CN106735207A - A kind of preparation method of high-compactness Cu/CuCr gradient composites - Google Patents
A kind of preparation method of high-compactness Cu/CuCr gradient composites Download PDFInfo
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- CN106735207A CN106735207A CN201611146787.8A CN201611146787A CN106735207A CN 106735207 A CN106735207 A CN 106735207A CN 201611146787 A CN201611146787 A CN 201611146787A CN 106735207 A CN106735207 A CN 106735207A
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000007596 consolidation process Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000000956 alloy Substances 0.000 claims description 15
- 229910045601 alloy Inorganic materials 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 41
- ZTXONRUJVYXVTJ-UHFFFAOYSA-N chromium copper Chemical compound [Cr][Cu][Cr] ZTXONRUJVYXVTJ-UHFFFAOYSA-N 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000000678 plasma activation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of preparation method of high-compactness Cu/CuCr gradient composites, it is to carry out consolidation to Cu powder and CuCr mixed-powders using discharge plasma sintering technique, by designing gradient temperature, 5~10min is incubated after applying to be heated to 700~900 DEG C with 50~200 DEG C/min while axial compressive force, you can obtain 10~50mm of diameter, draw ratio 0.1~1.0, consistency more than 99.0%, low gas content amount, electric-conductivity heat-conductivity high, the Cu/CuCr gradient composites of fine microstructures.The present invention can select different sintering conditions according to the size of Cu/CuCr gradient composites and proportioning demand, and process is simple, energy consumption are low, and gained Cu/CuCr gradient composites can be used as contact material of vacuum switch and excellent performance through a small amount of processing.
Description
Technical field
The present invention relates to plastic forming technology and PM technique, and in particular to a kind of high-compactness Cu/CuCr gradients
The preparation method of composite.
Background technology
At present, the contact material mainly acid bronze alloy that vacuum switch is used, wherein chromiumcopper is due to higher
Dieletric strength, big breaking current ability, good resistance fusion welding and relatively low current-carrying value and it is widely used.
The performance of contact material of chrome copper alloy is in close relations with its consistency.The relative density of chromiumcopper is improved, its power
Learn performance and electric conductivity is improved therewith, be favorably improved the performances such as the Breaking capacity of contact, anti-galvanic corrosion ability, anti-melting welding.Separately
On the one hand, the residual porosity inside alloy can produce liquid metals to splash under arcing, and in the acid of contact process and assemble
Wash and in electroplating process, be difficult to remove behind liquid inlet handhole hole, corrosion material.The consistency of traditional sintering CuCr alloy materials
About 95% or so, and be difficult to be improved again；And discharge plasma sintering technique (SPS), it is through powder using flash DC current
End or mould produce Joule heat and a kind of rapidly solidified shaping new technology direct-fired to powder, can significantly reduce forming temperature
And curring time, and plasma activation, discharge impact pressure and electric field-assisted diffusion effect etc. is produced in powder particle gap
Serial special effects, prepared CuCr alloy consistency is up to 99.8%.Additionally, both need not during using SPS consolidated powders
Preform is carried out to powder, it is not required that any lubricant of addition, there is short route, environmental protection, precision form.
Be the performance high for ensureing chromiumcopper, its conductive and heat-conductive ability, consistency, air content etc. be all to close because
Element.The electric conductivity of material is better, then the Breaking capacity for switching is bigger；Heat conductivility is better, then be more conducive to switch to radiate, and carries
Breaking capacity high, electrical erosion resistance performance and used life.In chromiumcopper, its electrical and thermal conductivity performance is completed mainly by copper, therefore
Copper and chromiumcopper are combined and are made graded alloy, be expected to improve its conductive and heat-conductive ability.
Laser welding technology, but laser welding technology being used the preparation of current Cu/CuCr graded alloy in faying face more
Easily produce stomata, fire check and harmful phase.The discharge plasma sintering technique that the present invention is used is by rationally design sintering
Mould, the Temperature Distribution being varied and controlled in mould, can prepare the high-compactness graded composite that conventional sintering method cannot be prepared
Material.Further, since the bulk composition of Cu/CuCr graded alloy is copper, can be prevented effectively from due to composition using powder sintering
The interface problem that difference is brought, such as thermal expansion coefficient difference cause interfacial stress mismatch and form micro-crack.Therefore, use
Discharge plasma sintering technique is expected to obtain the low Cu/CuCr gradient composites of high-compactness, electric-conductivity heat-conductivity high, air content.
The content of the invention
For the copper-based contact tip composite material of existing high-performance, especially Cu/CuCr gradient composites preparation method not
Foot part, it is an object of the invention to use discharge plasma sintering technique, by designing gradient temperature, there is provided a kind of height is caused
Density, electric-conductivity heat-conductivity high, the preparation method of the Cu/CuCr functionally gradient material (FGM)s of low gas content amount.
The present invention solves technical problem, adopts the following technical scheme that：
The preparation method of high-compactness Cu/CuCr gradient composites of the present invention, its feature is：Using plasma discharging
Sintering technology carries out consolidation to Cu powder and CuCr mixed-powders, by designing gradient temperature, applies axial mechanical pressure
While be heated to 700~900 DEG C with the heating rate of 50~200 DEG C/min after be incubated 5~10min, you can obtain high fine and close
Degree Cu/CuCr gradient composites.Specifically include following steps：
Step 1, the Ni metal powder for being not more than 200 mesh less than 500ppm, particle diameter from oxygen content；It is less than from oxygen content
The metal Cr powder of 800ppm, particle diameter between 80 mesh~240 mesh；
Composition according to required CuCr alloys weighs Cu powder and Cr powder, is mixed 10 hours using mechanical mixing, obtains equal
Even CuCr mixed-powders；
According to the ratio of Cu and CuCr in the size and composite of required Cu/CuCr gradient composites, weigh certain
The Cu powder and CuCr mixed-powders of amount are standby；
Step 2, Cu powder and CuCr mixed-powders are sequentially loaded into sintering graphite mould；According to required Cu/CuCr gradients
The ratio of Cu and CuCr in the size and composite of composite, adjusts the height and powder green bodies of upper and lower pressure head in mould
Position in tool；
Precompressed is carried out to the powder for installing using hand-operated hydraulic press, pressure is 8~12MPa；
Step 3, the thick carbon felt of the 4~6mm contour with graphite jig is wrapped in the graphite jig periphery for installing powder, then
It is placed in the furnace chamber of discharge plasma sintering stove, is evacuated to below 5Pa, shaping is sintered to powder；Sintering process
For：
Sintering pressure：10~60MPa；
Sintering temperature：700~900 DEG C；
Heating rate：50~300 DEG C/min；
Soaking time：2~15min；
High-compactness Cu/CuCr graded composite alloys, a diameter of 10~50mm of alloy, draw ratio are obtained after furnace cooling
It is 0.1~1.0.
Advantages of the present invention is embodied in：
1st, Cu/CuCr graded alloy, complex procedures, high cost, and composition surface are prepared and is easily produced using welding method and lacked
Fall into the electrical and thermal conductivity performance of influence material.And sintering method of the invention is performance (such as conductive and heat-conductive according to needed for composite
Performance), the ratio of Cu and CuCr in regulation composite, further according to the size and composite of Cu/CuCr gradient composites
The ratio of middle Cu and CuCr, using discharge plasma sintering technique, in same mould by adjust upper and lower fall head and
Powder green bodies position in a mold builds gradient temperature, realizes the consolidation of Cu powder and CuCr mixed-powders, obtains
Obtained the Cu/CuCr graded composite alloys of high-compactness, electric-conductivity heat-conductivity high and low gas content amount, operation is simple and low cost.
2nd, present invention optimizes the preparation technology of Cu/CuCr graded composite contact materials, under optimal conditions of the invention,
The advantage of the preparation technology can be given full play to, the Cu/CuCr gradients for obtaining high-compactness, electric-conductivity heat-conductivity high and low gas content amount are answered
Condensation material.
Specific embodiment
By following examples, the present 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
Amount is less than the metal Cr powder of 800ppm, particle diameter between 80 mesh~240 mesh.
Discharge plasma sintering stove used be LABOX-350 electric discharges of Japanese Sinter Land Inc companies production etc. from
Sub- sintering system, its current type is DC pulse current, and pulse train is 40:7.
Embodiment 1
The preparation of the present embodiment Cu/CuCr gradient composites is carried out as follows：
Step 1, Cu powder 700g, Cr powder 300g are weighed respectively, using mechanical mixing mixing 10h, obtain uniform CuCr
Mixed-powder；
Step 2,10g Cu powder and 8g CuCr mixed-powders are loaded into sintering graphite mould successively；Regulation sintering stone
The black upper and lower fall head of mould and powder green bodies position in a mold；The powder for installing is carried out using hand-operated hydraulic press
Precompressed, pressure is~10MPa；
Step 3, the graphite jig that will install powder superscribe the carbon felt contour with graphite jig, and its thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to below 5Pa, be passed through DC pulse current is carried out to powder
Thermal sintering.Its sintering process is as follows：
Sintering pressure：30MPa；
Sintering temperature：850℃；
Heating rate：100℃/min；
Soaking time：5min；
The Cu/CuCr graded composite alloys of a diameter of Φ 20mm are obtained after furnace cooling, its density is 8.60g/cm3,
Consistency is 99.7%, and oxygen content is 300ppm.
Embodiment 2
The preparation of the Cu/CuCr gradient composites of the present embodiment is carried out as follows：
Step 1, Cu powder 700g, Cr powder 300g are weighed respectively, using mechanical mixing mixing 10h, obtain uniform CuCr
Mixed-powder；
Step 2,10g Cu powder and 8g CuCr mixed-powders are loaded into mould successively；Adjust upper and lower fall head and
Powder green bodies position in a mold；Precompressed is carried out to the powder for installing using hand-operated hydraulic press, pressure is~10MPa；
Step 3, the graphite jig that will install powder superscribe the carbon felt contour with graphite jig, and its thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to below 5Pa, be passed through DC pulse current is carried out to powder
Thermal sintering.Its sintering process is as follows：
Sintering pressure：10MPa；
Sintering temperature：900℃；
Heating rate：300℃/min；
Soaking time：2min；
The Cu/CuCr graded composite alloys of a diameter of Φ 20mm are obtained after furnace cooling, its density is 8.64g/cm3,
Consistency is 99.8%, and oxygen content is 500ppm.
Embodiment 3
The preparation of the Cu/CuCr gradient composites of the present embodiment is carried out as follows：
Step 1, Cu powder 700g, Cr powder 300g are weighed respectively, using mechanical mixing mixing 10h, obtain uniform CuCr
Mixed-powder；
Step 2,10g Cu powder and 8g CuCr mixed-powders are loaded into mould successively；Adjust upper and lower fall head and
Powder green bodies position in a mold；Precompressed is carried out to the powder for installing using hand-operated hydraulic press, pressure is~10MPa；
Step 3, the graphite jig that will install powder superscribe the carbon felt contour with graphite jig, and its thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to below 5Pa, be passed through DC pulse current is carried out to powder
Thermal sintering.Its sintering process is as follows：
Sintering pressure：60MPa；
Sintering temperature：700℃；
Heating rate：50℃/min；
Soaking time：15min；
The Cu/CuCr graded composite alloys of a diameter of Φ 20mm are obtained after furnace cooling, its density is 8.53g/cm3,
Consistency is 99.1%, and oxygen content is 400ppm.
Claims (4)
1. a kind of preparation method of high-compactness Cu/CuCr gradient composites, it is characterised in that：Using discharge plasma sintering
Technology carries out consolidation to Cu powder and CuCr mixed-powders, by designing gradient temperature, applies the same of axial mechanical pressure
When be heated to 700~900 DEG C with the heating rate of 50~200 DEG C/min after be incubated 5~10min, that is, obtain high-compactness Cu/
CuCr gradient composites.
2. preparation method according to claim 1, it is characterised in that comprise the following steps：
Step 1, the Ni metal powder for being not more than 200 mesh less than 500ppm, particle diameter from oxygen content；It is less than from oxygen content
The metal Cr powder of 800ppm, particle diameter between 80 mesh~240 mesh；
Composition according to required CuCr alloys weighs Cu powder and Cr powder, is mixed 10 hours using mechanical mixing, obtains uniform
CuCr mixed-powders；
According to the ratio of Cu and CuCr in the size and composite of required Cu/CuCr gradient composites, weigh a certain amount of
Cu powder and CuCr mixed-powders are standby；
Step 2, Cu powder and CuCr mixed-powders are sequentially loaded into sintering graphite mould；According to required Cu/CuCr graded composites
The ratio of Cu and CuCr in the size and composite of material, adjusts the height and powder green bodies of upper and lower pressure head in a mold
Position；
Precompressed is carried out to the powder for installing using hand-operated hydraulic press, pressure is 8~12MPa；
Step 3, the thick carbon felt of the 4~6mm contour with graphite jig is wrapped in the graphite jig periphery for installing powder, then by it
It is placed in the furnace chamber of discharge plasma sintering stove, is evacuated to below 5Pa, shaping is sintered to powder；Sintering process is：
Sintering pressure：10~60MPa；
Sintering temperature：700~900 DEG C；
Heating rate：50~300 DEG C/min；
Soaking time：2~15min；
High-compactness Cu/CuCr gradient composites are obtained after furnace cooling.
3. the preparation method according to claim 1 or 2, it is characterised in that：Sintering method is according to the Cu/ according to needed for
The ratio of Cu and CuCr in the size and composite of CuCr gradient composites, using discharge plasma sintering technique, same
Gradient temperature is built in one mould by adjusting upper and lower fall head and powder green bodies position in a mold, is realized
The consolidation of Cu powder and CuCr mixed-powders.
4. the preparation method according to claim 1 and 2, it is characterised in that：Prepared Cu/CuCr gradient composites chis
It is very little to be：10~50mm of diameter, draw ratio 0.1~1.0.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502776A (en) * | 2017-08-31 | 2017-12-22 | 陕西斯瑞新材料股份有限公司 | A kind of batch fabrication method of the CuCr alloys of high-compactness high uniformity |
| CN107598172A (en) * | 2017-07-25 | 2018-01-19 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method of gradient multi-layer C uCr composite contact materials |
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
| CN111618297A (en) * | 2020-04-21 | 2020-09-04 | 陕西斯瑞新材料股份有限公司 | Preparation method of rapid sintering forming silver-based contact |
| CN112259278A (en) * | 2020-10-19 | 2021-01-22 | 西安工程大学 | Preparation method of particle composite fiber reinforced copper tin oxide contact material |
| CN112964745A (en) * | 2021-01-31 | 2021-06-15 | 华中科技大学 | Calibration method for preparing amorphous alloy internal temperature field by spark plasma sintering |
| CN113172235A (en) * | 2021-04-02 | 2021-07-27 | 西安交通大学 | Electrical contact preparation method based on multi-material metal synchronous 3D printing technology |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107598172A (en) * | 2017-07-25 | 2018-01-19 | 陕西斯瑞新材料股份有限公司 | A kind of preparation method of gradient multi-layer C uCr composite contact materials |
| CN107502776A (en) * | 2017-08-31 | 2017-12-22 | 陕西斯瑞新材料股份有限公司 | A kind of batch fabrication method of the CuCr alloys of high-compactness high uniformity |
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
| CN111618297A (en) * | 2020-04-21 | 2020-09-04 | 陕西斯瑞新材料股份有限公司 | Preparation method of rapid sintering forming silver-based contact |
| CN112259278A (en) * | 2020-10-19 | 2021-01-22 | 西安工程大学 | Preparation method of particle composite fiber reinforced copper tin oxide contact material |
| CN112259278B (en) * | 2020-10-19 | 2022-05-03 | 西安工程大学 | Preparation method of particle composite fiber reinforced copper tin oxide contact material |
| CN112964745A (en) * | 2021-01-31 | 2021-06-15 | 华中科技大学 | Calibration method for preparing amorphous alloy internal temperature field by spark plasma sintering |
| CN112964745B (en) * | 2021-01-31 | 2022-01-04 | 华中科技大学 | Calibration method for preparing amorphous alloy internal temperature field by spark plasma sintering |
| CN113172235A (en) * | 2021-04-02 | 2021-07-27 | 西安交通大学 | Electrical contact preparation method based on multi-material metal synchronous 3D printing technology |
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| CN106735207B (en) | 2018-06-15 |
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