CN1730207A - Production method of tungsten copper composite powder - Google Patents
Production method of tungsten copper composite powder Download PDFInfo
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- CN1730207A CN1730207A CN 200510021413 CN200510021413A CN1730207A CN 1730207 A CN1730207 A CN 1730207A CN 200510021413 CN200510021413 CN 200510021413 CN 200510021413 A CN200510021413 A CN 200510021413A CN 1730207 A CN1730207 A CN 1730207A
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Abstract
The invention relates to a method for preparing tungsten copper composite powder, which pertains to powder metallurgy domain. The invention takes blue tungsten (W20O58) or violet tungsten (W18O49) and cuprous oxide powder as materials and gets products used to produce tungsten copper composite material of fine grain by mechanical mixing, heat treating and reduce treating. The invention can increase productivity and decrease energy consumption. Compared with process taking WO3+CuO as material, it can deduce response time by 40%, and compared with that taking H2(WO4)+Cu(OH)2 as material it can cancel the step of heat decomposition to change state of oxidation.
Description
Technical field
The invention belongs to the production method of tungsten copper in the field of powder metallurgy (W-Cu) composite powder, particularly oxide and the cuprous oxide with tungsten is the method that raw material is produced class composite W-Cu powder.The class composite W-Cu powder that this method is produced especially is suitable as the fine grain tungsten-copper composite material that raw material production is used for microelectronic industry.
Background technology
The conventional WO that adopts
3With CuO roasting (calcining) under 800 ℃ of left and right sides temperature (phase transition temperature) after mechanical mixture,, handle through reduction again and promptly get class composite W-Cu powder to obtain the W-Cu composite oxides.Though this method has characteristics such as raw material sources are wider, defective such as have sintering temperature and energy consumption height, roasting time is long, productivity ratio is low.In the patent No. is US5,468,457, and denomination of invention is in " method for preparing the W-Cu composite oxides " patent documentation, discloses a kind of with wolframic acid (H at above-mentioned defective
2WO
3) and Cu (OH)
2Replace WO
3Prepare the method for W-Cu composite oxides with CuO as raw material, that is: after at first wolframic acid powder and hydroxide copper powder being mixed in proportion, the WO after slowly dewatering, make both to form dehydration by the thermal decomposition of hydrated state oxide
3New dehydrating mixt with CuO forms by dehydration, the surface area that has increased the two and surface-active, thereby makes this dehydrating mixt can be converted into the W-Cu composite oxides at about 600 ℃ of roasting temperatures.Though this patented technology effectively reduces direct employing WO
3Be mixed with the required sintering temperature of W-Cu composite oxides with CuO, but owing to need H
2WO
4And Cu (OH)
2Mixture carries out slow processed, if dewatering speed is very fast, static reactant layer then will be disturbed, and increase the distance between the reactant particle, stops solid-stately to synthesize and easily scab; In order to prevent that reactant from scabbing, reacting insufficient, in dehydration, require programming rate slowly, bed of material book, when 3～2 ℃/minute of programming rates, require thickness of feed layer only 0.5～0.75.Inch (12.7～19.1mm) lower tungsten, copper content in the raw material in addition, thereby, this method exist again productivity ratio and economic benefit lower, be unfavorable for large-scale industrial production and disadvantages such as industrial waste gas discharge arranged.
Summary of the invention
The production method that the objective of the invention is research on basis of background technology, a kind of class composite W-Cu powder of design; boost productivity and economic benefit, reduce production costs and energy consumption to reach, and technological operation is easy, reliable, be fit to purposes such as industrial scale production.
Solution of the present invention is to adopt active strong blue tungsten (W
20O
58) or purple tungsten (W
18O
49) and cuprous oxide (Cu
2O) produce class composite W-Cu powder for raw material.Its medium blue tungsten heterogeneous microstructure is than WO
3Rough surface, crackle are many and loose, and surface area is big, thus reactive infiltration is good, active strong; The crystal structure and the WO of purple tungsten
3Difference, the loose polycrystal particle group that each bulky grain is formed by numerous needle-likes or columnar grain, its apparent density is low, thereby makes diffusion reaction not only on the surface, also can carry out simultaneously in inside, and surface area is big especially, activity is stronger; And Cu
2Univalent copper ion among the O had not only had oxidisability, but also had had reproducibility, can spontaneously carry out disproportionated reaction.Therefore, adopt blue tungsten or purple tungsten and cuprous oxide to make raw material production class composite W-Cu powder and neither need mechanical activation, also do not need to change WO by dehydration
3Form with CuO; Can realize its purpose.Therefore, the inventive method comprises:
A, mechanical mixture: with blue tungsten (W
20O
58) or purple tungsten (W
18O
49) and cuprous oxide (Cu
2O) powder is that 75～95wt%, Cu content are that the ratio of 25～5wt% places mechanical mixer in W (percentage by weight) content in production composite powder, fully mix, mixed powder;
B, heat treatment: above-mentioned mixed powder is placed not heat-resisting boat with raw material reaction, send into and carry out roasting (calcining) in the high temperature belt oxidation furnace that can push away boat continuously or the converter and handle; Bisque pine dress thickness is 30～45mm, reacts under air 4～6 hours; Programming rate 2.5-4 ℃/minute, to 700 ℃ ± 20 ℃, constant temperature 30～60 minutes, WO
3The CuO composite oxides;
C, reduction are handled: will cross 40～60 mesh sieves by B gained composite oxides, screenings sends in the reduction furnace, reduction was handled 4～6 hours under reducing atmosphere and 800～900 ℃ of temperature, and 40～120 mesh sieves are crossed in the cooling back, promptly get the object class composite W-Cu powder.
The granularity of the blue tungsten of above-mentioned raw materials powder, purple tungsten and cuprous oxide is-200 orders.And described be not heat-resisting alloy steel boat or quartz boat, molybdenum boat with the heat-resisting boat of raw material reaction.Described reducing atmosphere is hydrogen reduction atmosphere or NH
3+ N
2Reducing atmosphere.
The present invention is owing to adopt active strong blue tungsten or purple tungsten is raw material with cuprous oxide, through mix, roasting and reduction processing promptly get object.Correspondence to generating the composite oxides operation stage reaction time then with WO
3+ CuO is that raw material shortens more than 40%, sintering temperature descends nearly 100 ℃; And with H
2WO
4+ Cu (OH)
2For the reaction time of raw material suitable, and need not advance thermal decomposition dehydration to change oxide form, also do not have industrial waste gas and discharge; Thereby it is short to have flow process, and technological operation is easy, reliable, and then can be enhanced about more than once production cost and energy consumption of productivity ratio is lower, and can carry out characteristics such as industrial scale production.
The specific embodiment 1
Present embodiment is an example with the class composite W-Cu powder of producing 1000g and containing W 80wt%, Cu 20wt% and can be used for continue back production fine grain tungsten-copper composite material:
A, mechanical mixture: granularity is blue tungsten 1001.9g of-200 purposes and cuprous oxide (Cu
2O) 225g places in the stainless steel V-type blender and mixed 1.5 hours, gets mixed powder;
B, heat treatment: above-mentioned mixed powder is placed in 150 * 130 * 50mm heat-resisting alloy steel boat, powder pine dress thickness 43mm, send into then in the high temperature belt oxidation furnace of 3 thermals treatment zone, from room temperature with 3.0 ℃/minute programming rate at the uniform velocity push away boat, after being heated to 700 ℃ under the air, constant temperature 40 minutes is cooled to room temperature then, gets WO
3The CuO composite oxides;
C, reduction are handled: the gained composite oxides are packed into after twin rollers is crossed 50 mesh sieves in the heat-resisting alloy steel boat, send in the 11 pipe molybdenum wire furnaces, 5.5 hours, hydrogen flowing quantity 3.8m are handled in reduction under nitrogen atmosphere and 840 ℃ of temperature
3/ hour, air pressure 4500～6000pa; Cold back is crossed 80 mesh sieves and is promptly got class composite W-Cu powder 1000g.
The specific embodiment 2
A, mechanical mixture: granularity is mixed 70 minutes to mixing for the blue tungsten of-200 purposes and each 1127.14g of cuprous oxide and 112.59g place in the stainless steel blender; Get mixed powder.
B, heat treatment: will be by A gained mixed powder; Be loaded in the molybdenum boat, pine dress thickness is 40mm, send into then in the high temperature belt oxidation furnace that pushes away boat continuously, under air at the uniform velocity push away boat and add thermal bake-out to 710 ℃ with 3.5 ℃/minute programming rate from room temperature after, constant temperature 50 minutes, be cooled to room temperature then, WO
3The oxide that CuO is compound;
All the other are all identical with embodiment 1, must contain the class composite W-Cu powder 1000g of W 90wt%, Cu 10wt%.
The specific embodiment 3
Present embodiment is with purple tungsten (W
18O
49) and cuprous oxide be raw material to produce class composite W-Cu powder be example, the granularity of two kinds of raw meal is-200 orders:
A, mechanical mixture: with purple tungsten 1050.12g, cuprous oxide 160.89g, place in the stainless steel V-type blender and fully mixed 70 minutes, get mixed powder;
B, heat treatment: with above-mentioned mixed powder pack in the quartz boat, pine dress thickness 38mm, send in the belt oxidation furnace that pushes away boat continuously, under air, be heated to 700 ℃ ± 10 ℃ with 4 ℃/minute programming rate after, constant temperature 50 minutes, be cooled to room temperature and promptly get WO
3The CuO composite oxides;
C, reduction are handled: after twin rollers is crossed 50 mesh sieves, place quartz boat to send in the 11 pipe molybdenum wire furnaces, at the NH of conventional flow and air pressure above-mentioned composite oxides
3+ N
2Reduction was handled 5.0 hours under atmosphere and the 880 ℃ of temperature, and the cooling back is crossed 100 mesh sieves and promptly got object class composite W-Cu powder 1000g.
Claims (4)
1, a kind of production method of class composite W-Cu powder; This method comprises:
A, mechanical mixture: is that 75～95Wt%, Cu content are that the ratio of 25～5wt% places mechanical mixer with blue tungsten or purple tungsten and cuprous oxide powder in W content in production composite powder, fully mix, mixed powder;
B, heat treatment: above-mentioned mixed powder is placed not heat-resisting boat with raw material reaction, send in the high temperature belt oxidation furnace that can push away boat continuously or the converter and carry out calcination process; Bisque pine dress thickness is 30～45mm, reacts under air 4～6 hours; Programming rate 2.5-4 ℃/minute, to 700 ℃ ± 20 ℃, constant temperature 30～60 minutes, WO
3The CuO composite oxides;
C, reduction are handled: will cross 40～60 mesh sieves by B gained composite oxides, screenings is sent in the reduction furnace, and reduction was handled 4～6 hours under reducing atmosphere and 800～900 ℃ of temperature, and 40～120 mesh sieves are crossed in the cooling back, promptly get the object class composite W-Cu powder.
2, press the production method of the described class composite W-Cu powder of claim 1; The granularity that it is characterized in that the blue tungsten of described raw meal, purple tungsten and cuprous oxide is-200 orders.
3, press the production method of the described class composite W-Cu powder of claim 1; It is characterized in that described heat-resisting boat is heat-resisting alloy steel boat or quartz boat, molybdenum boat.
4, press the production method of the described class composite W-Cu powder of claim 1; It is characterized in that described reducing atmosphere is hydrogen reduction atmosphere or NH
3+ N
2Reducing atmosphere.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510021413 CN1730207A (en) | 2005-08-04 | 2005-08-04 | Production method of tungsten copper composite powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510021413 CN1730207A (en) | 2005-08-04 | 2005-08-04 | Production method of tungsten copper composite powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850420A (en) * | 2010-06-25 | 2010-10-06 | 西安理工大学 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
| CN104001929A (en) * | 2014-06-20 | 2014-08-27 | 阮秀仕 | Method for manufacturing copper and tungsten alloy powder through mechanical alloying |
| CN104785275A (en) * | 2015-03-23 | 2015-07-22 | 北京科技大学 | Preparation method of copper modified violet tungsten oxide photocatalyst |
| CN109014232A (en) * | 2018-08-29 | 2018-12-18 | 北京科技大学 | A method of preparing ultra-fine tungsten-copper composite powder |
-
2005
- 2005-08-04 CN CN 200510021413 patent/CN1730207A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850420A (en) * | 2010-06-25 | 2010-10-06 | 西安理工大学 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
| CN101850420B (en) * | 2010-06-25 | 2012-02-08 | 西安理工大学 | Preparation method of tungsten-cladding-copper nanometer composite powder with controllable thickness of cladding coating |
| CN104001929A (en) * | 2014-06-20 | 2014-08-27 | 阮秀仕 | Method for manufacturing copper and tungsten alloy powder through mechanical alloying |
| CN104001929B (en) * | 2014-06-20 | 2017-02-08 | 福建国福天合电气科技有限公司 | Method for manufacturing copper and tungsten alloy powder through mechanical alloying |
| CN104785275A (en) * | 2015-03-23 | 2015-07-22 | 北京科技大学 | Preparation method of copper modified violet tungsten oxide photocatalyst |
| CN104785275B (en) * | 2015-03-23 | 2017-01-04 | 北京科技大学 | A kind of copper modifies the preparation method of purple tungsten photocatalyst |
| CN109014232A (en) * | 2018-08-29 | 2018-12-18 | 北京科技大学 | A method of preparing ultra-fine tungsten-copper composite powder |
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