CN102728843B - Preparation method for copper-chromium alloy powder and preparation method for copper-chromium contacts - Google Patents

Preparation method for copper-chromium alloy powder and preparation method for copper-chromium contacts Download PDF

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CN102728843B
CN102728843B CN201210239258.8A CN201210239258A CN102728843B CN 102728843 B CN102728843 B CN 102728843B CN 201210239258 A CN201210239258 A CN 201210239258A CN 102728843 B CN102728843 B CN 102728843B
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preparation
powder
inert gas
copper
alloy
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CN102728843A (en
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刘凯
王小军
王文斌
李刚
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Shaanxi Sirui Advanced Materials Co Ltd
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SHAANXI SIRUI INDUSTRIES Co Ltd
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Abstract

The invention relates to a preparation method for metal powder and applications of the metal powder. The preparation method comprises the following steps of: preparing copper bars and chrome blocks in a mass ratio of (5-9):(1-5); placing the prepared raw materials in a sealed container; vacuumizing the sealed container firstly, so that the internal pressure of the container is less than or equal to 8*10<-2>Pa; feeding inert gas into the container until the internal pressure of the container is -0.06MPa; heating the raw materials to 1600-2000 DEG C, and then carrying out heat preservation for 1-5 minutes at constant temperature so as to obtain alloy liquid; atomizing the alloy liquid in an ultrasonic atomizer, and continuously feeding inert gas into the ultrasonic atomizer while atomizing, wherein the frequency of the atomizer is 50-300 kHz, and the atomization time is 2-6 minutes; and carrying out 30-50 micron screening on the powder obtained through atomization so as to obtain the copper-chromium alloy powder. CuCr alloy crystalline grains obtained by using the preparation method for copper-chromium alloy powder are fine and high in spherical degree; and the contents of gas and impurities in the alloy are significantly reduced, thereby improving the purity of the alloy.

Description

A kind of preparation method of chromiumcopper powder and the preparation method of copper chromium contact
Technical field
The present invention relates to a kind of method of preparing metal dust, and relate to the purposes of this metal dust.
Background technology
CuCr alloy contact material has high proof voltage intensity, large drop-out current ability and good anti-melting welding and lowly dams performance and be widely used in the contact material of vacuum circuit breaker.As the cardia of vacuum circuit breaker, require CuCr alloy must possess following features:
(1) to there be alap gas and impurity content, guarantee that vacuum circuit breaker can not cause arc reignition and melting welding because of venting in interrupting process;
(2) Cu, Cr particle size are tiny as far as possible, are evenly distributed.Guarantee in interrupting process not or excessively to cause arc energy to assemble at Fu Ge place to cause the excessive ablation of contact surface and melting welding and cause failure of interruption because of Cr skewness.
CuCr contact mainly carries out industrial production by infiltration method and powder mixing method at present.The contact mechanical strength that infiltration method is made is better, but Cr particle is thick, easily forms macroscopical pore and component segregation; The contact metallographic structure that powder mixing method is made is even, but crystallite dimension is larger, and gas content is high, and density is low.In order to overcome the shortcoming of these traditional handicrafts, people have proposed other preparation method.Be specifically described as follows.
The technology of preparing of CuCr alloy powder is prepared in the disclosed a kind of vacuum induction melting of Chinese patent 1454417A gas atomization, and still dystectic Cr is in vacuum induction melting process, and temperature is up to 2200-2400 ℃.The temperature of superelevation causes the unstable meeting of crucible to bring impurity and the gas of crucible composition into, not only can not reduce gas and impurity content in alloy, also can bring new impurity into, and twice melting also causes the prolongation of technical process, uncontrollability to increase.
The preparation method of the disclosed a kind of magnetic levitation melting CuCr alloy of Chinese patent 101709393A.This patent has been avoided the pollution to material in conventional vacuum induction melting, but magnetic levitation melting alloy temperature is at 2000-2400 ℃, and cold-crucible and inert gas can not make aluminium alloy cooling evenly and rapidly, easily causes ingot structure thick, top segregation is serious, and property unanimous between the higher and lower levels is poor.
Summary of the invention
For the problem of prior art existence, the invention provides a kind of preparation method of chromiumcopper powder, the chromiumcopper powder sphericity making is high, and particle size high conformity, gas and impurity content are low.
The CuCr alloy grain that the method for chromiumcopper powder of the present invention obtains is tiny, and sphericity is high, and in alloy, the content of gas and impurity significantly reduces, and has improved the degree of purity of alloy.
The preparation method of chromiumcopper powder of the present invention, comprises the following steps:
(1) prepare copper rod and chromium piece with the mass ratio of 5-9:1-5;
(2) the raw material that prepare are placed in to closed container, first vacuumize and make container inner pressure
Figure 2012102392588100002DEST_PATH_IMAGE001
, then be-0.06MPa to passing into inert gas to container inner pressure in container, keep obtaining for constant temperature 1-5 minute aluminium alloy after then raw material being heated to 1600-2000 ℃;
(3) by the atomization in ultrasonic ultrasonic delay line memory of above-mentioned aluminium alloy, atomizer frequency is 50-300kHz, and nebulisation time is 2-6 minute, continues to pass into inert gas when atomization in atomizer;
(4) the screening of the powder obtaining after atomization being crossed to 30-50 micron, obtains chromiumcopper powder.
Preferably, step (3) in, described aluminium alloy is to be poured into evenly in ultrasonic ultrasonic delay line memory with the speed of 100-200kg/h.
Further preferably, described inert gas is at least one of argon gas, helium.
Still more preferably, step (3) in, in passing into inert gas, also pass into hydrogen, the volume that wherein passes into hydrogen is 0~10% of inert gas volume.
More preferably, inert gas is to be passed into evenly in ultrasonic ultrasonic delay line memory with the speed of 100-200kg/h.
Preferably, (2) step is to utilize magnetic force heating raw materials, and the electrical power of magnetic force is 80-90kW.
The preparation method of copper chromium contact of the present invention, its raw material is chromiumcopper powder, it is characterized in that described chromiumcopper powder is to be prepared from by above-mentioned preparation method.
The preparation method of copper chromium contact of the present invention, the copper chromium contact even tissue of acquisition, crystal grain is tiny, and high conformity has good vacuum break performance.
Accompanying drawing explanation
Fig. 1 is the alloy powder pattern photo that the present invention obtains.
Fig. 2 is the copper chromium contact metallographic that uses the present invention to obtain.
The specific embodiment
Embodiment mono-.
(1) prepare copper rod 9.00kg, chromium piece 1.00kg.
By copper rod and chromium packaged enter in the crucible of 10kg water jacketed copper crucible vacuum induction casting furnace (manufacturer: Hua Di metallurgical equipment manufactory of Jinzhou City), first vacuumize and make crucible internal pressure , then be-0.06MPa to passing into inert gas to crucible internal pressure in crucible, then open induction furnace general supply, regulate heating power button on induction furnace control panel to 80kW, in the time that raw material are heated to 1600-2000 ℃, to keep constant temperature 1 minute, obtain aluminium alloy.
(3) above-mentioned aluminium alloy is poured into atomization in ultrasonic ultrasonic delay line memory in ultrasonic ultrasonic delay line memory evenly with the speed of 200kg/h, atomizer frequency is 50kHz, and nebulisation time is 2 minutes, continues to pass into argon gas, helium and hydrogen when atomization in atomizer;
(4) the powder obtaining after atomization is crossed to the screening of 50 microns, obtained chromiumcopper powder.
(5) chromiumcopper powder is placed in to mould and is compressed to density at 6.15-6.89g/cm 3pressed compact, in vacuum sintering furnace, carry out vacuum-sintering, vacuum , sintering temperature 950-1050 ℃, insulation 4-6 hour, closes heating system, is cooled to room temperature and comes out of the stove.Pressed compact after sintering is suppressed again to 8.6g/cm 3above, in vacuum drying oven, carry out annealing in process, vacuum
Figure 507898DEST_PATH_IMAGE001
, annealing temperature is 950-1050 ℃, insulation 3-5 hour, finally closes heating system, is cooled to room temperature and comes out of the stove, and obtains the blank of copper chromium contact.
(6) after tested, every physicochemical property is as follows for the chromiumcopper powder of above-mentioned acquisition and copper chromium contact:
Figure 2012102392588100002DEST_PATH_IMAGE002
?。
Embodiment bis-.
(1) prepare copper rod 7.00kg, chromium piece 3.00kg.
By copper rod and chromium packaged enter in the crucible of 10kg water jacketed copper crucible vacuum induction casting furnace (manufacturer: Hua Di metallurgical equipment manufactory of Jinzhou City), first vacuumize and make crucible internal pressure
Figure 937743DEST_PATH_IMAGE001
, then be-0.06MPa to passing into inert gas to crucible internal pressure in crucible, then open equipment general supply, regulate heating power button on induction furnace control panel to 85kW, in the time that raw material are heated to 1600-2000 ℃, to keep constant temperature 3 minutes, obtain aluminium alloy.
(3) above-mentioned aluminium alloy is poured into atomization in ultrasonic ultrasonic delay line memory in ultrasonic ultrasonic delay line memory evenly with the speed of 150kg/h, atomizer frequency is 100kHz, and nebulisation time is 4 minutes, continues to pass into helium and hydrogen when atomization in atomizer.
(4) the powder obtaining after atomization is crossed to the screening of 50 microns, obtained chromiumcopper powder.
(5) chromiumcopper powder is placed in to mould and is compressed to density at 6.15-6.89g/cm 3pressed compact, in vacuum sintering furnace, carry out vacuum-sintering, vacuum
Figure 179368DEST_PATH_IMAGE001
, sintering temperature 950-1050 ℃, insulation 4-6 hour, closes heating system, is cooled to room temperature and comes out of the stove.Pressed compact after sintering is suppressed again to 8.6g/cm 3above, in vacuum drying oven, carry out annealing in process, vacuum
Figure 454492DEST_PATH_IMAGE001
, annealing temperature is 950-1050 ℃, insulation 3-5 hour, finally closes heating system, is cooled to room temperature and comes out of the stove, and obtains the blank of copper chromium contact.
(6) after tested, every physicochemical property is as follows for the chromiumcopper powder of above-mentioned acquisition and copper chromium contact:
Figure 284913DEST_PATH_IMAGE003
Embodiment tri-.
(1) prepare copper rod 5.00kg, chromium piece 5.00kg.
By copper rod and chromium packaged enter in the crucible of 10kg water jacketed copper crucible vacuum induction casting furnace (manufacturer: Hua Di metallurgical equipment manufactory of Jinzhou City), first vacuumize and make crucible internal pressure
Figure 620080DEST_PATH_IMAGE001
, then be-0.06MPa to passing into inert gas to crucible internal pressure in crucible, then open equipment general supply, regulate heating power button on induction furnace control panel to 90kW, in the time that raw material are heated to 1600-2000 ℃, to keep constant temperature 5 minutes, obtain aluminium alloy.
(3) above-mentioned aluminium alloy is poured into atomization in ultrasonic ultrasonic delay line memory in ultrasonic ultrasonic delay line memory evenly with the speed of 100kg/h, atomizer frequency is 300kHz, and nebulisation time is 6 minutes, continues to pass into argon gas when atomization in atomizer.
(4) the powder obtaining after atomization is crossed to the screening of 50 microns, obtained chromiumcopper powder.
(5) chromiumcopper powder is placed in to mould and is compressed to density at 6.15-6.89g/cm 3pressed compact, in vacuum sintering furnace, carry out vacuum-sintering, vacuum
Figure 349001DEST_PATH_IMAGE001
, sintering temperature 950-1050 ℃, insulation 4-6 hour, closes heating system, is cooled to room temperature and comes out of the stove.Pressed compact after sintering is suppressed again to 8.6g/cm 3above, in vacuum drying oven, carry out annealing in process, vacuum , annealing temperature is 950-1050 ℃, insulation 3-5 hour, finally closes heating system, is cooled to room temperature and comes out of the stove, and obtains the blank of copper chromium contact.
(6) after tested, every physicochemical property is as follows for the chromiumcopper powder of above-mentioned acquisition and copper chromium contact:
Figure 925793DEST_PATH_IMAGE004

Claims (7)

1. a preparation method for chromiumcopper powder, is characterized in that comprising the following steps:
(1) prepare copper rod and chromium piece with the mass ratio of 5-9:1-5;
(2) raw material that prepare are placed in to closed container, first vacuumize and make container inner pressure
Figure 2012102392588100001DEST_PATH_IMAGE001
, then be-0.06MPa to passing into inert gas to container inner pressure in container, keep obtaining for constant temperature 1-5 minute aluminium alloy after then raw material being heated to 1600-2000 ℃;
(3) by the atomization in ultrasonic ultrasonic delay line memory of above-mentioned aluminium alloy, atomizer frequency is 50-300kHz, and nebulisation time is 2-6 minute, continues to pass into inert gas when atomization in atomizer;
(4) powder obtaining after atomization is crossed to the screening of 30-50 micron, obtained chromiumcopper powder.
2. the preparation method of chromiumcopper powder as claimed in claim 1, is characterized in that step (3), and described aluminium alloy is to be poured into evenly in ultrasonic ultrasonic delay line memory with the speed of 100-200kg/h.
3. the preparation method of chromiumcopper powder as claimed in claim 1 or 2, is characterized in that described inert gas is at least one of argon gas, helium.
4. the preparation method of chromiumcopper powder as claimed in claim 3, is characterized in that step (3), also passes into hydrogen in passing into inert gas, and the volume that wherein passes into hydrogen is 0~10% of inert gas volume.
5. the preparation method of chromiumcopper powder as claimed in claim 3, is characterized in that inert gas is to be passed into evenly in ultrasonic ultrasonic delay line memory with the speed of 100-200kg/h.
6. the preparation method of chromiumcopper powder as claimed in claim 1, is characterized in that (2) step is to utilize magnetic force heating raw materials, and the electrical power of magnetic force is 80-90kW.
7. a preparation method for copper chromium contact, its raw material is chromiumcopper powder, it is characterized in that described chromiumcopper powder is to be prepared from by preparation method claimed in claim 1.
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CN106191511B (en) * 2016-08-05 2018-01-09 陕西斯瑞新材料股份有限公司 The preparation method of copper-chromium contact material
CN106086493B (en) * 2016-08-18 2018-02-09 江西理工大学 A kind of method that fast low temperature sintering prepares CuCr alloy materials
CN106710897B (en) * 2016-12-28 2018-05-25 陕西斯瑞新材料股份有限公司 A kind of preparation method of copper chromium composite contact
CN107671299A (en) * 2017-08-30 2018-02-09 西安理工大学 A kind of method that vacuum aerosolization prepares Cu Cr alloy powders
CN108441670B (en) * 2018-03-19 2020-06-16 陕西斯瑞新材料股份有限公司 Method for preparing copper-chromium 50 electric contact material by using vacuum consumable electrode arc furnace
CN109182833B (en) * 2018-08-28 2020-11-06 合肥工业大学 Copper-based powder metallurgy pantograph pan material taking spherical chromium powder as strengthening phase and preparation method thereof
CN113293309A (en) * 2021-04-09 2021-08-24 陕西斯瑞新材料股份有限公司 Vacuum consumable arc melting copper-chromium contact material structure optimization method
CN114042921B (en) * 2021-11-16 2024-03-22 宁波江丰电子材料股份有限公司 Chromium-silicon alloy powder and preparation method and application thereof

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JP2705998B2 (en) * 1990-08-02 1998-01-28 株式会社明電舎 Manufacturing method of electrical contact material
US5352404A (en) * 1991-10-25 1994-10-04 Kabushiki Kaisha Meidensha Process for forming contact material including the step of preparing chromium with an oxygen content substantially reduced to less than 0.1 wt. %
CN1219898C (en) * 2001-12-10 2005-09-21 北京有色金属研究总院 Alloy powders for preparing CuCr alloy probe material and preparation thereof
CN101709393A (en) * 2009-10-29 2010-05-19 重庆理工大学 Method for preparing contact material having high performance and low mixed copper-chromium alloy content

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Address after: 710077 high tech Zone, Shaanxi, Xi'an Zhang Road No. 87, No. 12

Patentee after: SHAANXI SIRUI ADVANCED MATERIALS CO., LTD.

Address before: Xi'an City, Shaanxi province 710077 fish of the village fish bucket Road No. 273

Patentee before: Shaanxi Sirui Industries Co., Ltd.