CN104946915A - Preparation method of fine-grained CuCr alloy - Google Patents
Preparation method of fine-grained CuCr alloy Download PDFInfo
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- CN104946915A CN104946915A CN201510382233.7A CN201510382233A CN104946915A CN 104946915 A CN104946915 A CN 104946915A CN 201510382233 A CN201510382233 A CN 201510382233A CN 104946915 A CN104946915 A CN 104946915A
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Abstract
The invention provides a preparation method of a fine-grained CuCr alloy, which comprises the processing steps that (1) an oxygen-free copper block and a chromium block are subjected to induction heating to be molten and dissolved mutually, molten liquid is ejected by argon gas pressure and subjected to centrifugal atomization by a copper roller rotation quenching melt spinning or a water-cooling rotating disk; (2) a fine-grained CuCr alloy material is subjected to ball milling by a high-energy ball mill under argon shield; (3) fine-grained composite CuCr alloy powder is loaded into a mould briquette to be made into a green blank; and (4) the green blank is loaded into a graphite drying pot, and placed in a vacuum sintering furnace to be sintered to form the fine-grained CuCr alloy. In the fine-grained CuCr alloy prepared by the method, the particle sizes of chromium particles are 0.5-10 micrometers, the surface hardness is 65-162HV, and the conductivity is 26.0-80.8% IACS (International Annealed Copper Standard); compared with the existing CuCr alloy with the equivalent chromium content, the particle sizes are reduced obviously, and the alloy performance is improved significantly; and the fine-grained CuCr alloy has more excellent effect in an application of an electrical contact material.
Description
Technical field
The invention belongs to technical field of metal material preparation, particularly a kind of method preparing thin brilliant CuCr alloy.
Background technology
Electrical contact is the contact member of electric switch instrument etc., and bear the task of on-off circuit and load current, therefore, its performance directly affects the reliability service of device for switching.CuCr alloy is the important breakthrough in power vacuum switch development history as the invention of contact material, it largely increases the performance of vacuum switch, through the lasting research and development of many decades, CuCr alloy instead of other material substantially, become mesolow big current vacuum switch preferred material and gradually to high-voltage, Large Copacity, lowly to dam, miniaturization development, therefore the performance of CuCr contact material is had higher requirement.
At present, CuCr contact material is based on CuCr50 alloy and CuCr25 alloy, and production technology rests on former basis always, i.e. method of impregnation, mixed powder sintering method and vacuum melting method, not too large renewal.Method of impregnation is to produce CuCr50 alloy contact material, finished product charge length during production only accounts for about 1/2 of original chromium powder skeleton structure length, due to copper and chromium fusing point differs greatly, interface wetting property is bad each other, infiltration method material heart portion often has shrinkage cavity and infiltration defect and crystal grain is larger; Powder mixing method porosity is up to 3% ~ 5%, and density is low, and these shortcomings seriously reduce the performance of material and the work-ing life of product; Although vacuum melting method can prepare the less CuCr alloy material of crystal grain, the CuCr25 feature organization prepared is chromium dendrite, is unfavorable for the further raising of dieletric strength.The microtexture of CuCr contact material has important impact to its macro property, the electrical property of contact material, as resistance fusion welding, arc ablation resistance and voltage endurance capability are not only relevant with the composition of composition contact material, and it is relevant with the size of composition material crystal grain, chromium particle size is tiny as far as possible and be uniformly distributed in contact surface, with the position avoiding the arc energy when powerful vacuum disconnect switch cut-offs too to concentrate on the comparatively large or segregation of chromium particle size, cause contact surface ablated and affect its conductivity.And chromium particle size is on average at about 70 ~ 180 μm in the final contact product that infiltration method and mixed powder sintering method are produced, with regard to prior art, the super refinement that realize chromium particle in CuCr contact material is also very difficult.
Summary of the invention
For the problem of existing CuCr electrical contact material in processability, the invention provides a kind of method preparing thin brilliant CuCr alloy, make pressed compact through press working again after first preparing the tiny CuCr composite powder of submicron order, eventually pass liquid phase sintering and obtain distributed components and the tiny CuCr alloy of chromium particle.In the CuCr alloy that the inventive method is obtained, chromium particle is tiny, the arc energy when powerful vacuum disconnect switch cut-offs can be avoided when using as electrical contact material too to concentrate on the position of chromium particle size comparatively large or segregation, thus avoid contact surface ablated and affect its conductivity.In addition, the inventive method regulates the mass percentage of chromium in CuCr alloy 10 ~ 50% by controlling thin brilliant composite powder component proportions.The vacuum liquid-phase sintering that the inventive method adopts compares conventional solid sintering significantly can shorten the time, and improve the over-all properties of contact material, and the inventive method is applied widely, obtained electrical contact material meets GBT-26867 standard.Technical scheme of the present invention is as follows:
Prepare a method for thin brilliant CuCr alloy, carry out according to following processing step:
(1) thin brilliant CuCr alloy material is prepared: method one: be the crucible that 1:1 ~ 9:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid ejection is rotated chilling through copper roller and get rid of band, wherein copper roller rotating speed is 1000 ~ 7000r/min, obtains the banded thin brilliant CuCr alloy material of thin slice;
Method two: be the crucible that 1:1 ~ 9:1 puts into bottom belt nozzle according to mass ratio by oxygen-free copper block and chromium block, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid is sprayed through water-cooled rotating disk centrifugal atomizatio, wherein rotating is 1000 ~ 7000r/min, obtains the thin brilliant CuCr alloy material of particulate state;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield thin slice band shape or the thin brilliant CuCr alloy material of particulate state, wherein the mass ratio of ball milling ball and alloy material is 10:1 ~ 3:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 3 ~ 60t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1100 ~ 1500 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 0.5 ~ 3h, obtains thin brilliant CuCr alloy of the present invention.
The purity of described oxygen-free copper block is 99.9%, and the purity of chromium block is 99.9%.
Described argon gas is high-purity argon gas, and purity is 99.99%.
The diameter of described ball milling ball is 3 ~ 10mm.
In described thin brilliant CuCr alloy, chromium grain diameter size is 0.5 ~ 10 μm, and the weight percent of chromium is 10 ~ 50%, and surface hardness is 65 ~ 162 HV, and specific conductivity is 26.0 ~ 80.8% IACS.
Beneficial effect of the present invention is as follows:
1, copper roller chilling gets rid of chromium particle shape in band and the thin brilliant composite Cu Cr alloy powder prepared of water-cooled rotating disk centrifugal atomizatio method is spherical or subsphaeroidal, and surfaces stick is few, and particle size distribution is narrow, uniform composition; In addition, the thin brilliant composite Cu Cr alloy powder yield that these two kinds of methods are prepared is high, and oxygen level is low, can enhance product performance.
2, the thin brilliant CuCr alloy microtexture fine uniform adopting thin brilliant composite Cu Cr alloy powder to prepare, in gained alloy, chromium grain diameter size is 0.5 ~ 10 μm, the chromium of separating out is evenly distributed on Copper substrate mutually, is conducive to follow-up preparation high-performance CuCr alloy contact material.
3, adopt the present invention to prepare CuCr alloy, the special moulding process of adjustment and sintering schedule can be relied on to regulate the content of chromium in alloy.
4, the CuCr alloy surface hardness that prepared by the present invention is 65 ~ 162 HV, specific conductivity is 26.0 ~ 80.8% IACS, and the CuCr alloy of more existing equal chromium content all has remarkable increase, and the application of electrical contact material has more excellent effect.
5, the present invention is few to facility investment, and cost is low, simple to operate, and it is convenient to control, and is easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is the banded thin brilliant CuCr alloy material scanning electron microscope (SEM) photograph of CuCr50 thin slice prepared by the embodiment of the present invention 1;
Fig. 2 is the banded thin brilliant CuCr alloy material scanning electron microscope (SEM) photograph of CuCr25 thin slice prepared by the embodiment of the present invention 2;
Fig. 3 is the partial enlargement scanning electron microscope (SEM) photograph of the banded thin brilliant CuCr alloy material of CuCr25 thin slice of Fig. 2;
Fig. 4 is thin brilliant CuCr25 alloy scanning electron microscope (SEM) photograph prepared by the embodiment of the present invention 2.
Embodiment
It is WK-3 high vacuum preparation of metals system that the copper roller chilling that the invention process adopts gets rid of carrying equipment.
The water-cooled rotating disk centrifugation apparatus that the invention process adopts is YX-1 vacuum metal powder preparation system.
The high energy ball mill that the invention process adopts is SPEX SamplePrep 8000M Mixer/Mill type mechanical ball grinding machine.
The press apparatus that the invention process adopts is 769YP-150F powder compressing machine.
The vacuum sintering furnace model that the invention process adopts is VQS-310.
Embodiment 1
The weight percent preparing chromium is the CuCr alloy of 50%, and processing step is as follows:
(1) thin brilliant CuCr alloy material is prepared: be the crucible that 1:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid ejection is rotated chilling through copper roller and get rid of band, wherein copper roller rotating speed is 1000r/min, obtains the banded thin brilliant CuCr alloy material of thin slice; As shown in Figure 1, wherein chromium grain diameter size is 0.1 ~ 1 μm;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield banded for thin slice thin brilliant CuCr alloy material, wherein the mass ratio of ball milling ball and alloy material is 10:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 3t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1100 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 0.5h, obtains the CuCr alloy of the present embodiment.
The CuCr50 alloy density of the present embodiment is 8.01g/cm
3, hardness is 140HV, specific conductivity 28.7%IACS.
Embodiment 2
The weight percent preparing chromium is the CuCr alloy of 25%, and processing step is as follows:
(1) thin brilliant CuCr alloy material is prepared: be the crucible that 3:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid ejection is rotated chilling through copper roller and get rid of band, wherein copper roller rotating speed is 1000r/min, obtains the banded thin brilliant CuCr alloy material of thin slice; As shown in Fig. 2, Fig. 3, wherein chromium grain diameter size is 0.1 ~ 1 μm
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield banded for thin slice thin brilliant CuCr alloy material, wherein the mass ratio of ball milling ball and alloy material is 3:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 60t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1500 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 3h, obtains the CuCr alloy of the present embodiment.As shown in Figure 4, in obtained alloy material, after sintering, chromium grain diameter size is 0.5 ~ 10 μm.
The CuCr25 alloy density of the present embodiment is 8.01g/cm
3, hardness is 120HV, specific conductivity 35.7%IACS.
Embodiment 3
The weight percent preparing chromium is the CuCr alloy of 50%, and processing step is as follows:
(1) thin brilliant CuCr alloy material is prepared: be the crucible that 1:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid is sprayed through water-cooled rotating disk centrifugal atomizatio, wherein rotating is 7000r/min, obtains the thin brilliant CuCr alloy material of particulate state;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield banded for thin slice thin brilliant CuCr alloy material, wherein the mass ratio of ball milling ball and alloy material is 10:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 60t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1100 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 0.5h, obtains the CuCr alloy of the present embodiment.
The CuCr50 alloy density of the present embodiment is 7.98g/cm
3, hardness is 162HV, specific conductivity 27.2%IACS.
Embodiment 4
The weight percent preparing chromium is the CuCr alloy of 50%, and processing step is as follows:
(1) thin brilliant CuCr alloy material is prepared: be the crucible that 3:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid is sprayed through water-cooled rotating disk centrifugal atomizatio, wherein rotating is 1000r/min, obtains the thin brilliant CuCr alloy material of particulate state;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield banded for thin slice thin peritectic alloy material, wherein the mass ratio of ball milling ball and alloy material is 3:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 3t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1500 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 0.5h, obtains the CuCr alloy of the present embodiment.
The CuCr50 alloy density of the present embodiment is 8.00g/cm
3, hardness is 156HV, specific conductivity 26.0%IACS.
Embodiment 5
The weight percent preparing chromium is the CuCr alloy of 10%, and processing step is as follows:
(1) thin brilliant CuCr alloy material is prepared: be the crucible that 9:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid is sprayed through water-cooled rotating disk centrifugal atomizatio, wherein rotating is 1000r/min, obtains the thin brilliant CuCr alloy material of particulate state;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield banded for thin slice thin peritectic alloy material, the wherein mass ratio 6:1 of ball milling ball and alloy material, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 20t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1500 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 1h, obtains the CuCr alloy of the present embodiment.
The CuCr10 alloy density of the present embodiment is 8.58g/cm
3, hardness is 65HV, specific conductivity 80.8%IACS.
Claims (5)
1. prepare a method for thin brilliant CuCr alloy, it is characterized in that carrying out according to following processing step:
(1) thin brilliant CuCr alloy material is prepared: method one: be the crucible that 1:1 ~ 9:1 puts into bottom belt nozzle by oxygen-free copper block and chromium block according to mass ratio, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid ejection is rotated chilling through copper roller and get rid of band, wherein copper roller rotating speed is 1000 ~ 7000r/min, obtains the banded thin brilliant CuCr alloy material of thin slice;
Method two: be the crucible that 1:1 ~ 9:1 puts into bottom belt nozzle according to mass ratio by oxygen-free copper block and chromium block, induction heating makes copper billet and chromium block melt to dissolve each other, through argon pressurization, melt liquid is sprayed through water-cooled rotating disk centrifugal atomizatio, wherein rotating is 1000 ~ 7000r/min, obtains the thin brilliant CuCr alloy material of particulate state;
(2) the thin brilliant CuCr alloy material of refinement: adopt high energy ball mill to carry out ball milling under argon shield thin slice band shape or the thin brilliant CuCr alloy material of particulate state, wherein the mass ratio of ball milling ball and alloy material is 10:1 ~ 3:1, obtains the thin brilliant composite Cu Cr alloy powder of even particle size distribution;
(3) pressed compact is shaping: thin brilliant composite Cu Cr alloy powder is loaded mould briquetting and makes pressed compact, pressure is 3 ~ 60t;
(4) pressed compact sintering: pressed compact is loaded graphite and does pot, put into vacuum sintering furnace and sinter, wherein vacuum tightness is 1 × 10
-4~ 9 × 10
-3pa, temperature is 1100 ~ 1500 DEG C, carries out liquid phase sintering and furnace cooling after being incubated 0.5 ~ 3h, obtains thin brilliant CuCr alloy.
2. a kind of method preparing thin brilliant CuCr alloy according to claim 1, it is characterized in that the purity of described oxygen-free copper block is 99.9%, the purity of chromium block is 99.9%.
3. a kind of method preparing thin brilliant CuCr alloy according to claim 1, it is characterized in that described argon gas is high-purity argon gas, purity is 99.99%.
4. a kind of method preparing thin brilliant CuCr alloy according to claim 1, is characterized in that the diameter of described ball milling ball is 3 ~ 10mm.
5. a kind of method preparing thin brilliant CuCr alloy according to claim 1, it is characterized in that in described thin brilliant CuCr alloy, chromium grain diameter size is 0.5 ~ 10 μm, the weight percent of chromium is 10 ~ 50%, and surface hardness is 65 ~ 162 HV, and specific conductivity is 26.0 ~ 80.8% IACS.
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