CN106735207B - 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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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 48
- 238000005245 sintering Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000007596 consolidation process Methods 0.000 claims abstract description 4
- 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
- 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
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 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 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 42
- 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
- 239000000203 mixture Substances 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
- 230000017525 heat dissipation 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
- 239000002245 particle Substances 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 methods 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 field, 5~10min is kept the temperature after being heated to 700~900 DEG C while applying axial compressive force with 50~200 DEG C/min, you can obtain diameter 10~50mm, draw ratio 0.1~1.0, consistency be more than 99.0%, low gas content amount, electric-conductivity heat-conductivity high, fine microstructures Cu/CuCr gradient composites.The present invention can select different sintering conditions according to the sizes of Cu/CuCr gradient composites and proportioning demand, simple for process, low energy consumption, and gained Cu/CuCr gradient composites can be used as contact material of vacuum switch and have excellent performance through a small amount of processing.
Description
Technical field
The present invention relates to plastic forming technologies and PM technique, and in particular to a kind of high-compactness Cu/CuCr gradients
The preparation method of composite material.
Background technology
At present, the contact material that vacuum switch uses is mainly acid bronze alloy, and wherein chromiumcopper is higher due to having
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 and its consistency are in close relations.The relative density of chromiumcopper improves, power
It learns performance and electric conductivity improves therewith, help to improve Breaking capacity, the performances such as anti-galvanic corrosion ability, anti-melting welding of contact.Separately
On the one hand, the residual porosity inside alloy can generate liquid metals splashing under arcing, and in the acid of contact process and assemble
It washes in electroplating process, is 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 mold generate Joule heat and to powder a kind of direct-fired rapidly solidified forming new technology, forming temperature can be significantly reduced
And curring time, and plasma activation, discharge impact pressure and electric field-assisted diffusion effect etc. one is generated in powder particle gap
Serial special effects, prepared CuCr alloy consistency are up to 99.8%.In addition, using SPS consolidated powders when had not both needed to
Preform is carried out to powder, it is not required that add any lubricant, there is short route, environmental protection, precision form.
To ensure the high performance of chromiumcopper, 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 switched is bigger；Heat conductivility is better, then is more conducive to switch heat dissipation, carries
High Breaking capacity, electrical erosion resistance performance and used life.In chromiumcopper, electrical and thermal conductivity performance is completed mainly by copper, therefore
Copper and chromiumcopper are combined graded alloy, are expected to improve its conductive and heat-conductive ability.
The preparation of Cu/CuCr graded alloy at present uses laser welding technology more, but laser welding technology is in faying face
Easily generate stomata, fire check and harmful phase.The discharge plasma sintering technique that the present invention uses is sintered by rationally designing
Mold, the Temperature Distribution being varied and controlled in mold can prepare the high-compactness graded composite that conventional sintering method can not be prepared
Material.Further, since the bulk composition of Cu/CuCr graded alloy is copper, can effectively avoid using powder sintering due to ingredient
Interface problem caused by difference, such as coefficient of thermal expansion difference lead to interfacial stress mismatch and form micro-crack.Therefore, it uses
Discharge plasma sintering technique is expected to obtain the low Cu/CuCr gradient composites of high-compactness, electric-conductivity heat-conductivity high, air content.
Invention content
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 field, provides a kind of high cause
Density, electric-conductivity heat-conductivity high, low gas content amount Cu/CuCr functionally gradient material (FGM)s preparation method.
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, feature are：Using plasma discharging
Sintering technology carries out consolidation to Cu powder and CuCr mixed-powders, by designing gradient temperature field, applies axial mechanical pressure
While be heated to 700~900 DEG C with the heating rate of 50~300 DEG C/min after keep the temperature 2~15min, you can obtain high fine and close
Spend Cu/CuCr gradient composites.Specifically comprise the following steps：
Step 1 selects oxygen content to be less than 500ppm, the Ni metal powder that grain size is not more than 200 mesh；Oxygen content is selected to be less than
The metal Cr powder of 800ppm, grain size between the mesh of 80 mesh~240；
Cu powder and Cr powder are weighed according to the ingredient of required CuCr alloys, mixed 10 hours using mechanical mixing, is obtained equal
Even CuCr mixed-powders；
According to the ratio of Cu and CuCr in the size of required Cu/CuCr gradient composites and composite material, weigh certain
The Cu powder and CuCr mixed-powders of amount are spare；
Cu powder and CuCr mixed-powders are sequentially loaded into sintering graphite mold by step 2；According to required Cu/CuCr gradients
The ratio of Cu and CuCr in the size and composite material of composite material, adjust upper and lower pressure head height and powder green bodies in mould
Position in tool；
Precompressed carries out the powder installed using hand-operated hydraulic press, pressure is 8~12MPa；
Step 3, the carbon felt that the 4~6mm thickness contour with graphite jig is wrapped in the graphite jig periphery for installing powder, then
It places it in the furnace chamber of discharge plasma sintering stove, is evacuated to 5Pa hereinafter, being sintered forming 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 is prepared using welding method, complex procedures are of high cost, and composition surface easily generates and lacks
Falling into influences the electrical and thermal conductivity performance of material.And the sintering method of the present invention is performance (such as conductive and heat-conductive according to needed for composite material
Performance), adjust composite material in Cu and CuCr ratio, further according to the size and composite material of Cu/CuCr gradient composites
The ratio of middle Cu and CuCr, using discharge plasma sintering technique, in same mold by adjust upper and lower fall head and
The position of powder green bodies in a mold builds gradient temperature field, realizes the consolidation of Cu powder and CuCr mixed-powders, obtains
The Cu/CuCr graded composite alloys of high-compactness, electric-conductivity heat-conductivity high and low gas content amount were obtained, process is simple and at low cost.
2nd, present invention optimizes the preparation process of Cu/CuCr graded composite contact materials, under the optimal conditions of the present invention,
The advantage of the preparation process 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.
Oxygen content is selected to be not more than the Ni metal powder of 200 mesh less than 500ppm, grain size in the following embodiments, oxygen is selected to contain
Metal Cr powder of the amount less than 800ppm, grain size between the mesh of 80 mesh~240.
Discharge plasma sintering stove used for Sinter Land Inc companies of Japan production LABOX-350 discharge etc. from
Sub- sintering system, current type be DC pulse current, pulse train 40:7.
Embodiment 1
The preparation of the present embodiment Cu/CuCr gradient composites carries out as follows：
Step 1 weighs Cu powder 700g, Cr powder 300g respectively, using mechanical mixing mixing 10h, obtains uniform CuCr
Mixed-powder；
Step 2 loads 10g Cu powder and 8g CuCr mixed-powders into sintering graphite mold successively；Adjust sintering stone
The position of the upper and lower fall head of black mold and powder green bodies in a mold；The powder installed is carried out using hand-operated hydraulic press
Precompressed, pressure are~10MPa；
The graphite jig for installing powder is superscribed the carbon felt contour with graphite jig by step 3, and thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to 5Pa and powder is carried out hereinafter, being passed through DC pulse current
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, density 8.60g/cm are obtained after furnace cooling3,
Consistency is 99.7%, oxygen content 300ppm.
Embodiment 2
The preparation of the Cu/CuCr gradient composites of the present embodiment carries out as follows：
Step 1 weighs Cu powder 700g, Cr powder 300g respectively, using mechanical mixing mixing 10h, obtains uniform CuCr
Mixed-powder；
Step 2 loads 10g Cu powder and 8g CuCr mixed-powders successively into mold；Adjust upper and lower fall head and
The position of powder green bodies in a mold；Precompressed carries out the powder installed using hand-operated hydraulic press, pressure is~10MPa；
The graphite jig for installing powder is superscribed the carbon felt contour with graphite jig by step 3, and thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to 5Pa and powder is carried out hereinafter, being passed through DC pulse current
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, density 8.64g/cm are obtained after furnace cooling3,
Consistency is 99.8%, oxygen content 500ppm.
Embodiment 3
The preparation of the Cu/CuCr gradient composites of the present embodiment carries out as follows：
Step 1 weighs Cu powder 700g, Cr powder 300g respectively, using mechanical mixing mixing 10h, obtains uniform CuCr
Mixed-powder；
Step 2 loads 10g Cu powder and 8g CuCr mixed-powders successively into mold；Adjust upper and lower fall head and
The position of powder green bodies in a mold；Precompressed carries out the powder installed using hand-operated hydraulic press, pressure is~10MPa；
The graphite jig for installing powder is superscribed the carbon felt contour with graphite jig by step 3, and thickness is~5mm, so
It is loaded into afterwards in the furnace chamber of discharge plasma sintering stove, is evacuated to 5Pa and powder is carried out hereinafter, being passed through DC pulse current
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, density 8.53g/cm are obtained after furnace cooling3,
Consistency is 99.1%, oxygen content 400ppm.
Claims (2)
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 field, applies the same of axial mechanical pressure
When be heated to 700~900 DEG C with the heating rate of 50~300 DEG C/min after keep the temperature 2~15min, that is, obtain high-compactness Cu/
CuCr gradient composites, specifically comprise the following steps：
Step 1 selects oxygen content to be less than 500ppm, the Ni metal powder that grain size is not more than 200 mesh；Oxygen content is selected to be less than
The metal Cr powder of 800ppm, grain size between the mesh of 80 mesh~240；
Cu powder and Cr powder are weighed according to the ingredient of required CuCr alloys, mixed 10 hours using mechanical mixing, is obtained uniform
CuCr mixed-powders；
According to the ratio of Cu and CuCr in the size of required Cu/CuCr gradient composites and composite material, weigh a certain amount of
Cu powder and CuCr mixed-powders are spare；
Cu powder and CuCr mixed-powders are sequentially loaded into sintering graphite mold by step 2；According to required Cu/CuCr graded composites
The ratio of Cu and CuCr in the size and composite material of material, adjust upper and lower pressure head height and powder green bodies in a mold
Position；
Precompressed carries out the powder installed using hand-operated hydraulic press, pressure is 8~12MPa；
Step 3, the carbon felt that the 4~6mm thickness 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 5Pa hereinafter, being sintered forming 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.
2. preparation method according to claim 1, it is characterised in that：Prepared Cu/CuCr gradient composites sizes
For：10~50mm of diameter, draw ratio 0.1~1.0.
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| 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 |
| CN108274009B (en) * | 2018-02-08 | 2020-05-22 | 合肥工业大学 | Cr target material repairing method |
| CN111618297B (en) * | 2020-04-21 | 2022-06-07 | 陕西斯瑞新材料股份有限公司 | Preparation method of rapid sintering forming silver-based contact |
| 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 |
| 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 |
| CN113172235B (en) * | 2021-04-02 | 2022-10-28 | 西安交通大学 | Electrical contact preparation method based on multi-material metal synchronous 3D printing technology |
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| CN101834077B (en) * | 2010-04-16 | 2012-02-01 | 河南理工大学 | Method for manufacturing pure copper/copper chromium alloy composite contact material |
| CN102632237B (en) * | 2012-05-17 | 2014-03-26 | 河南理工大学 | Method for manufacturing pure copper/ copper-chromium alloy composite contact material by spray deposition |
| CN105132726B (en) * | 2015-07-31 | 2017-03-08 | 陕西斯瑞新材料股份有限公司 | A kind of copper-chromium contact material suitable for contactor and preparation method thereof |
| CN105018768B (en) * | 2015-07-31 | 2017-05-03 | 陕西斯瑞新材料股份有限公司 | High-performance copper chromium contactor material and preparing method thereof |
| CN106180654B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares infiltration copper-chromium contact material |
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| CN106180653B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares copper tungsten contact material |
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