CN102492884A - Preparation method of novel tungsten-copper-zinc alloy material - Google Patents
Preparation method of novel tungsten-copper-zinc alloy material Download PDFInfo
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- CN102492884A CN102492884A CN2011104065302A CN201110406530A CN102492884A CN 102492884 A CN102492884 A CN 102492884A CN 2011104065302 A CN2011104065302 A CN 2011104065302A CN 201110406530 A CN201110406530 A CN 201110406530A CN 102492884 A CN102492884 A CN 102492884A
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Abstract
The invention discloses a preparation method of a tungsten-copper-zinc alloy material. The preparation method comprises the specific processes of: burdening and mixing micro-scale pure tungsten powder, tungsten powder coated by pure copper on the surface as well as micro-scale copper powder and zinc powder, and carrying out cold isostatic extrusion, spark plasma sintering (SPS) and other methods to prepare the tungsten-copper-zinc alloy material with relative density more than 95%. The preparation method has the advantages that: by virtue of the preparation method, the tungsten-copper-zinc composite material with the relative density more than 95%, high hardness and higher strength can be prepared; brass has higher strength and hardness than pure copper; and through combing high strength and high density of tungsten as well as high conductivity, high thermal conductivity, higher strength and hardness and other performances of brass, the high-temperature-resistant and corrosion-resistant tungsten-copper-zinc alloy material suitable for electric spark machining, electronic packaging and aerospace materials are prepared.
Description
Technical field
The present invention relates to the preparation technology of refractory metal and metal composite, belong to metallurgical technology field, especially a kind of preparation method of novel tungsten copper zinc alloy material.
Background technology
The tungsten-based composite material that the present invention relates to is tungsten-copper zinc alloy material.Tungsten-copper composite material has high-density, the low thermal coefficient of expansion of tungsten concurrently; The electric-conductivity heat-conductivity high property that copper is arranged again; Its heat conduction, conductivity and thermal expansivity can design through adjustment tungsten copper component concentration, therefore are widely used in the fields such as broken first material in microwave device, unicircuit packaged material, contact material and the war industry.
The technical matters of preparation tungsten-copper composite material has to dissolve usually oozes two kinds of methods such as method and powder metallurgy sintered method.
Though Tungsten-copper Composites has the advantage of tungsten and copper concurrently, its corresponding shortcoming is arranged also.Because the intensity of fine copper is lower, generally is lower than 200MPa, cause no matter adopting that to dissolve the method for oozing still be that the tungsten-copper composite material intensity and the toughness of powder metallurgy sintered method preparation is difficult to reach request for utilization.
The invention solves the problem that tungsten-copper composite material intensity is low, hardness is low, make freshly prepd tungsten copper zinc alloy material possess the higher hardness of high-density and the brass of tungsten, higher intensity and thermal conductivity, conductivity performance simultaneously.
Summary of the invention
The objective of the invention is to overcome tungsten-copper composite material intensity and the low shortcoming of hardness, provide a kind of and have tungsten and copper advantage concurrently and have tungsten copper zinc alloy composites of higher-strength, high firmness and preparation method thereof.
The present invention solves the problems of the technologies described above the technical scheme of being taked: utilize brass to replace fine copper as the bonding phase in the tungsten-copper composite material; Brass and tungsten coat mutually, connect; Wherein the content of tungsten is 60%～80%; All the other are brass, and utilize discharging plasma sintering equipment that material is carried out electricimpulse thermal treatment, and the phase structure of the inner brass bonding of control tungsten copper zinc alloy material phase is adjusted the material obdurability.
Mass percentage content for above-mentioned tungsten can be 60-80%; The brass bonding mass percent of middle copper mutually can be 59-70%.
Preparing method to above-mentioned tungsten copper zinc alloy material comprises the steps:
(1) prepares burden according to the component content of above-mentioned tungsten copper zinc alloy material, utilize " V " type blender that metal tungsten powder or copper coating tungsten powder, copper powder and metal zinc are mixed by certain mass percent.
(2) alloying element powder that mixes in the step (1) is reduced in nitrogen atmosphere, obtain mixing fully and the mechanical mixture of few oxidized three kinds of pure metal powders.
(3) during the metal-powder after will reducing is packed graphite jig into, utilize discharge plasma to carry out sintering, sintering temperature is 800 ℃～1200 ℃, exerts pressure to be that 20MPa～50MPa, sintered heat insulating time are 1min～5min, and sintering atmosphere is vacuum or argon shield.
(4) alloy material after the sintering preparation is carried out the electricimpulse vacuum heat treatment in discharging plasma sintering equipment; Precipitated phase pattern and composition in the regulation and control alloy structure; It is 400 ℃～800 ℃ that temperature is adopted in thermal treatment, and soaking time is 2h～4h, cools to room temperature with the furnace.
With respect to existing tungsten-copper composite material, the novel tungsten-brass matrix material of the present invention's preparation has following advantage:
The novel tungsten copper zinc alloy material of the present invention preparation is removed HMP, high-density and the low characteristics such as thermal expansivity that possess tungsten, has the high thermal conductivity and the high conductivity of copper concurrently, and this material also has characteristics such as high firmness that brass material has, HS simultaneously.Can carry out vacuum heat treatment through discharging plasma sintering equipment, adjust the intensity and the hardness of material through the phase composite of control brass bonding phase.
Description of drawings
Fig. 1 is the whole pattern of tungsten copper zinc alloy;
Fig. 2 is the local pattern that amplifies of tungsten copper zinc alloy.
Embodiment
Below in conjunction with six specific embodiments, the present invention is further understood in exemplary illustration and help.But the embodiment detail only is for the present invention is described, does not represent the whole technical schemes of the present invention under conceiving, and therefore can not be interpreted as the qualification to technical scheme of the present invention.Some do not depart from the unsubstantiality of the present invention's design changes, and for example simple the change or replacement of technical characterictic to have same or similar technique effect all belongs to rights protection scope of the present invention.
Embodiment 1
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and the middle mutually copper 59% of brass bonding, zinc 41%, the preparation method may further comprise the steps:
Step 1, selecting median size for use is tungsten powder, copper powder and the zinc powder of 2～4 μ m, utilizes hydrogen to reduce behind utilization " V " type blender mixing 24h, obtains the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 800 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out solid state sintering.
Step 3; The tungsten copper zinc alloy material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 600 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten-copper zinc alloy material of bonding phase composite.
Embodiment 2
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and the middle mutually copper 68% of brass bonding, zinc 32%, preparation technology may further comprise the steps:
Step 1, selecting median size for use is tungsten powder, copper powder and the zinc powder of 2～4 μ m, utilizes hydrogen to reduce behind utilization " V " type blender mixing 24h, obtains the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 800 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out solid state sintering.
Step 3; The tungsten copper zinc alloy material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 600 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten copper zinc alloy material of bonding phase composite.
Embodiment 3
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and the middle mutually copper 59% of brass bonding, zinc 41%, the preparation method may further comprise the steps:
Step 1; Utilize the mode of electroless plating to coat layer of copper at tungsten powder surface; Thickness of coating is 50nm; Be to utilize hydrogen to reduce behind copper facing tungsten powder, copper powder and zinc powder utilization " V " the type blender mixing 24h of 2～4 μ m with median size, obtain the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 800 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out solid state sintering.
Step 3; Tungsten-brass material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 600 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten copper zinc alloy material of bonding phase composite.
Embodiment 4
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and the middle mutually copper 59% of brass bonding, zinc 41%, the preparation method may further comprise the steps:
Step 1, selecting median size for use is tungsten powder, copper powder and the zinc powder of 2～4 μ m, utilizes hydrogen to reduce behind utilization " V " type blender mixing 24h, obtains the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 1200 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out liquid phase sintering.
Step 3; The tungsten copper zinc alloy material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 400 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten copper zinc alloy material of bonding phase composite.
Embodiment 5
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and brass bonding phase copper 68%, zinc 32%, preparation technology may further comprise the steps:
Step 1, selecting median size for use is tungsten powder, copper powder and the zinc powder of 2～4 μ m, utilizes hydrogen to reduce behind utilization " V " type blender mixing 24h, obtains the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 1200 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out liquid phase sintering.
Step 3; The tungsten copper zinc alloy material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 400 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten copper zinc alloy material of bonding phase composite.
Embodiment 6
A kind of tungsten copper zinc alloy material comprises following component and content (weight percent): tungsten 80%, and the middle mutually copper 59% of brass bonding, zinc 41%, the preparation method may further comprise the steps:
Step 1; Utilize the mode of electroless plating to coat layer of copper at tungsten powder surface; Thickness of coating is 50nm; Be to utilize hydrogen to reduce behind copper facing tungsten powder, copper powder and zinc powder utilization " V " the type blender mixing 24h of 2～4 μ m with median size, obtain the mixture of purity at three kinds of metal-powders more than 95%.
Step 2 is put into graphite jig with the powder that mixes, and in discharging plasma sintering equipment, carries out vacuum sintering.Sintering process adopts 1200 ℃ of sintering temperatures, and temperature rise rate is 50 ℃/min, and soaking time 5min carries out liquid phase sintering.
Step 3; The tungsten copper Zinc material that sintering is prepared continues in discharging plasma sintering equipment, to heat-treat, and thermal treatment temp adopts 400 ℃, and soaking time is 3h; Cool to room temperature then with the furnace, promptly obtain the tungsten copper zinc alloy material of bonding phase composite.
Claims (6)
1. the preparation method of a novel tungsten copper zinc alloy material, it is characterized in that: the content of tungsten is 60-80% in the said tungsten copper zinc alloy material, and all the other are bonding phase brass, and wherein the mass percent of copper is 59-70%; Its preparation method comprises the steps:
(1) prepares burden according to the component content of above-mentioned tungsten copper zinc alloy material, utilize " V " type blender that metal tungsten powder or copper coating tungsten powder, copper powder and metal zinc are mixed by certain mass percent.
(2) alloying element powder that mixes in the step (1) is reduced in nitrogen atmosphere, obtain mixing fully and the mechanical mixture of few oxidized three kinds of pure metal powders.
(3) during the metal-powder after will reducing is packed graphite jig into, utilize discharge plasma to carry out sintering, sintering temperature is 800 ℃～1200 ℃, exerts pressure to be that 20MPa～50MPa, sintered heat insulating time are 1min～5min, and sintering atmosphere is vacuum or argon shield.
(4) alloy material after the sintering preparation is carried out the electricimpulse vacuum heat treatment in discharging plasma sintering equipment; Precipitated phase pattern and composition in the regulation and control alloy structure; It is 400 ℃～800 ℃ that temperature is adopted in thermal treatment, and soaking time is 2h～4h, cools to room temperature with the furnace.
2. the preparation method of tungsten copper zinc alloy material according to claim 1; It is characterized in that: in the said step (1); The mean particle size of tungsten powder and copper coating tungsten powder, copper powder and zinc powder is 2～4 μ m, and the copper-plated thickness of coating of tungsten powder surface is 20nm～200nm; Hydrogen reduction method is adopted in reduction in the said step (2).
3. according to the preparation method of claim 1 and 2 described tungsten copper zinc alloy material, it is characterized in that: the discharge plasma that utilizes in the step (3) is sintered to solid state sintering, liquid phase sintering or substep sintering.
4. according to the preparation method of claim 1 and 2 described tungsten copper zinc alloy material; It is characterized in that: powder mixes more than the 24h in " V " type blender; Should make powder abundant, and the brass bonding can be distributed between the tungsten particle mutually uniformly after the sinter molding.
5. the preparation method of tungsten copper zinc alloy material according to claim 4 is characterized in that: in the step (4), and the α of thermal treatment control brass bonding phase, the composition of β phase in discharging plasma sintering equipment, the component content of control precipitated phase.
6. the preparation method of tungsten copper zinc alloy material according to claim 1 is characterized in that: the density of material is more than 95% behind the sintering, and the median size of tungsten grain is at 3～6 μ m, and the material hardness after the sintering preparation is more than HRC40.
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Cited By (9)
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| CN102925727A (en) * | 2012-11-14 | 2013-02-13 | 武汉理工大学 | Preparation method for high-performance Zn@W-Cu heat composite |
| CN104014792A (en) * | 2014-06-20 | 2014-09-03 | 阮秀仕 | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials |
| CN105256159A (en) * | 2015-10-22 | 2016-01-20 | 清华大学 | Tungsten and copper composite material and application thereof |
| CN106048301A (en) * | 2016-07-21 | 2016-10-26 | 安徽旭晶粉体新材料科技有限公司 | Spray method for preparing tungsten-containing copper alloy powder |
| CN106756159A (en) * | 2016-12-28 | 2017-05-31 | 北京有色金属研究总院 | A kind of preparation method of multilevel hierarchy tungsten particle reinforced aluminum matrix composites |
| CN107245594A (en) * | 2017-06-23 | 2017-10-13 | 歌尔股份有限公司 | The preparation method of powdered metallurgical material |
| CN107475995A (en) * | 2017-07-27 | 2017-12-15 | 巢湖市荣达塑业有限公司 | A kind of balancing weight for being adapted to rotary drum washing machine roller |
| CN112877577A (en) * | 2021-01-12 | 2021-06-01 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN113430439A (en) * | 2021-06-28 | 2021-09-24 | 北京理工大学 | Phase distribution uniformity control method of high-toughness active tungsten alloy |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102925727A (en) * | 2012-11-14 | 2013-02-13 | 武汉理工大学 | Preparation method for high-performance Zn@W-Cu heat composite |
| CN102925727B (en) * | 2012-11-14 | 2015-03-04 | 武汉理工大学 | Preparation method for high-performance Zn@W-Cu heat composite |
| CN104014792A (en) * | 2014-06-20 | 2014-09-03 | 阮秀仕 | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials |
| CN104014792B (en) * | 2014-06-20 | 2016-09-28 | 阮秀仕 | The method using discharge plasma sintering high-performance copper tungsten electric contact material |
| CN105256159A (en) * | 2015-10-22 | 2016-01-20 | 清华大学 | Tungsten and copper composite material and application thereof |
| CN106048301A (en) * | 2016-07-21 | 2016-10-26 | 安徽旭晶粉体新材料科技有限公司 | Spray method for preparing tungsten-containing copper alloy powder |
| CN106756159A (en) * | 2016-12-28 | 2017-05-31 | 北京有色金属研究总院 | A kind of preparation method of multilevel hierarchy tungsten particle reinforced aluminum matrix composites |
| CN106756159B (en) * | 2016-12-28 | 2018-06-15 | 北京有色金属研究总院 | A kind of preparation method of multilevel hierarchy tungsten particle reinforced aluminum matrix composites |
| CN107245594A (en) * | 2017-06-23 | 2017-10-13 | 歌尔股份有限公司 | The preparation method of powdered metallurgical material |
| CN107245594B (en) * | 2017-06-23 | 2019-02-26 | 歌尔股份有限公司 | The preparation method of powdered metallurgical material |
| CN107475995A (en) * | 2017-07-27 | 2017-12-15 | 巢湖市荣达塑业有限公司 | A kind of balancing weight for being adapted to rotary drum washing machine roller |
| CN112877577A (en) * | 2021-01-12 | 2021-06-01 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN112877577B (en) * | 2021-01-12 | 2022-02-08 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN113430439A (en) * | 2021-06-28 | 2021-09-24 | 北京理工大学 | Phase distribution uniformity control method of high-toughness active tungsten alloy |
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