CN106756376B - 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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- CN106756376B CN106756376B CN201611062105.5A CN201611062105A CN106756376B CN 106756376 B CN106756376 B CN 106756376B CN 201611062105 A CN201611062105 A CN 201611062105A CN 106756376 B CN106756376 B CN 106756376B
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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 applications.The tungsten-copper alloy includes the following component of mass percentage: copper 4~50%；Tungsten 50~85%；Silver 0.05~15%.Tungsten-copper alloy provided in an embodiment of the present invention is due to being added to silver element, silver improves the wettability of the two in tungsten phase and copper phase, the intergranular defect of tungsten, copper is compensated for simultaneously, eliminate existing gap between alloy, improve the consistency of alloy, so that alloy shows good caking power, and maintain the heating conduction of tungsten-copper alloy not less than 210 DEG C, conductivity 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, in particular to a kind of tungsten-copper alloy and its processing method and application.
Background technique
Tungstem-copper pscudo-alloy has both the high temperature resistant of tungsten and copper, high rigidity, low-expansion coefficient, high heat-conductivity conducting performance, good
The features such as plasticity, is therefore widely used in the fields such as Electronic Packaging, heat sink.
The preparation method of existing tungsten-copper alloy includes: that POROUS TUNGSTEN is that skeleton penetrates into liquid copper, hot compression tungsten-copper composite powder
End further includes the various technologies such as liquid-phase sintering recompression, explosion compression.
But since intersolubility is very small between different component in tungsten-copper system, even if being deposited at 1083 DEG C or more
In liquid copper, tungsten-copper pseudo-alloy is also difficult to realize complete density.Currently, the preparation method of tungsten-copper composite powder mainly has height
Warm reduction method and mechanical alloying method.
High-temperature reducing process is first to react wolframic acid amine salt (or tungsten oxide) to generate 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 ranges
With hydrogen reducing, a kind of tungsten-copper composite powder of tungsten phase coated copper phase is made.Since tungsten-copper is mutually in submicron order distribution, powder
Caking power substantially improves, but still is difficult to reach fully dense sintered density, need to add other additives such as Cr, Co etc. with
The all affinity metal of copper, tungsten, to further increase caking power.But the additive is after sintering, due to being solid-solubilized in
In Copper substrate, the physical properties such as conductive, thermally conductive of tungsten-copper alloy are greatly reduced.
Mechanical alloying method is to be mixed in a certain ratio tungsten and copper, and tungsten-copper composite powder is made by mechanical ball mill.But
Be, due to the difference of the particle size of tungsten and copper, specific gravity and hardness etc., using mechanical alloying method be difficult to be made tungsten and
The equally distributed tungsten-copper composite powder of copper, and the ratio of tungsten and copper is difficult to control accurately in composite powder.Meanwhile in mechanical milling process,
Due to grinding pot or ball abrasion and the impurity such as mixed Fe, Co, Cr will be greatly reduced the physics such as conductive, thermally conductive of tungsten-copper alloy
Performance.
Summary of the invention
It is low for alloy sintering ability existing for current tungsten-copper alloy, and although traditional sintering aids can be improved sintering
Ability, but the problems such as alloy is thermally conductive, electric conductivity reduces, the embodiment of the present invention provides a kind of tungsten-copper alloy and its processing method.
In order to achieve the above-mentioned object of the invention, technical scheme is as follows:
A kind of tungsten-copper alloy, the tungsten-copper alloy include the following component of mass percentage:
Copper 4~50%；
Tungsten 50~85%；
Silver 0.05~15%.
And the processing method of the tungsten-copper alloy, it at least includes the following steps:
The formula of tungsten-copper alloy weighs each raw material component as described above；
The weighed raw material components are subjected to mixed calcining processing, obtain the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are subjected to ball-milling treatment, obtain the nanometer or submicron order W-Cu composite powder of argentiferous；
The wolframic acid copper powders are subjected to reduction treatment, obtain submicron order tungsten copper argentum composite powder end；
Tungsten copper argentum composite powder end is pressed and sintering processes.
The tungsten-copper alloy that the above embodiment of the present invention provides, by being added silver element into tungsten, copper component, silver in tungsten phase and
The intergranular defect of tungsten, copper is compensated in copper phase, is eliminated alloy gap, the consistency of alloy is improved, so that alloy is shown
Good caking power, and it is able to maintain that the heating conduction of tungsten-copper alloy is not less than 30% not less than 210 DEG C, conductivity
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 during the 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 be precipitated, so that silver compensates for the gap between tungsten and copper, tungsten and tungsten, internal voids existing for tungsten-copper alloy are eliminated, are mentioned
The high consistency of alloy, to improve the physical property and mechanical performance of tungsten-copper alloy sintered body；The technique letter of this processing method
Single, equipment requirement is low, and the process-cycle is short, produces suitable for large-scale tungsten-copper alloy.
The tungsten-copper alloy that the above embodiment of the present invention provides compensates for the sky between tungsten and tungsten and tungsten due to the presence of silver
Gap, so that consistency has obtained further raising, meanwhile, good heating conduction and electric conductivity are also maintained, is suitble to use
In Electronic Packaging and heat sink material.
Detailed description of the invention
The oxide powder that Fig. 1 is W-19.7Cu-0.3Ag of embodiment of the present invention pattern after 800 DEG C of calcinings；
The oxide powder that Fig. 2 is W-19.7Cu-0.3Ag of the embodiment of the present invention is after 800 DEG C of calcinings, ratio of grinding media to material 3:1 (matter
Amount), revolving speed 700RPM ball milling 3h powder morphology；
The oxide powder that Fig. 3 is W-19.7Cu-0.3Ag of the embodiment of the present invention is after 800 DEG C of calcinings, ratio of grinding media to material 3:1 (matter
Amount), revolving speed 700RPM ball milling 3h waits powder morphology, the powder morphology after 800 DEG C of reduction 1h in flowing hydrogen；
Fig. 4 is that the W-19.5Cu-0.5Ag of 0.5 mass % silver of addition of the embodiment of the present invention is burnt for 1250 DEG C in hydrogen atmosphere
Scanning electron microscope after tying 1h；
Fig. 5 is that the W-19.5Cu-0.5Ag of 0.5 mass % silver of addition of the embodiment of the present invention is burnt for 1250 DEG C in hydrogen atmosphere
Silver element distribution map after tying 1h；
Fig. 6 is that the W-19.5Cu-0.5Ag of 0.5 mass % silver of addition of the embodiment of the present invention is burnt for 1250 DEG C in hydrogen atmosphere
Copper distribution map after tying 1h.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, 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 mass percentage:
Copper 4~50%；
Tungsten 50~85%；
Silver 0.05~15%.
In any embodiment, silver nanoparticle is distributed in W-Cu composite powder, the silver being solid-solution in copper during the sintering process
The wetability between tungsten copper can be improved, improve powder sintered performance.
Preferably, silver-colored mass percentage is 0.5~5.0%.When silver content is lower than 0.05%, under liquid phase
It is unobvious to the wettability modification between copper/tungsten, when being greater than 0.5%, show obvious wettability；And it is higher than 5%
When, silver content is had more than needed, and improvement is difficult to further increase, and cost of alloy is got higher.
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 greater than 99.9%, the WO3Purity be greater than 99.9%, it is subsequent using such raw material
Ball-milling Time can greatly shorten, can avoid due to other impurities mixed in mechanical milling process or the content mistake of other impurities
Thermal conductivity and electric conductivity high and that influence alloy.
The tungsten-copper alloy that the above embodiment of the present invention provides, by being added to silver element into tungsten, copper component, silver is in tungsten phase
With compensate for the intergranular defect of tungsten, copper in copper phase, eliminate alloy gap, improve the consistency of alloy, so that alloy shows
Good caking power out, and it is able to maintain that the heating conduction of tungsten-copper alloy is not less than 30% not less than 210 DEG C, conductivity
IACS。
The present invention is on the basis of tungsten-copper alloy recipe ingredient provided by the above embodiment, it is further provided the alloy
A kind of processing method.
In one embodiment, the processing method of the tungsten-copper alloy at least includes the following steps, as described above tungsten
The formula of copper alloy weighs the raw material of each component；
The raw material of the weighed component is subjected to mixing and calcination processing, obtains the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are subjected to ball-milling treatment, obtain the nanometer or submicron order W-Cu composite powder of argentiferous；
The wolframic acid copper powders are subjected to reduction treatment, obtain submicron order tungsten copper argentum composite powder end；
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 greater than 99.9%；
The purity of the Ag is greater than 99.9%, the WO3Purity be greater than 99.9%.Using such raw material, to avoid due to depositing
The thermal conductivity and electric conductivity of the alloy of refining are influenced in the too high levels of other impurities or other impurities.
In any embodiment, mixture calcination temperature is 500~900 DEG C, and the calcination time is 0.5~2h.
Natural cooling after calcining, is cooled to room temperature, carries out ball-milling treatment to the wolframic acid copper powders of the argentiferous of acquisition.
Preferably, ball material mass ratio is 1:1~3:1, and rotational speed of ball-mill is 400~900RPM.Under the ball material mixing match,
It can realize that oxide powder forms nanometer or the other W-Cu composite powder of submicron order in a short time.Further preferably
The equipment on ground, 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 the gas other than hydrogen, such as any in 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.
It is cooled to room temperature in hydrogen atmosphere after reduction treatment, is then pressed.The pressure of compression moulding is 10
~530MPa.When the pressing pressure of compression moulding is lower than 10MPa, alloy blank is difficult to form, and when being higher than 50MPa, base
Expect that internal stress increases, will lead to product and deform even cracking during the sintering process.
Preferably, the sintering temperature is 1100~1250 DEG C, and sintering atmosphere is the hydrogen atmosphere of flowing；It is lower than in temperature
At 1100 DEG C, it is difficult to realize sintering densification, when being higher than 1250 DEG C, copper can largely volatilize, it is difficult to guarantee that alloying component is stablized.
Further, further include the cooling in nitrogen atmosphere after sintering processes, avoid sample oxidation.The cooling rate is little
In 3 DEG C/min.When cooling rate is higher than the rate, Ag is difficult out of Cu matrix in sufficiently precipitation and the interface Cu/W or W/W, difficult
To achieve the purpose that improve alloy density and performance, and subsequent ageing treatment is needed, increases material production cost.
The processing method of tungsten-copper alloy provided in an embodiment of the present invention, the silver components of addition will be dissolved during the sintering process
Wetability between tungsten copper in copper, can be improved improves the sintering character of alloy powder, and in cooling procedure, it is silver-colored from copper phase
In be preferentially precipitated so that silver compensates for gap between tungsten and copper, eliminate internal voids existing for tungsten, copper alloy, improve
The consistency of alloy, to improve the physical property and mechanical performance of tungsten-copper alloy sintered body；This processing method simple process, if
Low for requiring, the process-cycle is short, produces suitable for large-scale tungsten-copper alloy.
Further, the tungsten-copper alloy that the embodiment of the present invention obtains compensates for the sky between tungsten and copper due to the presence of silver
Gap, so that consistency has obtained further raising, meanwhile, good heating conduction and electric conductivity are also maintained, is suitble to use
In Electronic Packaging and heat sink material.
The tungsten-copper alloy that embodiment provides in order to better illustrate the present invention, 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.
1 embodiment and comparative example formula table of table
It can be seen in table 1 that having higher sintering close by adding suitable Ag and can obtain under same sintering temperature
The W-Cu-Ag alloy of degree and performance.
From fig. 1, it can be seen that the argentiferous wolframic acid copper powders of calcining are easy to form the solid of bulk, for acquisition side due to temperature height
Just the material of processing is further processed, it is necessary to reduce its partial size by ball milling.
As can be seen from Figure 2, the partial size of powder can achieve sub-micro after ratio of grinding media to material 3:1 (quality), revolving speed 700RPM ball milling 3h
Meter level.It is more crisp since powder is compound, very tiny partial size can be reached in ball milling in short-term.
As can be seen from Figure 3, the reduction W-Cu-Ag alloyed powder that the powder of Fig. 2 obtains after 800 DEG C of reduction 1h in flowing hydrogen
End, since 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 is in hydrogen atmosphere after 1250 DEG C of sintering 1h, through the cold of 2 degree/min
But the alloy structure figure obtained after speed, it can be seen that tissue is very fine and close, and W phase granularity very little, and about 3~4 microns.
Fig. 5,6 for Fig. 4 tissue EPMA Ag and Cu Element area profile.It can be seen that Ag is precipitated and is divided from Cu matrix
It is distributed in the interface W/W and the interface W/Cu of easy stroke sintering defect, greatly improves the consistency of alloy.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (5)
1. a kind of tungsten-copper alloy, it is characterised in that: the tungsten-copper alloy is grouped as by the following group of mass percentage:
Copper 4~50%；
Tungsten 50~85%；
Silver 0.5~5.0%；
The alloy is using CuO, WO3Refine as raw material with Ag；The purity of the CuO is greater than 99.9%；Institute
State WO3Purity be greater than 99.9%；The purity of the Ag is greater than 99.9%；
Raw material components are subjected to mixing and calcination processing, obtain the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are subjected to ball-milling treatment, obtain the nanometer or submicron order W-Cu composite powder of argentiferous；
The wolframic acid copper powders are subjected to reduction treatment, obtain submicron order tungsten copper argentum composite powder end；
Tungsten copper argentum composite powder end is pressed and sintering processes；The sintering temperature is 1100~1250 DEG C, is burnt
Knot atmosphere is the hydrogen atmosphere of flowing；It further include the cooling in nitrogen atmosphere after the sintering processes, the cooling rate is not more than 3
℃/min。
2. a kind of processing method of tungsten-copper alloy as described in claim 1, at least includes the following steps:
The formula of tungsten-copper alloy described in accordance with the claim 1 weighs each raw material component；
The weighed raw material components are subjected to mixing and calcination processing, obtain the wolframic acid copper powders of argentiferous；
The wolframic acid copper powders are subjected to ball-milling treatment, obtain the nanometer or submicron order W-Cu composite powder of argentiferous；
The wolframic acid copper powders are subjected to reduction treatment, obtain submicron order tungsten copper argentum composite powder end；
Tungsten copper argentum composite powder end is pressed and sintering processes.
3. the processing method of tungsten-copper alloy as claimed in claim 2, 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 calcination temperature is 500~900 DEG C, the time 0.5~2 hour；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.
4. the processing method of tungsten-copper alloy as claimed in claim 2, it is characterised in that: the pressure of the compression moulding be 10~
530MPa。
5. the preparation of the processing method of tungsten-copper alloy as described in claim 1 or the tungsten-copper alloy as described in claim 2~4
Application of the tungsten-copper alloy in Electronic Packaging, heat sink.
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Families Citing this family (8)
| 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 |
| CN111390195B (en) * | 2020-03-27 | 2022-05-24 | 陕西理工大学 | Micro-interface quantum scattering-free tungsten-copper alloy and preparation method and application thereof |
| CN111910112B (en) * | 2020-07-01 | 2022-02-11 | 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 |
| 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 |
| 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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| CN1539579A (en) * | 2003-04-22 | 2004-10-27 | 中南大学 | Method for preparing high diffusive composite powder of wolfram steel |
| CN101078068A (en) * | 2007-07-05 | 2007-11-28 | 北京科技大学 | Method for preparing ultra-fine crystal grain tungsten-copper alloy and tungsten-copper alloy |
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