CN106180653B - The method that discharge plasma sintering prepares copper tungsten contact material - Google Patents

The method that discharge plasma sintering prepares copper tungsten contact material Download PDF

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CN106180653B
CN106180653B CN201610638086.XA CN201610638086A CN106180653B CN 106180653 B CN106180653 B CN 106180653B CN 201610638086 A CN201610638086 A CN 201610638086A CN 106180653 B CN106180653 B CN 106180653B
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copper
contact material
discharge plasma
copper tungsten
plasma sintering
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CN106180653A (en
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赵伟鹏
郭创立
周宁
周兴
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Shaanxi Sirui Advanced Materials Co Ltd
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Shaanxi Sirui Advanced Materials Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00Casting processes not provided for in groups B22D1/00 - B22D21/00
    • B22D23/04Casting by dipping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C3/00Selection of compositions for coating the surfaces of moulds, cores, or patterns
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention discloses a kind of method that discharge plasma sintering prepares copper tungsten contact material, comprise the following steps:Step 1, tungsten powder is poured into graphite jig, is positioned in plasma sintering stove and vacuumizes and pressurize, be passed through pulsed direct current and be warming up to 1,320 1480 DEG C, after being incubated 2.5 5min, furnace cooling obtains W skeleton;Step 2, copper billet is polished and is cleaned by ultrasonic clean, laser irradiation is carried out with the speed of 10 500 mm/seconds with laser and scanned, then carry out corona treatment, obtain that molten to ooze copper billet standby;Step 3, W skeleton is put into graphite boat, the molten copper billet that oozes is placed on W skeleton, is around filled using schmigel, is placed in the high temperature sintering furnace with protective gas atmosphere, after being warming up to 1,300 1400 DEG C, is incubated 23 hours, the copper tungsten sintered body after being sintered;Step 4, it is 50 100MPa in pressure by copper tungsten sintered body, temperature carries out vacuumizing hot pressing, is cooled to room temperature, that is, obtains copper tungsten contact material under conditions of being 800 850 DEG C.Production method of the present invention has the advantages of shortening the production cycle.

Description

The method that discharge plasma sintering prepares copper tungsten contact material
Technical field
The present invention relates to electrical contact preparing technical field, and in particular to a kind of discharge plasma sintering prepares copper tungsten contact material The method of material.
Background technology
The heart element of high-voltage switch gear, by its disjunction and connection, reach transmission, bear, disconnect, controlling the mesh of energy 's.High-voltage electric contact its Reliability of Microprocessor, durability, stability under high voltage, high current, the collective effect of high-temperature electric arc are Influence switch life, the key factor of safe and reliable and power network stability.
Copper tungsten contact especially during breaker division, can produce electric arc, largely because resistance to electric arc ability is stronger Energy is acted on contact, therefore the material of resistance to burning is the essential condition for ensureing breaker electrical endurance.
A kind of preparation method of copper tungsten contact of Publication No. CN102800420A disclosure of the invention, this method include following Step:(1) tungsten base processed:Tungsten powder, forming agent, wetting agent are mixed according to weight than 2100: 11: 15, are then placed in shaping It is compressing in mould, obtain tungsten base;(2) graphite crucible is made:According to the size for the copper tungsten contact to be made, choose corresponding Graphite bar and processed be made inner chamber be contact shape graphite crucible;(3) graphite crucible is dried:Graphite crucible is put Enter drying in oven;(4) graphite crucible is protected:Brushing graphite aqua or stickup graphite paper on the inwall of graphite crucible, then Graphite crucible is put into baking oven inside holding;(5) copper-bearing materials are prepared:According to the weight and graphite of the copper tungsten contact to be made The inner chamber size of crucible, copper-bearing materials corresponding to making;(6) crucible is filled:Tungsten base is put into graphite crucible bottom, then by cupric Material is put into graphite crucible, and is placed on the upper surface of tungsten base;(7) shove charge vacuumizes heating infiltration:By the graphite after charging Crucible is put into the heater in vacuum drying oven, is closed fire door and is started vavuum pump and vacuumized, vacuumizes rear heater Graphite crucible is heated, copper-bearing materials infiltration, which enters in tungsten base, obtains copper tungsten contact;(8) cool down:After the completion of heating, in constant temperature Graphite crucible is slowly exited into heater under state, is then shut off heater;(9) come out of the stove:Vavuum pump is closed after closing heater, Open fire door and take out graphite crucible, copper tungsten contact is taken out from graphite crucible.
It can be seen that from the technical process of above-mentioned preparation copper tungsten contact material, it is necessary to by tungsten powder advance comprising, be molded link Typically completed by uniformly adding forming agent and hydraulic press, and pre-sintering is carried out before high temperature oozes copper, to lift copper tungsten contact Material combination property, it is pre-sintered by being completed by vacuum sintering furnace, cause the shortcomings of production cost is high, power consumption is big.In high pressure Under the background that switching requirements are constantly lifted, the preparation of copper tungsten contact material, which improves optimization, becomes particularly significant.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of electric discharge shortened the production cycle and reduce energy consumption etc. The method that ion sintering prepares copper tungsten contact material.
The technical scheme for solving above-mentioned technical problem is as follows:
The method that discharge plasma sintering prepares copper tungsten contact material, comprises the following steps:
Step 1, sinter:Tungsten powder is poured into graphite jig, mould is placed in hydrogen furnace, powder is reduced, gently Burn, come out of the stove, be positioned in plasma sintering stove and vacuumize and pressurize, after pressure reaches 30-45MPa, be passed through pulse direct current Electric current is simultaneously warming up to 1320-1480 DEG C, and after being incubated 2.5-5min, furnace cooling obtains W skeleton;
Step 2, copper billet is handled:Copper billet is taken, is first mechanically polished, the copper billet after polishing is in ultrasonic cleaning solution Carry out ultrasonic wave cleaning, supersonic frequency 35-50KHz, temperature is 30-38 DEG C, after drying, with power be 5-20 watts continuous or Pulse laser carries out laser irradiation scanning with the speed of 10-500 mm/seconds, is cooled to room temperature, then carries out corona treatment, Obtain that molten to ooze copper billet standby;
Step 3, high temperature oozes copper:W skeleton is put into graphite boat, the molten copper billet that oozes is placed on W skeleton, around using firm Beautiful powder landfill, is placed in the high temperature sintering furnace with protective gas atmosphere, after being warming up to 1300-1400 DEG C, is incubated 2-3 hours, Copper tungsten sintered body after being sintered;
Step 4, hot pressing:In pressure it is 50-100MPa by copper tungsten sintered body, temperature is carried out under conditions of being 800-850 DEG C Hot pressing is vacuumized, hot pressing time 40-100min, room temperature is cooled to, that is, obtains copper tungsten contact material.
Preferably, the particle diameter of the tungsten powder is 4-8 μm.
Preferably, the pulsed direct current is 1200-1800A.
Preferably, protective gas described in step 3 is nitrogen.
Preferably, protective gas atmosphere flow >=0.2m3/ h/h,
Preferably, it is warming up to 1320-1480 DEG C in step 1 with 100-300 DEG C/min heating rate.
Preferably, corona treatment described in step 2 is that argon plasma is handled, processing time 15-20min.
Preferably, coating is scribbled on the surface of graphite jig and/or graphite boat, the chemical composition of the coating is high-alumina fly 25-40 parts by weight, passivator are 1-3 parts by weight, mica powder 4-8 parts by weight, graphite 5-10 parts by weight, water 1-3 parts by weight, are bonded Agent 20-30 parts by weight.
Preferably, wherein passivator is any in CrO3, KMnO4, K2Cr2O7;Binding agent be soda-lime glass, potash glass or It is any in three kinds of waterglass of sodium-potash glass.
The present invention remarkable result be:The present invention by plasma sintering technique by substituting shaping and pre-sintered two rings Section, while improving the arc resistant ablation property of copper tungsten contact material, production cost is substantially reduced, reduces power consumption.Prepare Copper tungsten contact material while performance is ensured, be not only effectively shortened the production cycle, reduce power consumption, and heat equal Even, programming rate is fast, and sintering temperature is low, and sintering time is short, and production efficiency is high, product tissue fine uniform, can keep raw material Nature, the copper tungsten contact material of high-compactness can be obtained.
Exemplified by obtaining mixed powder CuW70, CuW90 contact material with the inventive method, the following (table 1 of its performance detection:Mixed powder CuW70, CuW90 contact material performance detection table):
Table 1
In addition, after the present invention is provided with coating on the surface of graphite jig and graphite boat, because the coating can be resistant to More than 1500 DEG C of temperature, therefore, buffer action not only is served to the product and graphite jig of sintering, also contributed to pair The product of graphite jig and sintering plays a protective role.
Embodiment
Embodiment 1:
The method that discharge plasma sintering prepares copper tungsten contact material, comprises the following steps:
Step 1, sinter:The tungsten powder that particle diameter is 4 μm is poured into graphite jig, mould is placed in hydrogen furnace, to powder Reduced, it is light-burned, come out of the stove, be positioned in plasma sintering stove and vacuumize and pressurize, the corona treatment is argon gas Corona treatment, processing time 15min, after pressure reaches 30MPa, it is passed through 1200A pulsed direct current and with 100 DEG C/min heating rate is warming up to 1320 DEG C, after being incubated 2.5min, furnace cooling obtains W skeleton;
Step 2, copper billet is handled:Copper billet is taken, is first mechanically polished, the copper billet after polishing is in ultrasonic cleaning solution Ultrasonic wave cleaning, supersonic frequency 35KHz are carried out, temperature is 30 DEG C, after drying, with the continuous or pulse laser that power is 5 watts Laser irradiation scanning is carried out with the speed of 10 mm/seconds, is cooled to room temperature, then carries out corona treatment, obtains molten oozing copper billet It is standby;
Step 3, high temperature oozes copper:W skeleton is put into graphite boat, the molten copper billet that oozes is placed on W skeleton, around using firm Beautiful powder landfill, is placed in the high temperature sintering furnace with protective gas atmosphere, and the protective gas is nitrogen, protective gas atmosphere stream Measure as 0.2m3/ h/h, after being warming up to 1300 DEG C, 2 hours are incubated, the copper tungsten sintered body after being sintered;
Step 4, hot pressing:In pressure it is 50MPa by copper tungsten sintered body, temperature carries out vacuumizing heat under conditions of being 800 DEG C Pressure, hot pressing time 40min, is cooled to room temperature, that is, obtains copper tungsten contact material.
Coating is scribbled on the surface of the graphite jig and/or graphite boat, the chemical composition of the coating is the weight of high-alumina fly 25 Part is measured, passivator is 1 parts by weight, the parts by weight of mica powder 4, the parts by weight of graphite 5, the parts by weight of water 1, the parts by weight of binding agent 20.Wherein Passivator is CrO3, and binding agent is soda-lime glass.
Embodiment 2:
Step 1, sinter:The tungsten powder that particle diameter is 6 μm is poured into graphite jig, mould is placed in hydrogen furnace, to powder Reduced, it is light-burned, come out of the stove, be positioned in plasma sintering stove and vacuumize and pressurize, the corona treatment is argon gas Corona treatment, processing time 17.5min, after pressure reaches 37.5MPa, be passed through 1500A pulsed direct current and with 200 DEG C/min heating rate is warming up to 1400 DEG C, and after being incubated 3.75min, furnace cooling obtains W skeleton;
Step 2, copper billet is handled:Copper billet is taken, is first mechanically polished, the copper billet after polishing is in ultrasonic cleaning solution Ultrasonic wave cleaning, supersonic frequency 42.5KHz are carried out, temperature is 34 DEG C, after drying, with the continuous or pulse that power is 12.5 watts Laser carries out laser irradiation scanning with the speed of 255 mm/seconds, is cooled to room temperature, then carries out corona treatment, obtains molten ooze Copper billet is standby;
Step 3, high temperature oozes copper:W skeleton is put into graphite boat, the molten copper billet that oozes is placed on W skeleton, around using firm Beautiful powder landfill, is placed in the high temperature sintering furnace with protective gas atmosphere, and the protective gas is nitrogen, protective gas atmosphere stream Measure as 0.3m3/ h/h, after being warming up to 1350 DEG C, 2.5 hours are incubated, the copper tungsten sintered body after being sintered;
Step 4, hot pressing:In pressure it is 75MPa by copper tungsten sintered body, temperature carries out vacuumizing heat under conditions of being 825 DEG C Pressure, hot pressing time 70min, is cooled to room temperature, that is, obtains copper tungsten contact material.
Coating is scribbled on the surface of the graphite jig and/or graphite boat, the chemical composition of the coating is high-alumina fly 32.5 Parts by weight, passivator are 2 parts by weight, the parts by weight of mica powder 6, the parts by weight of graphite 7.5, the parts by weight of water 2, the parts by weight of binding agent 25. Wherein passivator is KMnO4, and binding agent is potash glass.
Embodiment 3:
Step 1, sinter:The tungsten powder that particle diameter is 8 μm is poured into graphite jig, mould is placed in hydrogen furnace, to powder Reduced, it is light-burned, come out of the stove, be positioned in plasma sintering stove and vacuumize and pressurize, the corona treatment is argon gas Corona treatment, processing time 20min, after pressure reaches 45MPa, it is passed through 1800A pulsed direct current and with 300 DEG C/min heating rate is warming up to 1480 DEG C, after being incubated 5min, furnace cooling obtains W skeleton;
Step 2, copper billet is handled:Copper billet is taken, is first mechanically polished, the copper billet after polishing is in ultrasonic cleaning solution Ultrasonic wave cleaning, supersonic frequency 50KHz are carried out, temperature is 38 DEG C, after drying, with the continuous or pulse laser that power is 20 watts Laser irradiation scanning is carried out with the speed of 500 mm/seconds, is cooled to room temperature, then carries out corona treatment, obtains molten oozing copper billet It is standby;
Step 3, high temperature oozes copper:W skeleton is put into graphite boat, the molten copper billet that oozes is placed on W skeleton, around using firm Beautiful powder landfill, is placed in the high temperature sintering furnace with protective gas atmosphere, and the protective gas is nitrogen, protective gas atmosphere stream Measure as 0.35m3/ h/h, after being warming up to 1400 DEG C, 3 hours are incubated, the copper tungsten sintered body after being sintered;
Step 4, hot pressing:In pressure it is 100MPa by copper tungsten sintered body, temperature carries out vacuumizing heat under conditions of being 850 DEG C Pressure, hot pressing time 100min, is cooled to room temperature, that is, obtains copper tungsten contact material.
Coating is scribbled on the surface of the graphite jig and/or graphite boat, the chemical composition of the coating is the weight of high-alumina fly 40 Part is measured, passivator is 3 parts by weight, the parts by weight of mica powder 8, the parts by weight of graphite 10, the parts by weight of water 3, the parts by weight of binding agent 30.Wherein Passivator is K2Cr2O7, and binding agent is sodium-potash glass.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks Domain, similarly it is included in the scope of patent protection of the present invention.

Claims (7)

1. the method that discharge plasma sintering prepares copper tungsten contact material, it is characterised in that comprise the following steps:
Step 1, sinter:Tungsten powder is poured into graphite jig, mould is placed in hydrogen furnace, powder is reduced, it is light-burned, go out Stove, it is positioned in plasma sintering stove and vacuumizes and pressurize, after pressure reaches 30-45MPa, is passed through pulsed direct current simultaneously 1320-1480 DEG C is warming up to, after being incubated 2.5-5min, furnace cooling obtains W skeleton;
Step 2, copper billet is handled:Copper billet is taken, is first mechanically polished, the copper billet after polishing is carried out in ultrasonic cleaning solution Ultrasonic wave is cleaned, and after drying, the continuous or pulse laser for being 5-20 watts with power is swashed with the speed of 10-500 mm/seconds Light irradiation scans, and is cooled to room temperature, then carries out discharge plasma processing, and it is standby to obtain infiltration copper billet;
Step 3, high temperature oozes copper:W skeleton is put into graphite boat, infiltration copper billet is placed on W skeleton, around using schmigel Landfill, is placed in the high temperature sintering furnace with protective gas atmosphere, after being warming up to 1300-1400 DEG C, is incubated 2-3 hours, obtains Copper tungsten sintered body after sintering;
Step 4, hot pressing:In pressure it is 50-100MPa by copper tungsten sintered body, temperature carries out taking out true under conditions of being 800-850 DEG C Empty hot pressing, hot pressing time 40-100min, room temperature is cooled to, that is, obtains copper tungsten contact material.
2. the method that discharge plasma sintering according to claim 1 prepares copper tungsten contact material, it is characterised in that described The particle diameter of tungsten powder is 4-8 μm.
3. the method that discharge plasma sintering according to claim 1 prepares copper tungsten contact material, it is characterised in that described Pulsed direct current is 1200-1800A.
4. the method that discharge plasma sintering according to claim 1 prepares copper tungsten contact material, it is characterised in that step In 3, the protective gas is nitrogen.
5. the method that the discharge plasma sintering according to claim 1 or 4 prepares copper tungsten contact material, it is characterised in that Protective gas atmosphere flow >=0.2m in described high temperature sintering furnace3/h。
6. the method that discharge plasma sintering according to claim 1 prepares copper tungsten contact material, it is characterised in that step In 1 1320-1480 DEG C is warming up to 100-300 DEG C/min heating rate.
7. the method that discharge plasma sintering according to claim 1 prepares copper tungsten contact material, it is characterised in that step The processing of discharge plasma described in 2 is handled for argon plasma.
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