CN105206435A - Gradient composite copper-chromium contact material and preparation method thereof - Google Patents
Gradient composite copper-chromium contact material and preparation method thereof Download PDFInfo
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- CN105206435A CN105206435A CN201510481498.2A CN201510481498A CN105206435A CN 105206435 A CN105206435 A CN 105206435A CN 201510481498 A CN201510481498 A CN 201510481498A CN 105206435 A CN105206435 A CN 105206435A
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- 239000000463 material Substances 0.000 title claims abstract description 63
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000011651 chromium Substances 0.000 claims abstract description 30
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 230000008595 infiltration Effects 0.000 claims abstract description 12
- 238000001764 infiltration Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims description 45
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 31
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
- 229910052802 copper Inorganic materials 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000002008 calcined petroleum coke Substances 0.000 claims description 15
- 238000007598 dipping method Methods 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 15
- 239000011236 particulate material Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 239000002808 molecular sieve Substances 0.000 claims description 12
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000010426 asphalt Substances 0.000 claims description 9
- 238000007493 shaping process Methods 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 7
- 206010020843 Hyperthermia Diseases 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000006392 deoxygenation reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000013467 fragmentation Methods 0.000 claims description 6
- 238000006062 fragmentation reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000036031 hyperthermia Effects 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 6
- 239000002006 petroleum coke Substances 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000004567 concrete Substances 0.000 claims description 3
- 238000005087 graphitization Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 239000012774 insulation material Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910021487 silica fume Inorganic materials 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000003466 welding Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910017813 Cu—Cr Inorganic materials 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/04—Co-operating contacts of different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
-
- B22F1/0003—
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a gradient composite copper-chromium contact material and a preparation method thereof. The gradient composite copper-chromium contact material is mainly composed of a CuCr50 layer and a CuCr1 layer. The CuCr50 layer comprises 45-55% of Cr with the balance being Cu by mass. The CuCr1 layer comprises 0.6-2.1% of Cr with balance being Cu by mass. The preparation method comprises the steps of raw material selection, powder mixing, compacting, infiltration and annealing. A product is improved based on the welding performance of a present copper-chromium contact material and the loop resistance. The infiltrated CuCr50 is prepared by a single-sheet infiltration technology, and the CuCr1 layer is formed by utilizing a designed temperature curve. An original contact composed of all CuCr50 is optimized into a contact composed of half CuCr50 and half of CuCr1, use of the strategic metal Cr is reduced, the loop resistance of the contact is reduced due to use of CuCr1, and the welding performance between the contact and a cup seat is improved.
Description
Technical field
The present invention relates to a kind of graded composite copper-chromium contact material and preparation method thereof, belong to field of metal matrix composite.
Background technology
Electrical contact is the contact element of appliance switch, is mainly responsible for the task of contact, disconnecting consumers electric current.Contact and arc quenching system are the fail safes of the heart of switch, switch, reliability and cut-off and close physical property and the electrical characteristics thereof that characteristic depends on contact material to a great extent.Therefore, its performance directly affects the reliability operation of device for switching.Cu-Cr contact materials is widely used on various circuit breaker, vacuum load switch and transformer change over switch because it has good resistance to arc erosion, resistance fusion welding and high strength.
But the composition due to traditional copper-chromium contact material is homogeneous, the heat conduction of copper chromium contact, bond strength and electrical property can not be significantly improved.Can not dispel the heat timely in interrupting process and cause material internal to produce larger thermal stress, causing copper chromium material surface crackle to produce, finally cause the partial exfoliation of material and make switch failure.Therefore, the contact material needing a kind of new improvement badly solves this problem.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned defect, provides a kind of graded composite copper-chromium contact material and preparation method thereof.The present invention is the improving product based on existing copper chromium contact material weldability and loop resistance carry out.The present invention designs a kind of monolithic infiltration process, prepares infiltration cu Cr50, adopts the temperature curve of design to form CuCr1 layer simultaneously.Feature of the present invention is that original full wafer CuCr50 contact is optimized for half CuCr50 half CuCr1, thus reduces the use to strategic Metal Cr, uses CuCr1 to decrease the loop resistance of contact blade, improves the welding performance of contact and cup simultaneously.
The technical scheme that the present invention solves the employing of its technical problem is as follows: a kind of graded composite copper-chromium contact material, and it is primarily of CuCr50 layer and CuCr1 layer composition, and CuCr50 composition of layer by mass fraction ratio is: Cr content 45-55%, Cu surplus; CuCr1 composition of layer by mass fraction ratio is: Cr content is 0.6-2.1%, Cu surplus; Its raw material are respectively the Cr powder of 65-200 micron and the Cu powder of less than 100 microns.
Preferably, described chromium powder is electrolytic chromium powder or aluminothermic reduction chromium powder, and described copper powder is electrolytic copper powder or atomized copper powder.
In above-mentioned either a program preferably, the purity of described chromium powder is 99.3%-99.98%.
In addition, the preparation method of this graded composite copper-chromium contact material, comprises the following steps:
(1) raw material are selected
Select the chromium powder of 65-200 micron and the copper powder of less than 100 microns;
(2) mixed powder
By Cu powder: Cr powder=7: the weight proportion of 3 forms the mixed-powder of Cu powder and Cr powder, subsequently by mixed powder: copper ball=1: the weight proportion of 1 is put into ball mill tank and carried out ball milling and mix powder 3-10 hour, ball-milling medium employing alcohol; Fully mix until alcohol volatilization under room temperature condition; Be on the one hand form certain porosity to the object adding Cu powder in Cr powder, be conducive to the fusing of follow-up Cu block and infiltrate; Ensure enough green densities on the other hand, thus can well be shaping when making follow-up compacting.
(3) pressed compact
Mixed powder after mixed is carried out pressed compact on four-column hydraulic press, point three sections of pressurizations, every section of employing height limit, to be pressed onto behind position pressurize 10 minutes, every spacer segment one minute; The press power parameter of this four-column hydraulic press is 6-7t/cm
2, green density is 4.2-5.5g/cm
3;
(4) infiltration
Loaded in graphite crucible by the pressed compact pressed, and place copper billet in the above, copper billet weight should be the 80-200% of pressed compact total weight; Be placed in vacuum sintering furnace by the graphite crucible loading pressed compact and Cu block and carry out infiltration process, vacuum degree is 1.0-1.0x10
-2pa, oozing copper temperature is 1080-1300 DEG C, temperature retention time 30-120 minute; This graphite crucible is made up of petroleum coke particles raw material, and grain graininess is 1 ~ 16mm and 0.03 ~ 0.05mm; In this step, the Cu liquid first melted first infiltrates in pressed compact and forms CuCr50 layer with Cr, and the Cu then do not oozed can form CuCr1 layer with thinner Cr powder particles in pressed compact on CuCr50; The combination of Cu and Cr mainly has thinner particle in original Cr powder, and at high temperature liquation and vacuum can form certain vapour pressure, and thin Cr particle is floated near Cu liquid, thus form CuCr1.
(5) anneal
Ooze the blank after copper and carry out annealing in process, annealing temperature is 500-850 DEG C, insulation 1-4 hour; Blank after annealing is graded composite copper-chromium contact material.The effect of this step: because cooling rate is too fast when infiltration, makes this alloy define the solid solution of certain saturation degree, cause the electrical property of material and hardness lower, the phase of solid solution can be made again to separate out by this step annealing, improve material property.
Preferably, chromium powder described in step (1) is before combination through following process:
A. described chromium powder is joined in the alumina crucible in chromium powder reduction furnace, to chromium powder upper surface distance crucible upper edge 10 ~ 20mm, stop reinforced, close fire door, furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa, is filled with the hydrogen that 1atm purity is greater than 99.9%, and described hydrogen dewaters through silica gel, molecular sieve successively, No. 105 catalyst deoxygenations, molecular sieves dewater and hyperthermia drying process, then furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa;
B. by the heating rate of 180 ~ 200 DEG C/h, furnace inner environment temperature is risen to 650 DEG C ~ 750 DEG C, continue to keep environment vacuum degree to be 6.5 × 10
-3pa-7.0 × 10
-3pa, is incubated 1 ~ 2 hour at 600 DEG C ~ 800 DEG C;
C. the hydrogen that purity is greater than 99.9% is filled with, described hydrogen is successively through silica gel, molecular sieve dewaters, No. 105 catalyst deoxygenations, molecular sieve dewaters and hyperthermia drying process, furnace inner environment hydrogen gas pressure is made to be 10 ~ 20Pa, by the heating rate of 100 ~ 150 DEG C/h, furnace inner environment temperature is risen to 1150 DEG C ~ 1250 DEG C again, after intensification terminates, be incubated 5 ~ 8 hours, then room temperature is cooled to the rate of temperature fall of 120 ~ 180 DEG C/h, obtain the chromium powder of oxygen content lower than 300ppm, wherein in described intensification, in the process of insulation and cooling, all continue to pass into hydrogen, to keep furnace inner environment air pressure for 10 ~ 20Pa.
In above-mentioned either a program preferably, the graphite crucible in step (4) is obtained by following step:
A. auxiliary material is added when calcined petroleum coke particulate material, broken; The formula of described calcined petroleum coke particulate material is: grain graininess is 16 ~ 12mm:16% ~ 17%; Grain graininess is 12 ~ 8mm:13% ~ 15%; Grain graininess is 8 ~ 4mm:13% ~ 15%; Grain graininess is 4 ~ 1mm:20% ~ 23%; All the other grain graininess are 0.03 ~ 0.05mm;
B. the calcined petroleum coke particulate material after fragmentation and auxiliary material are added in kneading pot and stir, then add liquid asphalt to kneading pot, continue to stir, make pitch infiltrate petroleum coke particles;
C. adopt pressure forming machine shaping, described pressure forming machine adopts vacuum vibration formula pressure forming machine; Described shaping vacuum degree-0.085MPa, specific pressure is 3MPa;
D. crucible green compact are put into crucible roasting furnace and carry out roasting, during shove charge, loaded in saggar by crucible green compact, and fill auxiliary material, be cured auxiliary material with curing agent, curing agent is ammoniacal liquor, guarantees that crucible green compact are indeformable in roasting process, obtains roasting product crucible; The heat temperature raising curve of described roasting adopts 480h curve;
E., after being flooded by roasting product crucible, dipping crucible is obtained; Described dipping carries out in impregnation tank, and its concrete grammar is loaded in impregnation tank by roasting product crucible, and vacuumize in tank, vacuum degree is greater than-0.085MPa, then adds liquid asphalt, then pressurizes in tank, and pressure is 2.0-2.5MPa, namely obtains dipping crucible after going out tank; Described dipping carries out 2 dippings;
F. will flood crucible graphite, obtain graphite crucible, describedly will flood crucible graphite, be carry out in inner string graphitization stove, adopt pot mouth to dock also in addition Expandable graphite sheet with the bottom of a pan during shove charge, insulation material Task-size Controlling is at 4 ~ 3mm, adopt 50h curve, furnace temperature reaches 2500 DEG C.
In above-mentioned either a program preferably, in the preparation process of graphite crucible, described auxiliary material is selected from SILICA FUME; The addition of described auxiliary material is 7% ~ 8% of calcined petroleum coke particulate material by mass percentage, and the granularity of described auxiliary material is less than 600 orders; The described amount adding liquid asphalt by mass percentage, is 25% ~ 28% of the calcined petroleum coke particulate material after whole fragmentation and auxiliary material.
In above-mentioned either a program preferably, the alcohol adding 5 ~ 7ml by every part of mixed-powder in step (2) carries out ball milling, and wherein every ball milling 50min ~ 60min shuts down and cools, and is cooled to after room temperature again carries out ball milling until ball mill tank.
Beneficial effect of the present invention:
1. the graded composite copper-chromium contact material that the inventive method is obtained in contrast to existing copper chromium contact and has saved strategic Metal Cr;
2. the graded composite copper-chromium contact material that the inventive method is obtained reduces loop resistance;
3. the graded composite copper-chromium contact material that the inventive method obtains improves the welding performance between contact and cup, conducting rod, and improves the heat dispersion of contact, improves the dielectric restorability of circuit breaker.
Brief Description Of Drawings
Fig. 1 is the structural representation of the graded composite copper-chromium contact material of prepared in accordance with the method for the present invention;
Fig. 2 is the metallographic structure figure of the graded composite copper-chromium contact material of prepared in accordance with the method for the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
A kind of graded composite copper-chromium contact material, it is primarily of CuCr50 layer and CuCr1 layer composition, and CuCr50 composition of layer by mass fraction ratio is: Cr content 45-55%, Cu surplus; CuCr1 composition of layer by mass fraction ratio is: Cr content is 0.6-2.1%, Cu surplus; Its raw material are respectively the Cr powder of 65-200 micron and the Cu powder of less than 100 microns.
Described chromium powder is electrolytic chromium powder or aluminothermic reduction chromium powder, and described copper powder is electrolytic copper powder or atomized copper powder.
The purity of described chromium powder is 99.3%-99.98%.
In addition, the preparation method of this graded composite copper-chromium contact material, comprises the following steps:
(1) raw material are selected
Select the chromium powder of 65-200 micron and the copper powder of less than 100 microns;
(2) mixed powder
By Cu powder: Cr powder=7: the weight proportion of 3 forms the mixed-powder of Cu powder and Cr powder, subsequently by mixed powder: copper ball=1: the weight proportion of 1 is put into ball mill tank and carried out ball milling and mix powder 3-10 hour, ball-milling medium employing alcohol; Fully mix until alcohol volatilization under room temperature condition; Be on the one hand form certain porosity to the object adding Cu powder in Cr powder, be conducive to the fusing of follow-up Cu block and infiltrate; Ensure enough green densities on the other hand, thus can well be shaping when making follow-up compacting.
(3) pressed compact
Mixed powder after mixed is carried out pressed compact on four-column hydraulic press, point three sections of pressurizations, every section of employing height limit, to be pressed onto behind position pressurize 10 minutes, every spacer segment one minute; The press power parameter of this four-column hydraulic press is 6-7t/cm
2, green density is 4.2-5.5g/cm
3;
(4) infiltration
Loaded in graphite crucible by the pressed compact pressed, and place copper billet in the above, copper billet weight should be the 80-200% of pressed compact total weight; Be placed in vacuum sintering furnace by the graphite crucible loading pressed compact and Cu block and carry out infiltration process, vacuum degree is 1.0-1.0x10
-2pa, oozing copper temperature is 1080-1300 DEG C, temperature retention time 30-120 minute; This graphite crucible is made up of petroleum coke particles raw material, and grain graininess is 1 ~ 16mm and 0.03 ~ 0.05mm; In this step, the Cu liquid first melted first infiltrates in pressed compact and forms CuCr50 layer with Cr, and the Cu then do not oozed can form CuCr1 layer with thinner Cr powder particles in pressed compact on CuCr50; The combination of Cu and Cr mainly has thinner particle in original Cr powder, and at high temperature liquation and vacuum can form certain vapour pressure, and thin Cr particle is floated near Cu liquid, thus form CuCr1.
(5) anneal
Ooze the blank after copper and carry out annealing in process, annealing temperature is 500-850 DEG C, insulation 1-4 hour; Blank after annealing is graded composite copper-chromium contact material.The effect of this step: because cooling rate is too fast when infiltration, makes this alloy define the solid solution of certain saturation degree, cause the electrical property of material and hardness lower, the phase of solid solution can be made again to separate out by this step annealing, improve material property.
Chromium powder described in step (1) is before combination through following process:
A. described chromium powder is joined in the alumina crucible in chromium powder reduction furnace, to chromium powder upper surface distance crucible upper edge 10 ~ 20mm, stop reinforced, close fire door, furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa, is filled with the hydrogen that 1atm purity is greater than 99.9%, and described hydrogen dewaters through silica gel, molecular sieve successively, No. 105 catalyst deoxygenations, molecular sieves dewater and hyperthermia drying process, then furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa;
B. by the heating rate of 180 ~ 200 DEG C/h, furnace inner environment temperature is risen to 650 DEG C ~ 750 DEG C, continue to keep environment vacuum degree to be 6.5 × 10
-3pa-7.0 × 10
-3pa, is incubated 1 ~ 2 hour at 600 DEG C ~ 800 DEG C;
C. the hydrogen that purity is greater than 99.9% is filled with, described hydrogen is successively through silica gel, molecular sieve dewaters, No. 105 catalyst deoxygenations, molecular sieve dewaters and hyperthermia drying process, furnace inner environment hydrogen gas pressure is made to be 10 ~ 20Pa, by the heating rate of 100 ~ 150 DEG C/h, furnace inner environment temperature is risen to 1150 DEG C ~ 1250 DEG C again, after intensification terminates, be incubated 5 ~ 8 hours, then room temperature is cooled to the rate of temperature fall of 120 ~ 180 DEG C/h, obtain the chromium powder of oxygen content lower than 300ppm, wherein in described intensification, in the process of insulation and cooling, all continue to pass into hydrogen, to keep furnace inner environment air pressure for 10 ~ 20Pa.
Graphite crucible in step (4) is obtained by following step:
A. auxiliary material is added when calcined petroleum coke particulate material, broken; The formula of described calcined petroleum coke particulate material is: grain graininess is 16 ~ 12mm:16% ~ 17%; Grain graininess is 12 ~ 8mm:13% ~ 15%; Grain graininess is 8 ~ 4mm:13% ~ 15%; Grain graininess is 4 ~ 1mm:20% ~ 23%; All the other grain graininess are 0.03 ~ 0.05mm;
B. the calcined petroleum coke particulate material after fragmentation and auxiliary material are added in kneading pot and stir, then add liquid asphalt to kneading pot, continue to stir, make pitch infiltrate petroleum coke particles;
C. adopt pressure forming machine shaping, described pressure forming machine adopts vacuum vibration formula pressure forming machine; Described shaping vacuum degree-0.085MPa, specific pressure is 3MPa;
D. crucible green compact are put into crucible roasting furnace and carry out roasting, during shove charge, loaded in saggar by crucible green compact, and fill auxiliary material, be cured auxiliary material with curing agent, curing agent is ammoniacal liquor, guarantees that crucible green compact are indeformable in roasting process, obtains roasting product crucible; The heat temperature raising curve of described roasting adopts 480h curve;
E., after being flooded by roasting product crucible, dipping crucible is obtained; Described dipping carries out in impregnation tank, and its concrete grammar is loaded in impregnation tank by roasting product crucible, and vacuumize in tank, vacuum degree is greater than-0.085MPa, then adds liquid asphalt, then pressurizes in tank, and pressure is 2.0-2.5MPa, namely obtains dipping crucible after going out tank; Described dipping carries out 2 dippings;
F. will flood crucible graphite, obtain graphite crucible, describedly will flood crucible graphite, be carry out in inner string graphitization stove, adopt pot mouth to dock also in addition Expandable graphite sheet with the bottom of a pan during shove charge, insulation material Task-size Controlling is at 4 ~ 3mm, adopt 50h curve, furnace temperature reaches 2500 DEG C.
In the preparation process of graphite crucible, described auxiliary material is selected from SILICA FUME; The addition of described auxiliary material is 7% ~ 8% of calcined petroleum coke particulate material by mass percentage, and the granularity of described auxiliary material is less than 600 orders; The described amount adding liquid asphalt by mass percentage, is 25% ~ 28% of the calcined petroleum coke particulate material after whole fragmentation and auxiliary material.
The alcohol adding 5 ~ 7ml by every part of mixed-powder in step (2) carries out ball milling, and wherein every ball milling 50min ~ 60min shuts down and cools, and is cooled to after room temperature again carries out ball milling until ball mill tank.
Through experimental test, the physicochemical property of graded composite copper-chromium contact material obtained in above-described embodiment is as shown in table 1.
Table 1
The structure of graded composite copper-chromium contact material obtained in above-described embodiment and metallographic structure are respectively as illustrated in fig. 1 and 2.Wherein 1 is CuCr1 layer, and 2 is CuCr50 layer.
Copper powder in above-described embodiment before combination also can through steps of processing: be loaded on conveyer belt by copper powder powder particle pine, make powder produce certain sintering at 450 ~ 750 DEG C through oxidation and carry out accelerated oxidation process, the copper powder mixed oxide of above-mentioned making, after pulverizing the reduction of Sum decomposition ammonia, can obtain the spongy copper powder of porous.
The graded composite copper-chromium contact material that the inventive method obtains in contrast to existing copper chromium contact and has saved strategic Metal Cr; The graded composite copper-chromium contact material that the inventive method obtains reduces loop resistance; Improve the welding performance between contact and cup, conducting rod, and improve the heat dispersion of contact, improve the dielectric restorability of circuit breaker.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention, every according in technical spirit of the present invention to any simple modification, equivalent variations that above embodiment is done, all fall within protection scope of the present invention.
Claims (8)
1. a graded composite copper-chromium contact material, it is characterized in that it is primarily of CuCr50 layer and CuCr1 layer composition, CuCr50 composition of layer by mass fraction ratio is: Cr content 45-55%, Cu surplus; CuCr1 composition of layer by mass fraction ratio is: Cr content is 0.6-2.1%, Cu surplus; Its raw material are respectively the Cr powder of 65-200 micron and the Cu powder of less than 100 microns.
2. graded composite copper-chromium contact material according to claim 1, it is characterized in that described chromium powder is electrolytic chromium powder or aluminothermic reduction chromium powder, described copper powder is electrolytic copper powder or atomized copper powder.
3. graded composite copper-chromium contact material according to claim 1 and 2, is characterized in that the purity of described chromium powder is 99.3%-99.98%.
4. the preparation method of the graded composite copper-chromium contact material according to the claims, is characterized in that this preparation method comprises the following steps:
(1) raw material are selected
Select the chromium powder of 65-200 micron and the copper powder of less than 100 microns;
(2) mixed powder
By Cu powder: Cr powder=7: the weight proportion of 3 forms the mixed-powder of Cu powder and Cr powder, subsequently by mixed powder: copper ball=1: the weight proportion of 1 is put into ball mill tank and carried out ball milling and mix powder 3-10 hour, ball-milling medium employing alcohol; Fully mix until alcohol volatilization under room temperature condition;
(3) pressed compact
Mixed powder after mixed is carried out pressed compact on four-column hydraulic press, point three sections of pressurizations, every section of employing height limit, to be pressed onto behind position pressurize 10 minutes, every spacer segment one minute; The press power parameter of this four-column hydraulic press is 6-7t/cm
2, green density is 4.2-5.5g/cm
3;
(4) infiltration
Loaded in graphite crucible by the pressed compact pressed, and place copper billet in the above, copper billet weight should be the 80-200% of pressed compact total weight; Be placed in vacuum sintering furnace by the graphite crucible loading pressed compact and Cu block and carry out infiltration process, vacuum degree is 1.0-1.0x10
-2pa, oozing copper temperature is 1080-1300 DEG C, temperature retention time 30-120 minute; This graphite crucible is made up of petroleum coke particles raw material, and grain graininess is 1 ~ 16mm and 0.03 ~ 0.05mm;
(5) anneal
Ooze the blank after copper and carry out annealing in process, annealing temperature is 500-850 DEG C, insulation 1-4 hour; Blank after annealing is graded composite copper-chromium contact material.
5. preparation method according to claim 4, is characterized in that chromium powder described in step (1) before combination through following process:
A. described chromium powder is joined in the alumina crucible in chromium powder reduction furnace, to chromium powder upper surface distance crucible upper edge 10 ~ 20mm, stop reinforced, close fire door, furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa, is filled with the hydrogen that latm purity is greater than 99.9%, and described hydrogen dewaters through silica gel, molecular sieve successively, No. 105 catalyst deoxygenations, molecular sieves dewater and hyperthermia drying process, then furnace inner environment vacuum degree is evacuated to 6.0 × 10
-3pa-7.0 × 10
-3pa;
B. by the heating rate of 180 ~ 200 DEG C/h, furnace inner environment temperature is risen to 650 DEG C ~ 750 DEG C, continue to keep environment vacuum degree to be 6.5 × 10
-3pa-7.0 × 10
-3pa, is incubated 1 ~ 2 hour at 600 DEG C ~ 800 DEG C;
C. the hydrogen that purity is greater than 99.9% is filled with, described hydrogen is successively through silica gel, molecular sieve dewaters, No. 105 catalyst deoxygenations, molecular sieve dewaters and hyperthermia drying process, furnace inner environment hydrogen gas pressure is made to be 10 ~ 20Pa, by the heating rate of 100 ~ 150 DEG C/h, furnace inner environment temperature is risen to 1150 DEG C ~ 1250 DEG C again, after intensification terminates, be incubated 5 ~ 8 hours, then room temperature is cooled to the rate of temperature fall of 120 ~ 180 DEG C/h, obtain the chromium powder of oxygen content lower than 300ppm, wherein in described intensification, in the process of insulation and cooling, all continue to pass into hydrogen, to keep furnace inner environment air pressure for 10 ~ 20Pa.
6. the preparation method according to claim 4 or 5, is characterized in that the graphite crucible in step (4) is obtained by following step:
A. auxiliary material is added when calcined petroleum coke particulate material, broken; The formula of described calcined petroleum coke particulate material is: grain graininess is 16 ~ 12mm:16% ~ 17%; Grain graininess is 12 ~ 8mm:13% ~ 15%; Grain graininess is 8 ~ 4mm:13% ~ 15%; Grain graininess is 4 ~ 1mm:20% ~ 23%; All the other grain graininess are 0.03 ~ 0.05mm;
B. the calcined petroleum coke particulate material after fragmentation and auxiliary material are added in kneading pot and stir, then add liquid asphalt to kneading pot, continue to stir, make pitch infiltrate petroleum coke particles;
C. adopt pressure forming machine shaping, described pressure forming machine adopts vacuum vibration formula pressure forming machine; Described shaping vacuum degree-0.085MPa, specific pressure is 3MPa;
D. crucible green compact are put into crucible roasting furnace and carry out roasting, during shove charge, loaded in saggar by crucible green compact, and fill auxiliary material, be cured auxiliary material with curing agent, curing agent is ammoniacal liquor, guarantees that crucible green compact are indeformable in roasting process, obtains roasting product crucible; The heat temperature raising curve of described roasting adopts 480h curve;
E., after being flooded by roasting product crucible, dipping crucible is obtained; Described dipping carries out in impregnation tank, and its concrete grammar is loaded in impregnation tank by roasting product crucible, and vacuumize in tank, vacuum degree is greater than-0.085MPa, then adds liquid asphalt, then pressurizes in tank, and pressure is 2.0-2.5MPa, namely obtains dipping crucible after going out tank; Described dipping carries out 2 dippings;
F. will flood crucible graphite, obtain graphite crucible, describedly will flood crucible graphite, be carry out in inner string graphitization stove, adopt pot mouth to dock also in addition Expandable graphite sheet with the bottom of a pan during shove charge, insulation material Task-size Controlling is at 4 ~ 3mm, adopt 50h curve, furnace temperature reaches 2500 DEG C.
7. preparation method according to claim 6, is characterized in that in the preparation process of graphite crucible, and described auxiliary material is selected from SILICA FUME; The addition of described auxiliary material is 7% ~ 8% of calcined petroleum coke particulate material by mass percentage, and the granularity of described auxiliary material is less than 600 orders; The described amount adding liquid asphalt by mass percentage, is 25% ~ 28% of the calcined petroleum coke particulate material after whole fragmentation and auxiliary material.
8. preparation method according to claim 7; it is characterized in that the alcohol adding 5 ~ 7ml by every part of mixed-powder in step (2) carries out ball milling; wherein every ball milling 50min ~ 60min shuts down and cools, and is cooled to after room temperature again carries out ball milling until ball mill tank.
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