CN104152734A - Method for preparing tungsten-copper alloy from spherical tungsten powder - Google Patents
Method for preparing tungsten-copper alloy from spherical tungsten powder Download PDFInfo
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- CN104152734A CN104152734A CN201410258559.4A CN201410258559A CN104152734A CN 104152734 A CN104152734 A CN 104152734A CN 201410258559 A CN201410258559 A CN 201410258559A CN 104152734 A CN104152734 A CN 104152734A
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Abstract
The invention discloses a method for preparing a tungsten-copper alloy from spherical tungsten powder. The method comprises the following steps of carrying out cold pressing on mixed powder at a pressure of 200-900MPa to obtain a preform body of which the relative density reaches 75%-85%; carrying out vacuum degassing on the preform body, placing the vacuum degassed preform body in a closed graphite crucible and placing a copper material on the upper surface of the preform body in the graphite crucible, wherein the mass of the copper material is 1.1-1.5 times that of the alloy copper in the step 1; filling the graphite crucible with aluminium oxide, heating the preform body and the copper material in the graphite crucible at a heating speed of 5-10 DEG C per minute, when the temperature reaches 900-1000 DEG C, maintaining the temperature for two hours and then continuously heating, copperizing at 1200-1300 DEG C and maintaining the temperature for 1-3 hours to obtain the tungsten-copper alloy. The tungsten-copper alloy prepared by the method disclosed by the invention has the advantages of high density, good compatibility of tungsten and copper and high conductivity.
Description
Technical field
The present invention relates to globular tungsten powder and prepare the method for tungsten-copper alloy.
Background technology
W-Cu alloy is the two-phase mixed structure that a kind of neither mutual solid solution being made up of the tungsten of body-centered cubic structure and the copper of face-centred cubic structure does not form again intermetallic compound, is commonly called pseudo-alloy.Therefore, it had both had the characteristic such as high strength, high rigidity, low-expansion coefficient of tungsten, had again the characteristic such as high-ductility, good conductive and heat-conductive of copper simultaneously.This distinctive over-all properties is widely used W-Cu alloy in contact material and electrode materials.
In the time of preparation W-Cu alloy, common adopted tungsten powder mean particle size is 2-8 μ m left and right, and copper powder granularity is tens microns, and production technique is: mixed powder, shaping, sintering, following process; Or adopt tungsten powder to be shaped, copper billet and tungsten pressed compact are overlayed to the infiltration technique of sintering at 1200～1300 DEG C of high temperature etc.In this conventional art, because W-Cu liquid phase wetting angle is non-vanishing and W-Cu does not dissolve again mutually, no matter be therefore that liquid phase sintering or solid state sintering are all difficult to make the relative density of sintered products to be greater than 98%.Though repressing and re-sintering or subsequent thermal processing can improve product density, cost increases, Efficiency Decreasing.Original tungsten particle will be grown up 5～10 times in liquid sintering process, causes the further alligatoring of tungsten grain in sintering.This alloy structure can not meet in recent years the requirement as the W-Cu alloy of hi-tech purposes.
Summary of the invention
For the problems referred to above, the object of the present invention is to provide a kind ofly have that density is high, method that tungsten and copper intermiscibility globular tungsten powder good and that specific conductivity is high are prepared tungsten-copper alloy.
The technical scheme solving the problems of the technologies described above is as follows:
Globular tungsten powder is prepared the method for tungsten-copper alloy, comprises the following steps:
Step 1, get and 10%-20% copper powder mix with globular tungsten powder 70%-80% end by weight percentage, wherein the diameter at globular tungsten powder end is 2-8 μ m, copper powder is that electrolytic copper powder median size is 45 μ m, with 100～130r/min speed ball milling mixed powder 5-10h, when ball milling mixed powder, steel ball is 5: 1 with the ratio of compound;
Step 2, mixed powder is colded pressing and made blank under 200-900MPa pressure condition, make the relative density of blank reach 75%-85%;
Step 3, blank is carried out to vacuum outgas, the blank of vacuum outgas is put into airtight plumbago crucible, and in plumbago crucible, puts into copper material, and copper material is put the upper surface in blank, the quality of copper material be step 1 interalloy copper mass 1.1-1.5 doubly;
Step 4, employing aluminum oxide carry out landfill to plumbago crucible, heat-up rate with 5-10 DEG C/min heats up to the blank in plumbago crucible and copper material, while being heated to 900-1000 DEG C, is incubated 2 hours, then continues to heat up, at 1200-1300 DEG C, ooze copper, insulation 1-3h makes tungsten-copper alloy.
Adopt such scheme, the present invention makes tungsten copper powder mix after blank, without first sintered skeleton, but be directly contained in airtight plumbago crucible, while being heated to 900-1000 DEG C, be incubated 2 hours, then continue to heat up, at 1200-1300 DEG C, ooze copper, and due to when the base, in blank, having electrolytic copper powder and relative density is 75%-85%, electrolytic copper powder at this temperature in blank also liquefies, the mobility of copper phase and the filling properties to hole are improved, it is high that thereby the tungsten-copper alloy that makes to make has density, tungsten and the advantage that copper intermiscibility is good and specific conductivity is high.
Preferably, in described step 4, in the time that intensification temperature approaches copper fusing point, in plumbago crucible, pass into shielding gas.By shielding gas, not only reduce the oxidation of copper under molten state, and under the effect of protection pressure gas; help flowing of copper phase; promoted the filling of copper relative porosity factor, therefore, the copper-tungsten that makes to make has advantages of that density is high, tungsten and copper intermiscibility is good and specific conductivity is high.
Preferably, passing into before shielding gas in plumbago crucible, first to vacuumizing in plumbago crucible.In vacuum environment, pass into after shielding gas; in plumbago crucible, be the atmosphere of shielding gas completely, blank and copper material in this atmosphere, the effect that can not be oxidized completely; and increased the gas pressure power of plumbago crucible, make copper more easily evenly infiltration in tungsten basal body.
Embodiment
Globular tungsten powder is prepared the method for tungsten-copper alloy, comprises the following steps:
Step 1, get and 10%-20% copper powder mix with globular tungsten powder 70%-80% end by weight percentage, wherein the diameter at globular tungsten powder end is 2-8 μ m, copper powder is that electrolytic copper powder median size is 45 μ m, with 100～130r/min speed ball milling mixed powder 5-10h, when ball milling mixed powder, steel ball is 5: 1 with the ratio of compound, and steel ball and compound adopt such ratio, is that the mixing in order to make compound can be more even.
Step 2, mixed powder is colded pressing and made blank under 200-900MPa pressure condition, make the relative density of blank reach 75%-85%.
Step 3, blank is carried out to vacuum outgas, will after the blank base of vacuum outgas, put into airtight plumbago crucible, and in plumbago crucible, put into copper material, copper material is put the upper surface in blank, the quality of copper material be step 1 interalloy copper mass 1.1-1.5 doubly.
Step 4, employing aluminum oxide carry out landfill to plumbago crucible, with the heat-up rate of 5-10 DEG C/min, the blank in plumbago crucible and copper material are heated up, and at 1200-1300 DEG C, ooze copper, and insulation 1-3h makes tungsten-copper alloy.In step 4, in the time that intensification temperature approaches copper fusing point, in plumbago crucible, pass into shielding gas.The flow velocity of shielding gas is 150-400ml/min, and shielding gas is nitrogen.Passing into before shielding gas in plumbago crucible, first to vacuumizing in plumbago crucible.
Except above step, the present invention also comprises the making to globular tungsten powder end, and detailed process is as follows:
Selecting raw material powder is tungsten powder in irregular shape, 200 orders sieve, purity > 99.9%, raw material powder is sent in airflow milling and ground, obtain the powder of the one-tenth individual particle of good dispersity, even particle size distribution, the separation wheel rotating speed of airflow milling is 2500-7000 rev/min, and grinding chamber pressure is 0.1MPa-1MPa, powder feeding rate 0.1-20kg/ hour.After raw material tungsten powder is fully dry, pack into for powder chamber, after excluding air with atmospheric isolation.Induction plasma producer first vacuumizes, and then passes into working gas Ar, starts induction plasma producer, sets up stable argon plasma torch, and original tungsten powder passes through H
2send into plasma torch, the powder sending quantity of tungsten powder is 50g/min, and the pressure of center gas (Ar) is 0.5Mpa-0.7MPa, and the flow of center gas Ar is 0.8m
3/ h, the defeated gas (H that helps
2) pressure be 0.5MPa-0.7MPa, the defeated gas (H that helps
2) flow be 0.8m
3/ h, the power loading on ruhmkorff coil is 40KW-90KW; The pressure of the main working gas argon gas when steady running of argon plasma torch is 0.5MPa-0.6MPa, and the pressure of back work gas hydrogen is 0.5MPa-0.6Mpa; The tungsten powder particles that enters argon plasma torch absorbs a large amount of heat and gasification, cracking rapidly in a short period of time, forms spherical droplets under capillary effect, and the high-temperature zone that speeds away enters water-cooled holding tank and solidifies.Form tiny spherical tungsten particle.Tungsten powder is collected respectively from heat exchange chamber bottom and secondary collecting chamber and filtering net.
Tungsten powder particle-size before and after nodularization and pattern are carried out to observation analysis with JSM-6700F high resolution scanning electron microscope, count the shared per-cent of spheroidal globule after spheroidizing, each sample random sampling statistics 3 times, then get the nodularization rate of arithmetical av as this sample, and measure the tap density of Cement Composite Treated by Plasma front and back tungsten powder with BT-300 powder tapping Density Measuring Instrument.Raw material tungsten powder particles is coacervate in irregular shape or loose porous granule, is the spherical of rule through said process tungsten powder after treatment, and smooth surface.In addition, after nodularization, the particle diameter of tungsten powder is also less than raw material tungsten powder.Plasma-treating technology is described except comprising nodularization process. the process of in addition tungsten powder being carried out to refinement.Refinement reason is because raw material tungsten powder is not single full particle, but loose POROUS TUNGSTEN particle or the coacervate that formed by many small-particles.These coacervates or unsound particle are sharply heated the rapid dissociation of meeting and make tungsten powder refinement in plasma arc.In addition, tungsten powder coexists in high-temperature zone gasification and melting process. and less nano particle may be the product of tungsten vapour condensation.Tungsten powder has experienced gasification-condensation process, and therefore product tungsten powder obtains refinement.
Embodiment 1:
Get by weight percentage and 10% copper powder mix with globular tungsten powder 80% end, the diameter at globular tungsten powder end is 2-8 μ m, and the median size of copper powder is 45 μ m, with 100r/min speed ball milling mixed powder 10h.Mixed powder is colded pressing and made blank under 900MPa pressure condition, make the relative density of blank reach 85%.Blank is carried out to vacuum outgas, the blank of vacuum outgas is put into airtight plumbago crucible, and in plumbago crucible, put into copper material, copper material is put the upper surface in blank, and the quality of copper material is 1.5 times of step 1 interalloy copper mass.Adopt aluminum oxide to carry out landfill to plumbago crucible, heat-up rate with 10 DEG C/min heats up to the blank in plumbago crucible and copper material, in the time of 900-1000 DEG C, is incubated 2 hours, then continues to heat up, when temperature approaches copper fusing point, first to vacuumizing in plumbago crucible.In plumbago crucible, pass into shielding gas again, the flow velocity of shielding gas is 150ml/min, and shielding gas is nitrogen.At 1200 DEG C, ooze copper, insulation 1h makes tungsten-copper alloy.
Embodiment 2:
Get by weight percentage and 15% copper powder mix with globular tungsten powder 75% end, the diameter at globular tungsten powder end is 2-8 μ m, and the median size of copper powder is 45 μ m, with 120r/min speed ball milling mixed powder 7h.Mixed powder is colded pressing and made blank under 400MPa pressure condition, make the relative density of blank reach 80%.Blank is carried out to vacuum outgas, and the blank of vacuum outgas is put into airtight plumbago crucible, and in plumbago crucible, puts into copper material, and copper material is put the upper surface in blank, and the quality of copper material is 1.4 times of step 1 interalloy copper mass.Adopt aluminum oxide to carry out landfill to plumbago crucible, heat-up rate with 8 DEG C/min heats up to the blank in plumbago crucible and copper material, in the time of 900-1000 DEG C, is incubated 2 hours, then continues to heat up, when temperature approaches copper fusing point, first to vacuumizing in plumbago crucible.In plumbago crucible, pass into shielding gas again, the flow velocity of shielding gas is 250ml/min, and shielding gas is nitrogen.At 1250 DEG C, ooze copper, insulation 2h makes tungsten-copper alloy.
Embodiment 3:
Get by weight percentage and 20% copper powder mix with globular tungsten powder 70% end, the diameter at globular tungsten powder end is 2-8 μ m, and the median size of copper powder is 45 μ m, with 130r/min speed ball milling mixed powder 5h.Mixed powder is colded pressing and made blank under 200MPa pressure condition, make the relative density of blank reach 75%.Blank is carried out to vacuum outgas, and the blank of vacuum outgas is put into airtight plumbago crucible, and in plumbago crucible, puts into copper material, and copper material is put the upper surface in blank, and the quality of copper material is 1.1 times of step 1 interalloy copper mass.Adopt aluminum oxide to carry out landfill to plumbago crucible, heat-up rate with 5 DEG C/min heats up to the blank in plumbago crucible and copper material, in the time of 900-1000 DEG C, is incubated 2 hours, then continues to heat up, when temperature approaches copper fusing point, first to vacuumizing in plumbago crucible.In plumbago crucible, pass into shielding gas again, the flow velocity of shielding gas is 250ml/min, and shielding gas is nitrogen.At 1300 DEG C, ooze copper, insulation 3h makes tungsten-copper alloy.
Claims (5)
1. globular tungsten powder is prepared the method for tungsten-copper alloy, it is characterized in that, comprises the following steps:
Step 1, journey is got the copper powder of 10%-20% and the globular tungsten powder end of 70%-80% is mixed by weight percentage, wherein the diameter at globular tungsten powder end is 2-8 μ m, copper powder is that electrolytic copper powder median size is 45 μ m, with 100～130r/min speed ball milling mixed powder 5-10h, when ball milling mixed powder, steel ball is 5: 1 with the ratio of compound;
Step 2, mixed powder is colded pressing and made blank under 200-900MPa pressure condition, make the relative density of blank reach 75%-85%;
Step 3, blank carry out vacuum outgas, and the blank of vacuum outgas is put into airtight plumbago crucible, and in plumbago crucible, put into copper material, and copper material is put the upper surface in blank, and the quality of copper material is 1.1-1.5 times of step 1 interalloy copper mass;
Step 4, employing aluminum oxide carry out landfill to plumbago crucible, heat-up rate with 5-10 DEG C/min heats up to the blank in plumbago crucible and copper material, while being heated to 900-1000 DEG C, is incubated 2 hours, then continues to heat up, at 1200-1300 DEG C, ooze copper, insulation 1-3h makes tungsten-copper alloy.
2. globular tungsten powder according to claim 1 is prepared the method for tungsten-copper alloy, it is characterized in that, in described step 4, in the time that intensification temperature approaches copper fusing point, in plumbago crucible, passes into shielding gas.
3. globular tungsten powder according to claim 2 is prepared the method for tungsten-copper alloy, it is characterized in that, the flow velocity of described shielding gas is 150-400ml/min.
4. the method for preparing tungsten-copper alloy according to the globular tungsten powder described in claim 2 or 3, is characterized in that, described shielding gas is nitrogen.
5. the method for preparing tungsten-copper alloy according to the globular tungsten powder described in claim 2 or 3, is characterized in that, passing into before shielding gas in plumbago crucible, first to vacuumizing in plumbago crucible.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105057680A (en) * | 2015-07-29 | 2015-11-18 | 昆山德泰新材料科技有限公司 | Preparation method of mechanical alloying copper-tungsten alloy powder |
| CN109234597A (en) * | 2018-11-22 | 2019-01-18 | 江苏经纬阀业有限公司 | A kind of tungsten-copper alloy and preparation method thereof |
| 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 |
| CN114582730A (en) * | 2022-02-28 | 2022-06-03 | 江南大学 | Method for preparing high-performance aluminum-based composite material heat dissipation substrate |
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| CN1995438A (en) * | 2006-12-22 | 2007-07-11 | 株洲硬质合金集团有限公司 | Method for preparing elconite |
| CN102312146A (en) * | 2011-08-05 | 2012-01-11 | 西安理工大学 | Preparation method of CuW70 contact material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1995438A (en) * | 2006-12-22 | 2007-07-11 | 株洲硬质合金集团有限公司 | Method for preparing elconite |
| CN102312146A (en) * | 2011-08-05 | 2012-01-11 | 西安理工大学 | Preparation method of CuW70 contact material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105057680A (en) * | 2015-07-29 | 2015-11-18 | 昆山德泰新材料科技有限公司 | Preparation method of mechanical alloying copper-tungsten alloy powder |
| CN105057680B (en) * | 2015-07-29 | 2018-03-27 | 昆山德泰新材料科技有限公司 | A kind of preparation method of mechanical alloying copper-tungsten powder |
| CN109234597A (en) * | 2018-11-22 | 2019-01-18 | 江苏经纬阀业有限公司 | A kind of tungsten-copper alloy and preparation method thereof |
| 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 |
| CN114582730A (en) * | 2022-02-28 | 2022-06-03 | 江南大学 | Method for preparing high-performance aluminum-based composite material heat dissipation substrate |
| CN114582730B (en) * | 2022-02-28 | 2022-11-04 | 江南大学 | Method for preparing high-performance aluminum matrix composite heat dissipation substrate |
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