CN106180742B - A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders - Google Patents

A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders Download PDF

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CN106180742B
CN106180742B CN201610562700.9A CN201610562700A CN106180742B CN 106180742 B CN106180742 B CN 106180742B CN 201610562700 A CN201610562700 A CN 201610562700A CN 106180742 B CN106180742 B CN 106180742B
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powder
ball
alloy
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CN106180742A (en
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索红莉
刘婧
马麟
喻丹
王毅
刘敏
孟易晨
王田田
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Beijing University of Technology
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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling

Abstract

A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders, belongs to conductor of high-temperature superconductor coat baseband domain.Ball milling NiO, WO in advance of the invention3Mixed-powder, it is big to solve Ni poor fluidities during pure Ni, pure W mixing and ball millings, plastic deformation, W good fluidities, it is non-breakable the problem of；The preparation of nanoscale NiW alloy powders lays the first stone for the billet preparation of fine grain size again.Mechanical attrition method has that cost is low, yield is high, simple for process, the advantages of alloy substrate composition transfer is flexible, is the Perfected process of extensive prepares coating conductor Ni nanoparticle W alloy powder.

Description

A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders
Technical field
The present invention relates to a kind of preparation method of coating conductor NiW alloy base band alloy nano-powders, belong to high temperature and surpass Lead baseband technology field used for coating conductor.
Background technology
Since YBCO high-temperature superconductor bands being prepared from oak forest National Laboratory of the U.S. in 1996 using RABiTS methods, coating Conductor NiW alloy base bands gradually develop from pure nickel, Ni5W, Ni7W to W atomic percentage concs higher Ni9W, Ni9.3W, The further mechanical property and magnetic property for improving NiW alloy base bands on the basis of sharp keen cubic texture is obtained is expected, to meet YBCO coating conductors are widely applied.But the relatively low intrinsic property of high-tungsten alloy base band stacking fault energy cause deformation process S types, Copper types orientation shifts, raised growth twin occurs in recrystallization process, has seriously undermined high-tungsten alloy base band cube and has knitted The formation of structure.
The formation of NiW alloy base belt for coated conductor strong cubic texture is set up the W elements in initial billet and is uniformly distributed With in the control of crystallite dimension：The method of alloy powder prepares coating conductor NiW alloy base bands, can be effectively prevented from tradition Powder metallurgic method preparation NiW alloy billet W Elemental redistributions are uneven and homogenize the problem of crystallite dimension is excessive after heat treatment.Enter One step uses alloy nano-powder prepares coating conductor NiW alloy base band billets, then can be by NiW alloy billet crystallite dimension controls System is within 10 μm.
The preparation of alloy nano-powder has mechanical alloying method, Amorphous Crystallization method, sol-gal process, vapour deposition process etc., Distinct methods have its each feature and the scope of application：The nanometer powder of pure nickel is prepared using solution phase chemical reduction；Spray drying Method can not directly prepare nanoscale alloy powder, it is adaptable to the preparation of micron order alloy powder；Amorphous Crystallization method is applied to amorphous The strong soft magnetic materials of change ability, after the low-dimensional materials such as amorphous powder, silk and band are obtained, is sintered through hot extrusion or HTHP Etc. method synthesizing block sample；Sol-gal process be readily able to hydrolysis metallic compound inorganic salts or alkoxide in certain solvent with Water reacts, and need to be usually used in SiC, SnO by hydrolysis and polycondensation process and gradually gelation2Deng the preparation of nanometer powder.
The preparation research of current NiW alloy nanoparticles used for coating conductor is still in space state.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation method of coating conductor NiW alloy base band alloy nano-powders.
A kind of preparation method of coating conductor NiW alloy base band alloy nano-powders comprises the following steps：
(1)NiO、WO3The mixing of powder and tube reducing
Choose that mass fraction purity is NiO powder that 99.99%, granularity is 3~5 μm and mass fraction purity is 99.95%th, granularity is 2 μm~3 μm of WO3Powder, matches somebody with somebody powder for 5~12 by W atomic percentage concs, is placed in high energy ball mill Ball milling 20h obtains alloy powder of the granularity in 300nm~500nm.Ball milling uses 5mm~8mm tungsten-cobalt hard alloy ball, ball powder Mass ratio is 20:1, mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.
(2)NiO、WO3The two steps reduction of nanometer mixed-powder
The nanometer mixed-powder that step (1) is obtained is placed in drying box and dried, and drying temperature is 50 DEG C, and drying time is 3h.Dried powder is loosely laid in porcelain boat bottom, powder overlay thickness is in below 1mm.Reduction reaction is in hydrogen furnace Carry out, the reaction first step is incubated 40min at 490 DEG C, second step is incubated 180min at 750 DEG C, and wherein course of reaction uses purity 99.9995% high-purity hydrogen, throughput is 100~110L/h.
(3) mechanical alloying of Ni, W mixed-powder
Ni, W mixed-powder that step (2) is obtained are placed in high energy ball mill, using liquid nitrogen gas washing, are continually fed into liquid nitrogen Start ball milling after 15min.Ball milling uses a diameter of 3~5mm tungsten-cobalt hard alloy ball, and ball powder mass ratio is 20:1, ball milling turns Speed is 300r/min.Ball grinder is moved into glove box and stands 30min and take out after mechanical ball mill 48h, obtain granularity 500~ 800nm alloy powder.
The preparation method for the Ni nanoparticle W alloy powder that the present invention is designed, advance ball milling NiO, WO3Mixed-powder, solve Ni poor fluidities, plastic deformation are big during pure Ni, pure W mixing and ball millings, W good fluidities, it is non-breakable the problem of；Nanometer The preparation of level NiW alloy powders lays the first stone for the billet preparation of fine grain size again.Mechanical attrition method have cost it is low, production High, simple for process, the advantages of alloy substrate composition transfer is flexible is measured, is that extensive prepares coating conductor Ni nanoparticle W is closed The Perfected process at bronze end.
Brief description of the drawings
The forward and backward XRD spectrum of Ni, W mixed-powder mechanical alloying in Fig. 1, example 1
Embodiment
With reference to embodiment, the present invention is described further, but the present invention is not limited in following examples.
Example 1
Choose that mass fraction purity is NiO powder that 99.99%, granularity is 3~5 μm and mass fraction purity is 99.95%th, granularity is 2 μm~3 μm of WO3Powder, weighs NiO powder 5.463g, WO3Powder 0.892g is placed in high energy ball mill The middle common 20h of ball milling obtains alloy powder of the granularity in 300nm~500nm.Ball milling uses 5mm~8mm tungsten-cobalt hard alloy ball, Ball powder mass ratio is 20:1, mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.By obtained nanometer Mixed-powder is placed in drying box and dried, and drying temperature is 50 DEG C, and drying time is 3h.Dried powder is loosely laid in Porcelain boat bottom, powder overlay thickness is in below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is in 490 DEG C of insulations 40min, second step is incubated 180min at 750 DEG C, and wherein course of reaction uses the high-purity hydrogen of purity 99.9995%, throughput For 100~110L/h.Obtained Ni, W mixed-powder is placed in high energy ball mill, using liquid nitrogen gas washing, liquid nitrogen is continually fed into Start ball milling after 15min.Ball milling uses a diameter of 3~5mm tungsten-cobalt hard alloy ball, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min.Ball grinder is moved into glove box and stands 30min and take out after mechanical ball mill 48h, obtain granularity 500~ 800nm alloy powder.
Example 2
Choose that mass fraction purity is NiO powder that 99.99%, granularity is 3~5 μm and mass fraction purity is 99.95%th, granularity is 2 μm~3 μm of WO3Powder, weighs NiO powder 5.000g, WO3Powder 1.345g is placed in high energy ball mill Middle ball milling 20h obtains alloy powder of the granularity in 300nm~500nm.Ball milling uses 5mm~8mm tungsten-cobalt hard alloy ball, ball Powder mass ratio is 20:1, mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.Obtained nanometer is mixed Conjunction powder, which is placed in drying box, to be dried, and drying temperature is 50 DEG C, and drying time is 3h.Dried powder is loosely laid in porcelain Boat bottom, powder overlay thickness is in below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is in 490 DEG C of insulations 40min, second step is incubated 180min at 750 DEG C, and wherein course of reaction uses the high-purity hydrogen of purity 99.9995%, throughput For 100~110L/h.Obtained Ni, W mixed-powder is placed in high energy ball mill, using liquid nitrogen gas washing, liquid nitrogen is continually fed into Start ball milling after 15min.Ball milling uses a diameter of 3~5mm tungsten-cobalt hard alloy ball, and ball powder mass ratio is 20:1, ball milling turns Speed is 300r/min.Ball grinder is moved into glove box and stands 30min and take out after mechanical ball mill 48h, obtain granularity 500~ 800nm alloy powder.
Example 3
Choose that mass fraction purity is NiO powder that 99.99%, granularity is 3~5 μm and mass fraction purity is 99.95%th, granularity is 2 μm~3 μm of WO3Powder, weighs NiO powder 4.816g, WO3Powder 1.533g is placed in high energy ball mill Middle ball milling 20h obtains alloy powder of the granularity in 300nm~500nm.Ball milling uses 5mm~8mm tungsten-cobalt hard alloy ball, ball Powder mass ratio is 20:1, mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.Obtained nanometer is mixed Conjunction powder, which is placed in drying box, to be dried, and drying temperature is 50 DEG C, and drying time is 3h.Dried powder is loosely laid in porcelain Boat bottom, powder overlay thickness is in below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is in 490 DEG C of insulations 40min, second step is incubated 180min at 750 DEG C, and wherein course of reaction uses the high-purity hydrogen of purity 99.9995%, throughput For 100~110L/h.Obtained Ni, W mixed-powder is placed in high energy ball mill, using liquid nitrogen gas washing, liquid nitrogen is continually fed into Start ball milling after 15min.Ball milling uses a diameter of 3~5mm tungsten-cobalt hard alloy ball, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min.Ball grinder is moved into glove box and stands 30min and take out after mechanical ball mill 48h, obtain granularity 500~ 800nm alloy powder.

Claims (1)

1. a kind of preparation method of coating conductor NiW alloy base band alloy nano-powders, it is characterised in that including following step Suddenly：
(1)NiO、WO3The mixing of powder and tube reducing
Choose the WO that granularity is 3~5 μm of NiO powder and granularity is 2 μm~3 μm3Powder, by W atomic percentage concs be 5%~ 12% matches somebody with somebody powder, is placed in ball milling 20h in high energy ball mill and obtains alloy powder of the granularity in 300nm~500nm；Ball milling uses 5mm ~8mm tungsten-cobalt hard alloy ball；Ball powder mass ratio is 20:1, mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm；
(2)NiO、WO3The two steps reduction of nanometer mixed-powder
The nanometer mixed-powder that step (1) is obtained is placed in drying box and dried, and drying temperature is 50 DEG C, and drying time is 3h； Dried powder is loosely laid in porcelain boat bottom, powder overlay thickness is in below 1mm；Reduction reaction is entered in hydrogen furnace OK, the reaction first step is incubated 40min at 490 DEG C, and second step is incubated 180min at 750 DEG C, and wherein course of reaction uses hydrogen, gas Flow is 100~110L/h；
(3) mechanical alloying of Ni, W mixed-powder
Ni, W mixed-powder that step (2) is obtained are placed in high energy ball mill, using liquid nitrogen gas washing, are continually fed into liquid nitrogen Start ball milling after 15min；Ball milling uses a diameter of 3~5mm tungsten-cobalt hard alloy ball, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min；Ball grinder is moved into glove box and stands 30min and take out after mechanical ball mill 48h, obtain granularity 500~ 800nm alloy powder.
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CN1428218A (en) * 2001-12-27 2003-07-09 韩国机械研究院 Method for preparing tungsten-copper base composite powder and sintered alloy made up by using said composite powder for making radiator
CN1844431A (en) * 2006-05-19 2006-10-11 北京工业大学 Ni-base alloy composite baseband and method for preparing discharge plasma thereof
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CN1428218A (en) * 2001-12-27 2003-07-09 韩国机械研究院 Method for preparing tungsten-copper base composite powder and sintered alloy made up by using said composite powder for making radiator
CN1844431A (en) * 2006-05-19 2006-10-11 北京工业大学 Ni-base alloy composite baseband and method for preparing discharge plasma thereof
CN101635185A (en) * 2009-08-28 2010-01-27 北京工业大学 Method for preparing Ni-W alloy base band with non/low magnetic cubic texture
CN104759632A (en) * 2015-03-23 2015-07-08 北京科技大学 Method of preparing nano-crystalline powdered alloy powder

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