CN104946915B - A kind of method for preparing fine grain CuCr alloys - Google Patents
A kind of method for preparing fine grain CuCr alloys Download PDFInfo
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Abstract
The present invention provides a kind of method for preparing fine grain CuCr alloys, and processing step is：（1）Make copper billet melt with chromium block oxygen-free copper block and chromium block sensing heating to dissolve each other, melt liquid is sprayed through argon pressurization and gets rid of band or water cooling rotating disk centrifugal atomizatio by copper roller rotation chilling；（2）Fine grain CuCr alloy materials are subjected to ball milling under argon gas protection using high energy ball mill；（3）Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting；（4）Pressed compact is loaded into the dry pot of graphite, vacuum sintering furnace is put into and is sintered and obtain fine grain CuCr alloys.Fine grain CuCr alloys prepared by the present invention, the particle size of chromium particle is 0.5 ~ 10 μm, case hardness is that 65 ~ 162 HV, electrical conductivity are 26.0 ~ 80.8%IACS, the CuCr alloy particle diameters of more existing equal chromium content are obviously reduced, alloy property is dramatically increased, and has more excellent effect in the application of electrical contact material.
Description
Technical field
The invention belongs to technical field of metal material preparation, more particularly to a kind of method for preparing fine grain CuCr alloys.
Background technology
Electrical contact is the contact element of electric switch instrument and meter etc., bears on-off circuit and load current
Task, therefore, its performance directly affect the reliability service of device for switching.CuCr alloys are electricity as the invention of contact material
Important breakthrough in power vacuum switch development history, it drastically increases the performance of vacuum switch, by persistently grinding for many decades
Study carefully and develop, CuCr alloys instead of other materials substantially, the preferred material as mesolow high current vacuum switch is simultaneously
Gradually to high voltage, Large Copacity, it is low dam, miniaturization develops, therefore the performances of CuCr contact materials is proposed higher
Requirement.
At present, CuCr contact materials are based on CuCr50 alloys and CuCr25 alloys, and production Technology is rested on always
In original basis, i.e. method of impregnation, mixed powder sintering method and vacuum melting method update without too not big.Method of impregnation is to produce CuCr50 alloys
Based on contact material, finished product charge length during production only accounts for 1/2 or so of original chromium powder skeleton structure length, due to copper and chromium
Fusing point differ greatly, each other interface wellability it is bad, infiltration method material center portion often has shrinkage cavity and infiltration defect and crystalline substance
Grain is larger；Powder mixing method porosity is up to 3% ~ 5%, and consistency is low, and these shortcomings seriously reduce the performance of material and making for product
Use the life-span；Although vacuum melting method can prepare the less CuCr alloy materials of crystal grain, the CuCr25 feature organizations prepared
For chromium dendrite, it is unfavorable for the further raising of dieletric strength.The microstructure of CuCr contact materials has weight to its macro property
The influence wanted, the electrical property of contact material, as resistance fusion welding, arc ablation resistance and voltage endurance capability not only with composition contact material
Composition is relevant, and relevant with the size of composition material crystal grain, and chromium particle size is as tiny as possible and uniformly divides in contact surface
Cloth, to avoid when powerful vacuum disconnect switch cut-offs arc energy from excessively concentrating on, chromium particle size is larger or portion of segregation
Position, causes contact surface ablated and influences its electric conductivity.And the final contact product that infiltration method is produced with mixed powder sintering method
Middle chromium particle size is average at 70 ~ 180 μm or so, for prior art, to realize the super of chromium particle in CuCr contact materials
Level refinement is also highly difficult.
The content of the invention
The problem of for existing CuCr electrical contact materials in processability, the present invention provides one kind and prepares fine grain CuCr conjunctions
The method of gold, is made pressed compact through pressure processing again after first preparing the tiny CuCr composite powders of submicron order, eventually passes liquid phase
Distributed components and the tiny CuCr alloys of chromium particle is made in sintering.Chromium particle is thin in CuCr alloys made from the inventive method
It is small, the arc energy when powerful vacuum disconnect switch cut-offs can be avoided excessively to concentrate on chromium when being used as electrical contact material
Particle size is larger or position of segregation, so as to avoid contact surface ablated and influence its electric conductivity.In addition, the inventive method
The weight/mass percentage composition of chromium in CuCr alloys is adjusted 10~50% by controlling fine grain composite powder component ratio.Present invention side
The vacuum liquid-phase sintering that method is used can significantly shorten the time compared to conventional solid sintering, improve the comprehensive of contact material
Can, and the inventive method is applied widely, and obtained electrical contact material meets the standards of GBT- 26867.The technical side of the present invention
Case is as follows：
A kind of method for preparing fine grain CuCr alloys, is carried out according to following processing step：
（1）Prepare fine grain CuCr alloy materials：Method one：According to mass ratio it is 1 by oxygen-free copper block and chromium block：1~9：1 puts
Enter the crucible of bottom belt nozzle, sensing heating makes copper billet be dissolved each other with the fusing of chromium block, melt liquid sprayed through argon pressurization and passed through
Copper roller rotates chilling and gets rid of band, and wherein copper roller rotating speed is 1000~7000r/min, obtains thin slice banding fine grain CuCr alloy materials；
Method two：According to mass ratio it is 1 by oxygen-free copper block and chromium block：1~9：1 is put into the crucible of bottom belt nozzle, sensing
Heating makes copper billet be dissolved each other with the fusing of chromium block, sprays melt liquid through argon pressurization and passes through water cooling rotating disk centrifugal atomizatio, wherein
Rotating is 1000~7000r/min, obtains graininess fine grain CuCr alloy materials；
（2）Refine fine grain CuCr alloy materials：Thin slice banding or graininess fine grain CuCr alloy materials are protected in argon gas
Lower use high energy ball mill carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 10：1~3：1, obtain particle diameter distribution
Uniform fine grain composite Cu Cr alloy powder；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 3~60t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1100~1500 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 0.5~3h, obtains
The fine grain CuCr alloys of the present invention.
The purity of the oxygen-free copper block is 99.9%, and the purity of chromium block is 99.9%.
The argon gas is high-purity argon gas, and purity is 99.99%.
A diameter of 3~10mm of the ball milling ball.
Chromium grain diameter size is 0.5 ~ 10 μm in the fine grain CuCr alloys, and the percentage by weight of chromium is 10~50%,
Case hardness is 65 ~ 162 HV, and electrical conductivity is 26.0 ~ 80.8% IACS.
Beneficial effects of the present invention are as follows：
1st, copper roller chilling gets rid of chromium in the fine grain composite Cu Cr alloy powder that band and water cooling rotating disk centrifugal atomizatio method are prepared
Grain is shaped as spherical or subsphaeroidal, and surfaces stick is few, and particle size distribution is narrow, and composition is uniform；In addition, prepared by both approaches
The fine grain composite Cu Cr alloy powder high income gone out, oxygen content is low, can enhance product performance.
2nd, in the fine grain CuCr alloy microstructure fine uniforms prepared using fine grain composite Cu Cr alloy powder, gained alloy
Chromium grain diameter size is 0.5 ~ 10 μm, and the chromium of precipitation is mutually evenly distributed on Copper substrate, is conducive to subsequently preparing high-performance
CuCr alloy contact material.
3rd, CuCr alloys are prepared using the present invention, alloy can be adjusted by the special moulding process of adjustment and sintering schedule
The content of middle chromium.
4th, the CuCr alloy surfaces hardness for preparing of the present invention is that 65 ~ 162 HV, electrical conductivity are 26.0 ~ 80.8% IACS, compared with
The CuCr alloys of existing equal chromium content are dramatically increased, and have more excellent effect in the application of electrical contact material.
5th, the present invention is few to equipment investment, and cost is low, simple to operate, easy to control, it is easy to accomplish industrialization.
Brief description of the drawings
Fig. 1 is CuCr50 thin slice banding fine grain CuCr alloy material scanning electron microscope (SEM) photographs prepared by the embodiment of the present invention 1；
Fig. 2 is CuCr25 thin slice banding fine grain CuCr alloy material scanning electron microscope (SEM) photographs prepared by the embodiment of the present invention 2；
Fig. 3 is the partial enlargement scanning electron microscope (SEM) photograph of Fig. 2 CuCr25 thin slice banding fine grain CuCr alloy materials；
Fig. 4 is fine grain CuCr25 alloy scanning electron microscope (SEM) photographs prepared by the embodiment of the present invention 2.
Embodiment
The copper roller chilling that the present invention implements to use gets rid of carrying device for WK-3 high vacuum metal preparation systems.
The present invention implements the water cooling rotating disk centrifugation apparatus used for YX-1 vacuum metal powder preparation systems.
The present invention implements the high energy ball mill used for SPEX SamplePrep 8000M Mixer/Mill type mechanical balls
Grinding machine.
The present invention implements the press apparatus used for 769YP-150F powder compressing machines.
The present invention implements the vacuum sintering furnace model VQS-310 used.
Embodiment 1
The percentage by weight for preparing chromium is 50% CuCr alloys, and processing step is as follows：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 1 by oxygen-free copper block and chromium block：1 is put into bottom belt nozzle
Crucible, sensing heating melts copper billet and chromium block to dissolve each other, spray melt liquid through argon pressurization and rotate chilling by copper roller
Band is got rid of, wherein copper roller rotating speed is 1000r/min, obtains thin slice banding fine grain CuCr alloy materials；As shown in figure 1, wherein chromium
Grain particle size is 0.1 ~ 1 μm；
（2）Refine fine grain CuCr alloy materials：Thin slice banding fine grain CuCr alloy materials are used into height under argon gas protection
Energy ball mill carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 10：1, obtain the uniform fine grain of particle diameter distribution and answer
Close CuCr alloyed powders；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 3t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1100 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 0.5h, obtains the present embodiment
CuCr alloys.
The CuCr50 alloy densities of the present embodiment are 8.01g/cm3, hardness is 140HV, electrical conductivity 28.7%IACS.
Embodiment 2
The percentage by weight for preparing chromium is 25% CuCr alloys, and processing step is as follows：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 3 by oxygen-free copper block and chromium block：1 is put into bottom belt nozzle
Crucible, sensing heating melts copper billet and chromium block to dissolve each other, spray melt liquid through argon pressurization and rotate chilling by copper roller
Band is got rid of, wherein copper roller rotating speed is 1000r/min, obtains thin slice banding fine grain CuCr alloy materials；Such as Fig. 2, shown in Fig. 3, wherein
Chromium grain diameter size is 0.1 ~ 1 μm
（2）Refine fine grain CuCr alloy materials：Thin slice banding fine grain CuCr alloy materials are used into height under argon gas protection
Energy ball mill carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 3：1, obtain the uniform fine grain of particle diameter distribution and be combined
CuCr alloyed powders；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 60t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1500 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 3h, obtains the present embodiment
CuCr alloys.As shown in figure 4, chromium grain diameter size is 0.5 ~ 10 μm after being sintered in obtained alloy material.
The CuCr25 alloy densities of the present embodiment are 8.01g/cm3, hardness is 120HV, electrical conductivity 35.7%IACS.
Embodiment 3
The percentage by weight for preparing chromium is 50% CuCr alloys, and processing step is as follows：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 1 by oxygen-free copper block and chromium block：1 is put into bottom belt nozzle
Crucible, sensing heating melts copper billet and chromium block to dissolve each other, through argon pressurization by melt liquid spray by water cooling rotating disk from
The heart is atomized, and wherein rotating is 7000r/min, obtains graininess fine grain CuCr alloy materials；
（2）Refine fine grain CuCr alloy materials：Thin slice banding fine grain CuCr alloy materials are used into height under argon gas protection
Energy ball mill carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 10：1, obtain the uniform fine grain of particle diameter distribution and answer
Close CuCr alloyed powders；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 60t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1100 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 0.5h, obtains the present embodiment
CuCr alloys.
The CuCr50 alloy densities of the present embodiment are 7.98g/cm3, hardness is 162HV, electrical conductivity 27.2%IACS.
Embodiment 4
The percentage by weight for preparing chromium is 50% CuCr alloys, and processing step is as follows：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 3 by oxygen-free copper block and chromium block：1 is put into bottom belt nozzle
Crucible, sensing heating melts copper billet and chromium block to dissolve each other, through argon pressurization by melt liquid spray by water cooling rotating disk from
The heart is atomized, and wherein rotating is 1000r/min, obtains graininess fine grain CuCr alloy materials；
（2）Refine fine grain CuCr alloy materials：Thin slice banding fine grain alloy material is used into high energy ball under argon gas protection
Grinding machine carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 3：1, obtain the uniform fine grain composite Cu Cr of particle diameter distribution
Alloyed powder；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 3t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1500 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 0.5h, obtains the present embodiment
CuCr alloys.
The CuCr50 alloy densities of the present embodiment are 8.00g/cm3, hardness is 156HV, electrical conductivity 26.0%IACS.
Embodiment 5
The percentage by weight for preparing chromium is 10% CuCr alloys, and processing step is as follows：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 9 by oxygen-free copper block and chromium block：1 is put into bottom belt nozzle
Crucible, sensing heating melts copper billet and chromium block to dissolve each other, through argon pressurization by melt liquid spray by water cooling rotating disk from
The heart is atomized, and wherein rotating is 1000r/min, obtains graininess fine grain CuCr alloy materials；
（2）Refine fine grain CuCr alloy materials：Thin slice banding fine grain alloy material is used into high energy ball under argon gas protection
Grinding machine carries out the mass ratio 6 of ball milling, wherein ball milling ball and alloy material：1, obtain the uniform fine grain composite Cu Cr of particle diameter distribution and close
Bronze；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 20t；
（4）Pressed compact is sintered：By pressed compact load the dry pot of graphite, be put into vacuum sintering furnace and be sintered, wherein vacuum be 1 ×
10-4~9 × 10-3Pa, temperature is 1500 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 1h, obtains the present embodiment
CuCr alloys.
The CuCr10 alloy densities of the present embodiment are 8.58g/cm3, hardness is 65HV, electrical conductivity 80.8%IACS.
Claims (4)
1. a kind of method for preparing fine grain CuCr alloys, it is characterised in that carried out according to following processing step：
（1）Prepare fine grain CuCr alloy materials：According to mass ratio it is 1 by oxygen-free copper block and chromium block：1~9：1 is put into bottom belt spray
The crucible of mouth, sensing heating makes copper billet be dissolved each other with the fusing of chromium block, sprays melt liquid through argon pressurization and passes through water cooling rotating disk
Centrifugal atomizing, wherein rotating are 1000~7000r/min, obtain graininess fine grain CuCr alloy materials；
（2）Refine fine grain CuCr alloy materials：Graininess fine grain CuCr alloy materials are used into high-energy ball milling under argon gas protection
Machine carries out ball milling, and the wherein mass ratio of ball milling ball and alloy material is 10：1~3：1, obtain the uniform fine grain of particle diameter distribution and be combined
CuCr alloyed powders；
（3）Pressed compact is molded：Pressed compact is made in fine grain composite Cu Cr alloy powder loading mould briquetting, pressure is 3~60t；
（4）Pressed compact is sintered：Pressed compact is loaded into the dry pot of graphite, vacuum sintering furnace is put into and is sintered, wherein vacuum is 1 × 10-4
~9 × 10-3Pa, temperature is 1100~1500 DEG C, carries out liquid-phase sintering and is incubated furnace cooling after 0.5~3h, obtains fine grain
Chromium grain diameter size is 0.5 ~ 10 μm in CuCr alloys, the fine grain CuCr alloys, and the percentage by weight of chromium is 50%, surface
Hardness is 140 ~ 162 HV, and electrical conductivity is 26.0 ~ 28.7% IACS.
2. a kind of method for preparing fine grain CuCr alloys according to claim 1, it is characterised in that the oxygen-free copper block
Purity is 99.9%, and the purity of chromium block is 99.9%.
3. a kind of method for preparing fine grain CuCr alloys according to claim 1, it is characterised in that the argon gas is high-purity
Argon gas, purity is 99.99%.
4. a kind of method for preparing fine grain CuCr alloys according to claim 1, it is characterised in that the ball milling ball it is straight
Footpath is 3~10mm.
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| US4766274A (en) * | 1988-01-25 | 1988-08-23 | Westinghouse Electric Corp. | Vacuum circuit interrupter contacts containing chromium dispersions |
| DE10010723B4 (en) * | 2000-03-04 | 2005-04-07 | Metalor Technologies International Sa | Method for producing a contact material semifinished product for contact pieces for vacuum switching devices and contact material semi-finished products and contact pieces for vacuum switching devices |
| KR100400356B1 (en) * | 2000-12-06 | 2003-10-04 | 한국과학기술연구원 | Methods of Microstructure Control for Cu-Cr Contact Materials for Vacuum Interrupters |
| CN101540238B (en) * | 2009-04-30 | 2011-06-22 | 西安交通大学 | Preparation process of alloyed copper-chromium contact material |
| CN103060604A (en) * | 2013-01-24 | 2013-04-24 | 陕西斯瑞工业有限责任公司 | Contact material applied to middle-high-voltage vacuum switch-on/off and preparation method for same |
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