CN106498205B - A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity - Google Patents
A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity Download PDFInfo
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- CN106498205B CN106498205B CN201611145943.9A CN201611145943A CN106498205B CN 106498205 B CN106498205 B CN 106498205B CN 201611145943 A CN201611145943 A CN 201611145943A CN 106498205 B CN106498205 B CN 106498205B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0425—Copper-based alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention discloses a kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity, it is to carry out consolidation to CuCr mixed-powders using discharge plasma sintering, by optimizing sintering mold structure, 2~8min is incubated while applying axial mechanical pressure after 10~50 DEG C/min is heated to 800~880 DEG C in a manner of step temperature rising, you can acquisition diameter is that 0.04~1.0, consistency is more than 99.0% and fluctuation both axially and radially is less than 1%, the sintering cylinder ingots of composition even tissue not less than 50mm, draw ratio.The present invention can select different sintering condition according to the size requirements of CuCr alloys, and technique is simple, and the cycle is short, and production efficiency is high, gained CuCr alloys through follow-up a small amount of processing can finished product and as the parts of vacuum circuit breaker in high-power power transmission and transforming equipment.
Description
Technical field
The present invention relates to a kind of manufacture method of copper-based vacuum contact material, more particularly to a kind of large scale high-compactness are high
The manufacture method of the CuCr alloys of uniformity.
Background technology
CuCr alloys are used as contact material because having preferable resistance to arc erosion ability and good drop-out current ability
It is widely used in mesohigh vacuum circuit breaker.The performance of CuCr alloys depend primarily on its institutional framework compactness and
Even property.Because the mutual solubility between Cu and Cr is very low, wellability is poor, therefore in considerably long one section of CuCr alloys research and development
In, be all first to prepare to have effigurate porous C r skeletons using powder metallurgic method, then infiltration cu and obtain CuCr conjunctions
Golden product；Cold or hot re-pressing is carried out to the CuCr alloys after infiltration again if necessary, product is reached satisfactory density and strong
Degree.
So far, the manufacture method of CuCr alloys mainly has infiltration method, sintering process and arc melting method.Shaped using first two
Method, Cr keep graininess to be distributed in Cu matrixes, limited by preparation technology substantially, and product always has a certain amount of defect, shadow
Ring the performance and used life of material.
Discharge plasma sintering (SPS) be using flash DC current flow through powder or mould produce Joule heat and to powder
End carries out a kind of new technology of rapidly solidified shaping.The sintering technology can significantly reduce forming temperature and curring time, and in powder
A series of special effectses such as plasma activation, discharge impact pressure and electric field-assisted diffusion effect are produced in last particulate interspaces, are recognized
To be to prepare fine grain, a kind of high efficiency, low cost method of bulk nanometer material.In the recent period, Chinese patent 106086493A is disclosed
A kind of method that fast low temperature sintering prepares CuCr alloy materials, this method are low to the progress of CuCr mixed-powders using SPS
Warm solid-phase sintering.Because SPS is that powder and graphite jig are directly heated by electric current, therefore the quality of sintered body and current density
It is distributed relevant namely in close relations with the size of powder compact and mould, structure and electrical and thermal conductivity performance.Using the burning of routine
Mould is tied, with the increase (sample diameter and thickness increase) of sintered sample size, especially when sintered sample diameter is more than
During 50mm, CURRENT DISTRIBUTION inhomogeneities increase radially and axially, sintering temperature skewness is directly resulted in, and then influence
The composition and structural homogenity of sintered body.Particular, it is important that heat needs the time in powder green bodies and mould inside conduction, because
This improves the inhomogeneities that heating rate will dramatically increase sintering temperature.In addition, with the increase of sintered sample size, sintering
Powder amount increases, and the gas emissions increase in sintering process in powder compact, gas release will be unfavorable for by improving heating rate, from
And influence the consistency of sintered body.Therefore, consider from the heat transfer in sintering process and gas discharge angles degree, prepared using SPS
Large scale sample, heating rate are also unsuitable too fast.It follows that patent 106086493A use and be rapidly heated (heating rate for
50~300 DEG C/min) mode is not suitable for preparing with high-compactness, (diameter is more than the large scale CuCr alloys of high uniformity
50mm)。
To sum up, by feasible sintering mold reasonable in design and optimization sintering process, CuCr alloy plasma dischargings are controlled
CURRENT DISTRIBUTION in sintering process, improve temperature distribution evenness, accelerate gas discharge, be manufacture large scale, high-compactness, into
Divide the key with the CuCr alloys of even tissue.This is particularly important in the application aspect for manufacturing high highly sophisticated products to promoting SPS.
The content of the invention
For existing vacuum contact material, especially high-compactness (relative density is more than 99%), composition even tissue
The weak point of large scale CuCr alloy manufacturing methods, it is an object of the invention to using discharge plasma sintering technique, pass through
Improve mould structure, improve electric current distribution and optimize sintering process parameter, there is provided a kind of large scale high-compactness is high uniformly
The manufacture method of the CuCr alloys of property, to lift the quality of China's vacuum contact material.
The present invention solves technical problem, adopts the following technical scheme that：
The manufacture method of the CuCr alloys of large scale high-compactness high uniformity of the present invention, its feature are：Will be by Cu powder
The CuCr mixed-powders mixed with Cr powder, are put into precompressed in graphite jig, are then placed in discharge plasma sintering system again
In, it is heated to 800~880 DEG C in a manner of step temperature rising in 10~50 DEG C/min while applying axial compressive force, insulation 2~
8min, consolidation is carried out to CuCr mixed-powders, that is, obtain the CuCr alloy cylinder ingots of large scale high-compactness high uniformity.
Specifically comprise the following steps：
Step 1, from oxygen content less than 500ppm, particle diameter be not more than 200 mesh Ni metal powder；It is less than from oxygen content
The metal Cr powder of 800ppm, particle diameter between the mesh of 80 mesh~240；
According to the composition of required CuCr alloys, Cu powder and Cr powder are weighed, using mechanical mixing mixing 10h, is obtained uniform
CuCr mixed-powders；According to required product size, it is standby to weigh a certain amount of CuCr mixed-powders；
Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr
The graphite jig of mixed-powder carries out precompressed, and pressure is 8~12MPa；
Step 3, the thick carbon felts of 4~6mm are wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on
In the burner hearth of discharge plasma sintering system, below 5Pa is evacuated to, is passed through DC pulse current, CuCr mixed-powders are entered
Row consolidation, process conditions are：
Axial compressive force is 10~60MPa；
Heating rate is 10~50 DEG C/min；
Sintering temperature is 800~880 DEG C；
Soaking time is 2~8min；
The CuCr alloy cylinder ingots of large scale high-compactness high uniformity are obtained after furnace cooling, its diameter is not less than
50mm, draw ratio are 0.04~1.0.
Graphite jig used in the present invention include graphite former, graphite liner set and two pressure heads (respectively as seaming chuck and
Push-down head), be symmetrically arranged with the external cylindrical surface of the pressure head it is some axially through air discharge duct, the upper surface of the pressure head
It is provided with radiating blind hole.
The sintering temperature is preferably 820~860 DEG C；Soaking time is preferably 3~5min；Axial compressive force is preferably 20~
40MPa；The heating rate is preferably 10~20 DEG C/min in room temperature to 300 DEG C of sections, and more than 300 DEG C are preferably 30~50
℃/min。
Beneficial effects of the present invention are embodied in：
1st, the present invention improves electric current distribution, accelerates the gas discharge in powder green bodies, adopt by improving mould structure
The batch of the uniform CuCr alloys cylinder ingots of large scale, high-compactness, structural constituent is realized with discharge plasma sintering technique
Shaping, technique is simple, and the cycle is short, and production efficiency is high；Gained CuCr alloys through follow-up a small amount of processing can finished product and be used as big work(
The parts of vacuum circuit breaker in rate power transmission and transforming equipment, it can significantly lift the quality of domestic vacuum contact material.
2nd, present invention optimizes the manufacturing process of large scale CuCr alloys, when axial mechanical pressure, heating rate, sintering temperature
Degree and soaking time be respectively preferably 30MPa, 15 DEG C/min (≤300 DEG C) and 35 DEG C/min (>300 DEG C), 850 DEG C and 5min
When, the advantage of the manufacturing process can be more given full play to, consistency is obtained more than 99.5% and fluctuation both axially and radially is less than
0.3%th, the CuCr alloy products of composition even tissue.
Brief description of the drawings
Fig. 1 is the fractionation floor map of each part of graphite jig used in the present invention；
Fig. 2 is the dimensional structure diagram of pressure head in graphite jig used in the present invention；
Fig. 3 is the profile after graphite jig assembling used in the present invention；
Fig. 4 is that the SEM of the gained CuCr alloy products of the embodiment of the present invention 1 schemes；
Label in figure：1 is graphite former, and 2 be graphite liner set, and 3 be pressure head, and 3a is air discharge duct, and 3b is radiating blind hole, 4
For CuCr mixed-powders.
Embodiment
By following examples, the invention will be further described, but embodiments of the present invention are not limited only to this.
It is not more than the Ni metal powder of 200 mesh less than 500ppm, particle diameter from oxygen content in the following embodiments, is contained from oxygen
Metal Cr powder of the amount less than 800ppm, particle diameter between the mesh of 80 mesh~240；
As shown in Figures 1 to 3, it includes graphite former 1, in graphite to the structural representation of graphite jig used in following embodiments
Bushing 2 and two pressure heads 3 (respectively as seaming chuck and push-down head), be symmetrically arranged with the external cylindrical surface of pressure head it is some vertically
The air discharge duct 3a run through, the upper surface of pressure head are provided with radiating blind hole 3b.Air discharge duct is semi-cylindrical, totally 8, equal in rice font
It is even to be distributed in pressure head external cylindrical surface.The depth of radiating blind hole accounts for the 1/3~2/3 of pressure head total height.In use, by graphite liner set
It is placed in graphite former, then push-down head (radiating blind hole is down) is placed in graphite liner set, then fills CuCr mixed-powders 4
Fill out in graphite liner set, finally seaming chuck (radiating blind hole is upward) is placed in neck bush.The size of graphite jig is by sintering
The size of sample determines.
Discharge plasma sintering stove used is LABOX-6020 electric discharges of Japanese Sinter Land Inc. companies production etc.
Ion sintering system, its current type are DC pulse current, pulse train 40:7.
Embodiment 1
The large scale CuCr alloys of the present embodiment are carried out as follows：
Step 1, Cu powder 7.0kg, Cr powder 3.0kg are weighed respectively, using mechanical mixing mixing 10h, obtain uniform
CuCr mixed-powders；3.35kg CuCr mixed-powders are weighed to be used to sinter；
Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr
The graphite jig of mixed-powder carries out precompressed, and pressure is~10MPa；
Step 3 ,~thick 5mm carbon felt is wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on
In the burner hearth of discharge plasma sintering system, below 5Pa is evacuated to, is passed through DC pulse current, CuCr mixed-powders are entered
Row consolidation, process conditions are：
Axial compressive force is 30MPa；
Heating rate be 15 DEG C/min (≤300 DEG C) and 35 DEG C/min (>300℃)；
Sintering temperature is 850 DEG C；
Soaking time is 5min；
Φ 80mm × 80mm CuCr alloy cylinder ingots are obtained after furnace cooling, its density is 8.31g/cm3(consistency
For 99.6%), the fluctuation of consistency both axially and radially is less than 0.3%.Its SEM figures are as shown in Figure 4, it can be seen that product composition
Uniformly, fine microstructures are uniform.
Embodiment 2
The large scale CuCr alloys of the present embodiment are carried out as follows：
Step 1, Cu powder 14.0kg, Cr powder 6.0kg are weighed respectively, using mechanical mixing mixing 10h, obtain uniform
CuCr mixed-powders；5.66kg CuCr mixed-powders are weighed to be used to sinter；
Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr
The graphite jig of mixed-powder carries out precompressed, and pressure is~10MPa；
Step 3 ,~thick 5mm carbon felt is wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on
In the burner hearth of discharge plasma sintering system, below 5Pa is evacuated to, is passed through DC pulse current, CuCr mixed-powders are entered
Row consolidation, process conditions are：
Axial compressive force is 60MPa；
Heating rate be 10 DEG C/min (≤300 DEG C) and 30 DEG C/min (>300℃)；
Sintering temperature is 800 DEG C；
Soaking time is 8min；
Φ 120mm × 60mm CuCr alloy cylinder ingots are obtained after furnace cooling, its density is 8.28g/cm3It is (fine and close
Spend for 99.3%), the fluctuation of consistency both axially and radially is less than 0.6%, and composition is uniform, and fine microstructures are uniform.
Embodiment 3
The large scale CuCr alloys of the present embodiment are carried out as follows：
Step 1, Cu powder 7.0kg, Cr powder 3.0kg are weighed respectively, using mechanical mixing mixing 10h, obtain uniform
CuCr mixed-powders；655g CuCr mixed-powders are weighed to be used to sinter；
Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr
The graphite jig of mixed-powder carries out precompressed, and pressure is~10MPa；
Step 3 ,~thick 5mm carbon felt is wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on
In the burner hearth of discharge plasma sintering system, below 5Pa is evacuated to, then passes to DC pulse current, to CuCr mixed powders
End carries out consolidation, and process conditions are：
Axial compressive force is 10MPa；
Heating rate be 20 DEG C/min (≤300 DEG C) and 50 DEG C/min (>300℃)；
Sintering temperature is 880 DEG C；
Soaking time is 2min；
Φ 100mm × 10mm CuCr alloy cylinder ingots are obtained after furnace cooling, its density is 8.29g/cm3It is (fine and close
Spend for 99.4%), the fluctuation of consistency both axially and radially is less than 0.5%, and composition is uniform, and fine microstructures are uniform.
Embodiment 4
The large scale CuCr alloys of the present embodiment are carried out as follows：
Step 1, Cu powder 7.0kg, Cr powder 3.0kg are weighed respectively, using mechanical mixing mixing 10h, obtain uniform
CuCr mixed-powders；78.6g CuCr mixed-powders are weighed to be used to sinter；
Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr
The graphite jig of mixed-powder carries out precompressed, and pressure is~10MPa；
Step 3 ,~thick 5mm carbon felt is wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on
In the burner hearth of discharge plasma sintering system, below 5Pa is evacuated to, then passes to DC pulse current, to CuCr mixed powders
End carries out consolidation, and process conditions are：
Axial compressive force is 20MPa；
Heating rate be 20 DEG C/min (≤300 DEG C) and 50 DEG C/min (>300℃)；
Sintering temperature is 840 DEG C；
Soaking time is 3min；
Φ 50mm × 30mm CuCr alloy cylinder ingots are obtained after furnace cooling, its density is 8.30g/cm3(consistency
For 99.5%), the fluctuation of consistency both axially and radially is less than 0.4%, and composition is uniform, fine microstructures are uniform.
Claims (5)
- A kind of 1. manufacture method of the CuCr alloys of large scale high-compactness high uniformity, it is characterised in that：The CuCr mixed-powders that will be mixed by Cu powder and Cr powder, are put into precompressed in graphite jig, are then placed in electric discharge etc. again In ion sintering system, 800~880 are heated in a manner of step temperature rising in 10~50 DEG C/min while applying axial compressive force DEG C, 2~8min is incubated, consolidation is carried out to CuCr mixed-powders, that is, obtains the CuCr of large scale high-compactness high uniformity Alloy cylinder ingots；Specifically comprise the following steps：Step 1,It is not more than the Ni metal powder of 200 mesh less than 500ppm, particle diameter from oxygen content；From oxygen content less than 800ppm, particle diameter Metal Cr powder between the mesh of 80 mesh~240；According to the composition of required CuCr alloys, Cu powder and Cr powder are weighed, using mechanical mixing mixing 10h, is obtained uniform CuCr mixed-powders；According to required product size, it is standby to weigh a certain amount of CuCr mixed-powders；Step 2, weighted CuCr mixed-powders are loaded into graphite jig；Using hand-operated hydraulic press to installing CuCr mixing The graphite jig of powder carries out precompressed, and pressure is 8~12MPa；Step 3, the thick carbon felts of 4~6mm are wrapped in the graphite jig periphery for installing CuCr mixed-powders, be then placed on electric discharge In the burner hearth of plasma agglomeration system, below 5Pa is evacuated to, is passed through DC pulse current, CuCr mixed-powders are consolidated Form shape, process conditions are：Axial compressive force is 10~60MPa；Heating rate is 10~50 DEG C/min；Sintering temperature is 800~880 DEG C；Soaking time is 2~8min；The CuCr alloy cylinder ingots of large scale high-compactness high uniformity are obtained after furnace cooling；Wherein, the graphite jig includes graphite former, graphite liner covers and two pressure heads, right on the external cylindrical surface of the pressure head Claim be provided with it is some axially through air discharge duct, the upper surface of the pressure head is provided with radiating blind hole.
- 2. manufacture method according to claim 1, it is characterised in that manufactured CuCr alloy cylinder ingots sizes are：Directly Footpath is not less than 50mm, and draw ratio is 0.04~1.0.
- 3. manufacture method according to claim 1, it is characterised in that：The heating rate is in room temperature to 300 DEG C of sections 10~20 DEG C/min, more than 300 DEG C are 30~50 DEG C/min.
- 4. manufacture method according to claim 1, it is characterised in that：The sintering temperature is 820~860 DEG C, during insulation Between be 3~5min.
- 5. manufacture method according to claim 1, it is characterised in that：The axial compressive force is 20~40MPa.
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