: pressure is 400MPa, pressurize 5min.
The density adopting 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.As shown in Figure 5, as can be seen from Figure 5 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for the microstructure of this matrix material.
Embodiment 5:
For vacuum hot dip, vacuum oven will be placed in by W powder after surface treatment, with high-purity Zn powder for raw material, first at the high-purity Zn film of the coated one deck of W particle surface, then Zn W powder, Cu powder volume ratio are carried out ball milling according to W:Cu=70:30vol% and mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 400MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, and Cu particle diameter is 10 μm; Then put into hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 1000oC-30min, specifically, is warming up to 1000oC, is incubated 30min, with stove Temperature fall, obtains preparing compact W-Cu composite material at 1000oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, temperature is 700oC, and soaking time is 30min.
The technique of described isostatic cool pressing is: pressure is 400MPa, pressurize 5min.
The density adopting 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.As shown in Figure 6, as can be seen from Figure 6 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for the microstructure of this matrix material.
Embodiment 6:
For vacuum hot dip, vacuum oven will be placed in by W powder after surface treatment, with high-purity Zn powder for raw material, first at the high-purity Zn film of the coated one deck of W particle surface, then Zn W powder, Cu powder volume ratio are carried out ball milling according to W:Cu=90:10vol% and mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 100MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, and Cu particle diameter is 10 μm; Then put into hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-60min, specifically, is warming up to 900oC, is incubated 60min, with stove Temperature fall, obtains preparing compact W-Cu composite material at 900oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, temperature is 500oC, and soaking time is 40min.
The technique of described isostatic cool pressing is: pressure is 100MPa, pressurize 5min.
The density adopting 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.As shown in Figure 7, as can be seen from Figure 7 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for the microstructure of this matrix material.
Embodiment 7:
For vacuum hot dip, vacuum oven will be placed in by W powder after surface treatment, with high-purity Zn powder for raw material, first at the high-purity Zn film of the coated one deck of W particle surface, then Zn W powder, Cu powder volume ratio are carried out ball milling according to W:Cu=80:20vol% and mixed on QM-3SP2 type (Nanjing Univ. Instrument Factory) ball mill, then powder is carried out under 200MPa, carry out isostatic cool pressing and obtain base substrate, wherein W particle diameter is 10 μm, and Cu particle diameter is 10 μm; Then put into hydrogen atmosphere stove, carry out pressureless sintering by given process, sintering process is 900oC-90min, specifically, is warming up to 900oC, is incubated 90min, with stove Temperature fall, obtains preparing compact W-Cu composite material at 900oC.
To W powder surface-treated method be: a certain amount of W powder is stirred 1h in the hydrochloric acid of 17%, then with distilled water cleaning to pH be 7, vacuum drying.
Described Vacuum Heat depositing process is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, temperature is 500oC, and soaking time is 60min.
The technique of described isostatic cool pressing is: pressure is 200MPa, pressurize 5min.
The density adopting 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.As shown in Figure 8, as can be seen from Figure 8 W-Cu matrix material is very fine and close, and W, Cu are evenly distributed for the microstructure of this matrix material.
Claims (7)
1. the preparation method of a Zn W-Cu heat matrix material, it is characterized in that with the method for Zn block for target employing magnetron sputtering, or the Zn powder being 99.9% with purity adopts Vacuum Heat depositing process at the high-purity Zn film of W powder Surface coating one deck, obtain Zn@W powder, again by Zn@W powder, 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 under 100-400MPa, carry out isostatic cool pressing acquisition base substrate, finally base substrate is put into hydrogen furnace and carry out atmosphere sintering, obtain Zn@W-Cu heat matrix material.
2. the preparation method of Zn@W-Cu heat matrix material according to claim 1, is characterized in that the technique of described magnetron sputtering is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, power is 50-120W, and sputtering time is 5-15min, and temperature is 90-200oC.
3. the preparation method of Zn@W-Cu heat matrix material according to claim 1, is characterized in that described Vacuum Heat depositing process is: vacuum tightness is 1 × 10
-3~ 1 × 10
-4pa, temperature is 400-700oC, and soaking time is 30-60min.
4. the preparation method of Zn@W-Cu heat matrix material according to claim 1, is characterized in that described atmosphere sintering technique is: sintering temperature is 800oC ~ 1000oC, and soaking time is 30min ~ 90min, H
2in atmosphere.
5. the preparation method of Zn@W-Cu heat matrix material according to claim 1, is characterized in that the purity of described Zn target is 99.99%.
6. the preparation method of Zn@W-Cu heat matrix material according to claim 1, it is characterized in that the purity of described W powder is 99.9%, particle diameter is 2 ~ 10 μm.
7. the preparation method of Zn@W-Cu heat matrix material according to claim 1, it is characterized in that the purity of described Cu powder is 99.9%, particle diameter is 1 ~ 10 μm.
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Cited By (1)
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| CN107671279A (en) * | 2017-09-13 | 2018-02-09 | 武汉理工大学 | The preparation method of tungsten copper silver carbon system composite |
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| CN103849824B (en) * | 2014-03-11 | 2016-09-21 | 武汉理工大学 | CNT strengthens the preparation method of W-Cu heat composite |
| 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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