CN106756376A - tungsten-copper alloy and its processing method and application - Google Patents
tungsten-copper alloy and its processing method and application Download PDFInfo
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- CN106756376A CN106756376A CN201611062105.5A CN201611062105A CN106756376A CN 106756376 A CN106756376 A CN 106756376A CN 201611062105 A CN201611062105 A CN 201611062105A CN 106756376 A CN106756376 A CN 106756376A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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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
Abstract
The invention discloses a kind of tungsten-copper alloy and its processing method and application.The tungsten-copper alloy includes the following component of weight/mass percentage composition：Copper 4~50%；Tungsten 50~85%；Silver 0.05~15%.Tungsten-copper alloy provided in an embodiment of the present invention is due to the addition of silver element, silver improves both wettabilities in tungsten phase and copper phase, compensate for the intergranular defect of tungsten, copper simultaneously, eliminate the space existed between alloy, improve the consistency of alloy, so that alloy shows good caking power, and maintain tungsten-copper alloy heat conductivility be not less than 210 DEG C, conductance be not less than 30%IACS.Therefore, it is very suitable for being applied in Electronic Packaging and heat sink material.
Description
Technical field
The invention belongs to technical field of alloy material, more particularly to a kind of tungsten-copper alloy and its processing method and application.
Background technology
Tungstem-copper pscudo-alloy has the high temperature resistant of tungsten and copper, high rigidity, low-expansion coefficient, high heat-conductivity conducting performance, good concurrently
The features such as plasticity, therefore be widely used in the field such as Electronic Packaging, heat sink.
The preparation method of existing tungsten-copper alloy includes：POROUS TUNGSTEN is that skeleton penetrates into liquid copper, hot compression tungsten-copper composite powder
End, also including various technologies such as liquid-phase sintering recompression, blast compressions.
But, because intersolubility is very small between different component in tungsten-copper system, therefore, even if being deposited more than 1083 DEG C
In liquid copper, tungsten-copper pseudo-alloy is also difficult to complete density.Currently, the preparation method of tungsten-copper composite powder mainly has height
Warm reducing process and mechanical alloying method.
High-temperature reducing process is first by wolframic acid amine salt (or tungsten oxide) reaction generation copper tungstate (CuWO3) and tungstic acid
(WO3) tungsten-copper composite oxide power, through ball milling or atomization refinement after, by the alloy powder under 300~500 DEG C of scopes
With hydrogen reducing, a kind of tungsten-copper composite powder of tungsten phase coated copper phase is obtained.Because tungsten-copper is distributed in submicron order, powder
Caking power is substantially improved, but still be difficult to reach fully dense sintered density, it is necessary to add other additives such as Cr, Co etc. with
Copper, tungsten all metals with compatibility, further to improve caking power.But, the additive after sintering, due to being solid-solubilized in
In Copper substrate, the physical properties such as conduction, the heat conduction of tungsten-copper alloy are greatly reduced.
Mechanical alloying method is to mix tungsten and copper by a certain percentage, and tungsten-copper composite powder is obtained by mechanical ball mill.But
Be, due to the difference of the aspects such as the particle size of tungsten and copper, proportion and hardness, using mechanical alloying method it is difficult to be obtained tungsten and
The equally distributed tungsten-copper composite powder of copper, and the ratio of tungsten and copper is difficult to precise control in composite powder.Meanwhile, in mechanical milling process,
The impurity such as Fe, Co, the Cr being mixed into due to the abrasion of grinding pot or ball can substantially reduce the physics such as conduction, the heat conduction of tungsten-copper alloy
Performance.
The content of the invention
The alloy sintering ability existed for current tungsten-copper alloy is low, although and traditional sintering aids can improve sintering
Ability, but alloy heat conduction, electric conductivity are the problems such as reduce, and the embodiment of the present invention provides a kind of tungsten-copper alloy and its processing method.
In order to realize foregoing invention purpose, technical scheme is as follows：
A kind of tungsten-copper alloy, the tungsten-copper alloy includes the following component of weight/mass percentage composition：
Copper 4~50%；
Tungsten 50~85%；
Silver 0.05~15%.
And, the processing method of the tungsten-copper alloy is at least comprised the following steps：
The formula of tungsten-copper alloy weighs each raw material components as described above；
The raw material components that will be weighed carry out mixed calcining treatment, obtain the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are carried out into ball-milling treatment, the nanometer or submicron order W-Cu composite powder of argentiferous is obtained；
The wolframic acid copper powders are carried out into reduction treatment, submicron order tungsten copper argentum composite powder end is obtained；
The tungsten copper argentum composite powder end is pressed and sintering processes.
The tungsten-copper alloy that the above embodiment of the present invention is provided, by adding silver element in tungsten, copper component, silver in tungsten phase and
The intergranular defect of tungsten, copper is compensate in copper phase, alloy space is eliminated, the consistency of alloy is improve so that alloy shows
Good caking power, and be able to maintain that tungsten-copper alloy heat conductivility be not less than 210 DEG C, conductance be not less than 30%
IACS。
The processing method of tungsten-copper alloy provided in an embodiment of the present invention, the silver components of addition, is solid-solution in sintering process
In copper, the wetability between tungsten copper can be improved, improve the sintering character of alloy powder, and in cooling procedure, silver is from copper phase
It is preferential to separate out so that silver compensate for the space between tungsten and copper, tungsten and tungsten, the internal voids of tungsten-copper alloy presence are eliminated, carry
The consistency of alloy high, so as to improve the physical property and mechanical performance of tungsten-copper alloy sintered body；The letter of this processing method technique
Single, equipment requirement is low, and the process-cycle is short, is suitable for large-scale tungsten-copper alloy production.
The above embodiment of the present invention provide tungsten-copper alloy due to silver presence, compensate for tungsten and, the sky between tungsten and tungsten
Gap so that consistency has obtained further raising, meanwhile, good heat conductivility and electric conductivity is also maintained, it is adapted to use
In Electronic Packaging and heat sink material.
Brief description of the drawings
Fig. 1 for embodiment of the present invention W-19.7Cu-0.3Ag oxide powder 800 DEG C calcine after pattern；
After Fig. 2 is calcined for the oxide powder of embodiment of the present invention W-19.7Cu-0.3Ag at 800 DEG C, ratio of grinding media to material 3:1 (matter
Amount), rotating speed 700RPM ball milling 3h powder morphologies；
After Fig. 3 is calcined for the oxide powder of embodiment of the present invention W-19.7Cu-0.3Ag at 800 DEG C, ratio of grinding media to material 3:1 (matter
Amount), rotating speed 700RPM ball millings 3h waits powder morphology, the powder morphology after 800 DEG C of reduction 1h in flowing hydrogen；
Fig. 4 is that the embodiment of the present invention adds the silver-colored W-19.5Cu-0.5Ag of 0.5 mass % 1250 DEG C of burnings in hydrogen atmosphere
ESEM after knot 1h；
Fig. 5 is that the embodiment of the present invention adds the silver-colored W-19.5Cu-0.5Ag of 0.5 mass % 1250 DEG C of burnings in hydrogen atmosphere
Silver element distribution map after knot 1h；
Fig. 6 is that the embodiment of the present invention adds the silver-colored W-19.5Cu-0.5Ag of 0.5 mass % 1250 DEG C of burnings in hydrogen atmosphere
Copper distribution map after knot 1h.
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of tungsten-copper alloy.The tungsten-copper alloy includes the following component of weight/mass percentage composition：
Copper 4~50%；
Tungsten 50~85%；
Silver 0.05~15%.
In any embodiment, silver nanoparticle is distributed in W-Cu composite powder, and the silver in copper is solid-solution in sintering process
The wetability between tungsten copper can be improved, powder sintered performance is improved.
Preferably, silver-colored weight/mass percentage composition is 0.5~5.0%.When silver content is less than 0.05%, under liquid phase
It is unobvious to the wettability modification between copper/tungsten, during more than 0.5%, show obvious wettability；And it is higher than 5%
When, having more than needed occurs in silver content, and improvement is difficult to further raising, and cost of alloy is uprised.
In the component of above-mentioned alloy, using CuO, WO3, Ag refined as raw material, the purity of the CuO is big
In 99.9%；The purity of the Ag is more than the 99.9%, WO3Purity be more than 99.9%, using such raw material, subsequently
Ball-milling Time can greatly shorten, the content mistake of the other impurities or other impurities due to being mixed into mechanical milling process can be avoided
Thermal conductivity and electric conductivity high and that influence alloy.
The tungsten-copper alloy that the above embodiment of the present invention is provided, by the way that to the addition of silver element in tungsten, copper component, silver is in tungsten phase
With compensate for the intergranular defect of tungsten, copper in copper phase, eliminate alloy space, improve the consistency of alloy so that alloy is showed
Go out good caking power, and be able to maintain that tungsten-copper alloy heat conductivility be not less than 210 DEG C, conductance be not less than 30%
IACS。
The present invention is on the basis of the tungsten-copper alloy recipe ingredient that above-described embodiment is provided, it is further provided the alloy
A kind of processing method.
In one embodiment, the processing method of the tungsten-copper alloy is at least comprised the following steps, as described above tungsten
The formula of copper alloy weighs the raw material of each component；
The raw material of the component that will be weighed is mixed and calcination processing, obtains the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are carried out into ball-milling treatment, the nanometer or submicron order W-Cu composite powder of argentiferous is obtained；
The wolframic acid copper powders are carried out into reduction treatment, submicron order tungsten copper argentum composite powder end is obtained；
The tungsten copper argentum composite powder end is pressed and sintering processes.
In above-mentioned processing and treating method, using CuO, WO3, Ag as raw material, the purity of the CuO is more than 99.9%；
The purity of the Ag is more than the 99.9%, WO3Purity be more than 99.9%.Using such raw material, to avoid due to depositing
The thermal conductivity and electric conductivity of the alloy of refining are influenceed in the too high levels of other impurities or other impurities.
In any embodiment, mixture calcining heat is 500~900 DEG C, and the calcination time is 0.5~2h.
Natural cooling after calcining, is cooled to room temperature, and the wolframic acid copper powders of the argentiferous to obtaining carry out ball-milling treatment.
Preferably, ball material mass ratio is 1:1~3:1, rotational speed of ball-mill is 400~900RPM.Under the ball material mixing match,
Can in a short time realize that oxide powder forms nanometer or the other W-Cu composite powder of submicron order.Further preferably
Ground, the equipment of ball-milling treatment uses star-like ball mill.
Preferably, the reducing agent of the reduction is hydrogen；Reduction temperature is 600~800 DEG C；The recovery time is 0.5
~2.5h.It is of course also possible to use any in the gas beyond hydrogen, such as carbon monoxide, hydrogen sulfide, methane, sulfur monoxide
Kind, but due to for reducing gas leakage or contamination accident is avoided the occurrence of, ordinary priority uses hydrogen.
Room temperature is cooled to after reduction treatment in hydrogen atmosphere, is then pressed.Compressing pressure is 10
~530MPa.When compressing pressing pressure is less than 10MPa, alloy blank is difficult to be molded, and when higher than 50MPa, base
Material internal stress increases, and product can be caused to deform even cracking in sintering process.
Preferably, the sintering temperature is 1100~1250 DEG C, and sintering atmosphere is the hydrogen atmosphere of flowing；It is less than in temperature
At 1100 DEG C, it is difficult to realize sintering densification, when higher than 1250 DEG C, copper can largely volatilize, it is difficult to ensure alloying component stabilization.
Further, cooling in nitrogen atmosphere is additionally included in after sintering processes, it is to avoid sample oxidation.The cooldown rate is little
In 3 DEG C/min.When cooldown rate is higher than the speed, Ag is difficult from Cu matrixes in fully precipitation and Cu/W or W/W interfaces, difficult
Improve the purpose of alloy density and performance to reach, and need follow-up Ageing Treatment, increased material production cost.
The processing method of tungsten-copper alloy provided in an embodiment of the present invention, the silver components of addition will the solid solution in sintering process
In the wetability between tungsten copper in copper, can be improved, the sintering character of alloy powder is improved, and in cooling procedure, it is silver-colored from copper phase
In preferentially separate out so that the space that silver compensate between tungsten and copper, eliminate the internal voids that tungsten, copper alloy are present, improve
The consistency of alloy, so as to improve the physical property and mechanical performance of tungsten-copper alloy sintered body；This processing method process is simple, if
Low for requiring, the process-cycle is short, is suitable for large-scale tungsten-copper alloy production.
Further, the tungsten-copper alloy that the embodiment of the present invention is obtained, due to the presence of silver, compensate for the sky between tungsten and copper
Gap so that consistency has obtained further raising, meanwhile, good heat conductivility and electric conductivity is also maintained, it is adapted to use
In Electronic Packaging and heat sink material.
In order to better illustrate tungsten-copper alloy provided in an embodiment of the present invention, it is explained further below by multiple embodiments
Explanation.
Embodiment
To save length, the recipe ingredient of each embodiment and comparative example is listed in Table 1 below.
The embodiment of table 1 and comparative example formula table
It can be seen in table 1 that can obtain close with sintering higher under same sintering temperature by adding appropriate Ag
The W-Cu-Ag alloys of degree and performance.
From fig. 1, it can be seen that the argentiferous wolframic acid copper powders of calcining, because temperature is high, easily form the solid of bulk, for acquisition side
Just it is processed further the material for the treatment of, it is necessary to reduce its particle diameter by ball milling.
As can be seen from Figure 2, in ratio of grinding media to material 3:1 (quality), the particle diameter of powder can reach sub-micro after rotating speed 700RPM ball millings 3h
Meter level.It is more crisp because powder is compound, very tiny particle diameter can be reached in ball milling in short-term.
As can be seen from Figure 3, the reduction W-Cu-Ag alloyed powders that the powder of Fig. 2 is obtained after 800 DEG C of reduction 1h in flowing hydrogen
End, because the recovery time is shorter, powder diameter remains as submicron order, can greatly promote the sintering character of powder.
As can be seen from Figure 4, the W-19.5Cu-0.5Ag of Fig. 3 in hydrogen atmosphere 1250 DEG C sintering 1h after, through the cold of 2 degree/min
But the alloy structure figure for being obtained after speed, it can be seen that tissue is very fine and close, and W phase granularity very littles, about 3~4 microns.
Fig. 5,6 are Ag the and Cu Element area profiles of the EPMA of Fig. 4 tissues.It can be seen that Ag is separated out and divided from Cu matrixes
W/W interfaces and W/Cu interfaces that easy stroke sinters defect are distributed in, the consistency of alloy is greatly improved.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (8)
1. a kind of tungsten-copper alloy, it is characterised in that：Including the following component of weight/mass percentage composition：
Copper 4~50%；
Tungsten 50~85%；
Silver 0.05~15%.
2. tungsten-copper alloy as claimed in claim 1, it is characterised in that：The weight/mass percentage composition of the silver is 0.5~5.0%.
3. tungsten-copper alloy as claimed in claim 1, it is characterised in that：The alloy is using CuO, WO3With Ag as raw material
Refining is carried out to form；The purity of the CuO is more than 99.9%；The WO3Purity be more than 99.9%；The purity of the Ag is more than
99.9%.
4. a kind of processing method of tungsten-copper alloy as described in claims 1 to 3 is any, at least comprises the following steps：
Formula according to any described tungsten-copper alloy of claims 1 to 3 weighs each raw material components；
The raw material components that will be weighed are mixed and calcination processing, obtain the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are carried out into ball-milling treatment, the nanometer or submicron order W-Cu composite powder of argentiferous is obtained；
The wolframic acid copper powders are carried out into reduction treatment, submicron order tungsten copper argentum composite powder end is obtained；
The tungsten copper argentum composite powder end is pressed and sintering processes.
5. the processing method of tungsten-copper alloy as claimed in claim 4, it is characterised in that：In the ball milling, ball material is according to matter
Amount is than being 1:1~3:1,400~900RPM of rotational speed of ball-mill；The calcining heat is 500~900 DEG C, 0.5~2 hour time；Institute
The reducing agent for stating reduction treatment is hydrogen；Reduction temperature is 600~800 DEG C；The recovery time is 0.5~2.5h.
6. the processing method of tungsten-copper alloy as claimed in claim 4, it is characterised in that：The compressing pressure be 10~
530MPa。
7. the processing method of tungsten-copper alloy as claimed in claim 4, it is characterised in that：The sintering temperature is 1100~1250
DEG C, sintering atmosphere is the hydrogen atmosphere of flowing；Cooling in nitrogen atmosphere is additionally included in after the sintering processes, the cooldown rate is not
More than 3 DEG C/min.
8. the processing method system of tungsten-copper alloy as described in claims 1 to 3 or the tungsten-copper alloy as described in claim 4~9
Standby tungsten-copper alloy Electronic Packaging, it is heat sink in application.
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Cited By (8)
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| CN108149101A (en) * | 2017-08-13 | 2018-06-12 | 广东省材料与加工研究所 | A kind of manufacturing process of high-density large-area tungsten-copper alloy life slab |
| CN111390195A (en) * | 2020-03-27 | 2020-07-10 | 陕西理工大学 | Micro-interface quantum-scattering-free tungsten-copper alloy and preparation method and application thereof |
| CN111910112A (en) * | 2020-07-01 | 2020-11-10 | 昆山家锐电子科技有限公司 | Tungsten-copper alloy material and preparation method and application thereof |
| TWI747671B (en) * | 2020-12-18 | 2021-11-21 | 遠東科技大學 | Method for manufacturing homogeneous tungsten-copper alloy |
| CN113695689A (en) * | 2021-09-10 | 2021-11-26 | 贵州群建精密机械有限公司 | Tool electrode for high-temperature alloy electric spark machining |
| CN114318100A (en) * | 2021-12-13 | 2022-04-12 | 合肥工业大学 | Silver-doped tungsten-copper composite material and preparation method thereof |
| CN114932222A (en) * | 2022-06-17 | 2022-08-23 | 合肥工业大学智能制造技术研究院 | Method for improving density of tungsten-copper alloy |
| CN114959333A (en) * | 2022-05-31 | 2022-08-30 | 河源市凯源硬质合金股份有限公司 | Tungsten-copper alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108149101A (en) * | 2017-08-13 | 2018-06-12 | 广东省材料与加工研究所 | A kind of manufacturing process of high-density large-area tungsten-copper alloy life slab |
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| CN114318100A (en) * | 2021-12-13 | 2022-04-12 | 合肥工业大学 | Silver-doped tungsten-copper composite material and preparation method thereof |
| CN114959333A (en) * | 2022-05-31 | 2022-08-30 | 河源市凯源硬质合金股份有限公司 | Tungsten-copper alloy and preparation method thereof |
| CN114959333B (en) * | 2022-05-31 | 2022-11-11 | 河源市凯源硬质合金股份有限公司 | Tungsten-copper alloy and preparation method thereof |
| CN114932222A (en) * | 2022-06-17 | 2022-08-23 | 合肥工业大学智能制造技术研究院 | Method for improving density of tungsten-copper alloy |
| CN114932222B (en) * | 2022-06-17 | 2023-11-07 | 合肥工业大学智能制造技术研究院 | Method for improving density of tungsten-copper alloy |
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