CN106180742A - A kind of preparation method of coating conductor NiW alloy base band alloy nano-powder - Google Patents

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

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CN106180742A
CN106180742A CN201610562700.9A CN201610562700A CN106180742A CN 106180742 A CN106180742 A CN 106180742A CN 201610562700 A CN201610562700 A CN 201610562700A CN 106180742 A CN106180742 A CN 106180742A
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powder
ball
alloy
ball milling
preparation
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CN106180742B (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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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

The preparation method of a kind of coating conductor NiW alloy base band alloy nano-powder, belongs to conductor of high-temperature superconductor coat baseband domain.Present invention ball milling NiO, WO in advance3Mixed-powder, solve Ni poor fluidity during pure Ni, pure W mixing and ball milling, plastic deformation big, W good fluidity, the most breakable problem；The preparation of nanoscale NiW alloy powder is again that the billet preparation of fine grain size lays the first stone.It is high, simple for process that mechanical attrition method has low cost, yield, and the alloy substrate composition transfer advantage such as flexibly, is the Perfected process preparing Ni nanoparticle W alloy powder used for coating conductor on a large scale.

Description

A kind of preparation method of coating conductor NiW alloy base band alloy nano-powder
Technical field
The present invention relates to the preparation method of a kind of coating conductor NiW alloy base band alloy nano-powder, belong to high temperature and surpass Lead baseband technology field used for coating conductor.
Background technology
Since oak forest National Laboratory of the U.S. in 1996 uses RABiTS method to prepare YBCO high-temperature superconductor band, coating Conductor NiW alloy base band gradually develops to W atomic percentage conc higher Ni9W, Ni9.3W from pure nickel, Ni5W, Ni7W, Mechanical property and the magnetic property of NiW alloy base band is improved further, to meet on the basis of being expected to obtain sharp keen cubic texture YBCO coating conductor wider application.But the relatively low intrinsic property of high-tungsten alloy base band stacking fault energy cause deformation process S type, Copper type orientation offsets, raised growth twin occurs in recrystallization process, has seriously undermined high-tungsten alloy base band cube and has knitted The formation of structure.
Being uniformly distributed of W element in initial billet is set up in being formed of NiW alloy base belt for coated conductor strong cubic texture With in the control of crystallite dimension: the method for NiW alloy base belt for coated conductor prepared by alloy powder, can be effectively prevented from tradition Powder metallurgic method prepares the problem that NiW alloy billet W Elemental redistribution is uneven and after homogenization heat treatment, crystallite dimension is excessive.Enter One step uses alloy nano-powder to prepare NiW alloy base belt for coated conductor billet, then can be by NiW alloy billet crystallite dimension control 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 has its each feature and the scope of application: the nanometer powder of pure nickel uses solution phase chemical reduction to prepare；It is spray-dried Method can not directly prepare nanoscale alloy powder, it is adaptable to the preparation of micron order alloy powder；Amorphous Crystallization method is applicable to amorphous The soft magnetic materials that change ability is strong, after obtaining the low-dimensional materials such as amorphous powder, silk and band, sinters through hot extrusion or High Temperature High Pressure Etc. method synthesizing block sample；Sol-gal process be readily able to hydrolysis metallic compound inorganic salt or alkoxide in certain solvent with Water reacts, and need to be usually used in SiC, SnO through hydrolysis and polycondensation process and gradually gelation2Preparation Deng nanometer powder.
The preparation research of current NiW alloy nanoparticle used for coating conductor is still in space state.
Summary of the invention
The purpose of the present invention is to propose to the preparation method of a kind of coating conductor NiW alloy base band alloy nano-powder.
The preparation method of a kind of coating conductor NiW alloy base band alloy nano-powder comprises the following steps:
(1)NiO、WO3The mixing of powder and tube reducing
Choose mass fraction purity be 99.99%, granularity be that the NiO powder of 3～5 μm is with mass fraction purity 99.95%, granularity is 2 μm～the WO of 3 μm3Powder, is 5～12 to join powder by W atomic percentage conc, is placed in ball in high energy ball mill Mill 20h obtains the granularity alloy powder at 300nm～500nm.Ball milling uses the tungsten-cobalt hard alloy ball of 5mm～8mm, ball opaque Amount ratio is 20:1, and mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.
(2)NiO、WO3Two step reduction of nanometer mixed-powder
Being placed in drying baker by the nanometer mixed-powder that step (1) obtains and be dried, baking temperature is 50 DEG C, and drying time is 3h.Being laid in bottom porcelain boat by loose for dried powder, powder overlay thickness is at below 1mm.Reduction reaction is in hydrogen furnace Carrying out, 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 purity The high-purity hydrogen of 99.9995%, throughput is 100～110L/h.
(3) mechanical alloying of Ni, W mixed-powder
Ni, W mixed-powder that step (2) obtains is placed in high energy ball mill, uses liquid nitrogen gas washing, be continually fed into liquid nitrogen Ball milling is started after 15min.Ball milling uses the tungsten-cobalt hard alloy ball of a diameter of 3～5mm, and ball powder mass ratio is 20:1, and ball milling turns Speed is 300r/min.After mechanical ball milling 48h, ball milling is filled to move into and stands 30min in glove box and take out, obtain granularity 500～ The alloy powder of 800nm.
The preparation method of the Ni nanoparticle W alloy powder of present invention design, ball milling NiO, WO in advance3Mixed-powder, solve Ni poor fluidity during pure Ni, pure W mixing and ball milling, plastic deformation are big, W good fluidity, the most breakable problem；Nanoscale The preparation of NiW alloy powder is again that the billet preparation of fine grain size lays the first stone.Mechanical attrition method has low cost, yield High, simple for process, the advantages such as alloy substrate composition transfer is flexible, are to prepare Ni nanoparticle W alloy used for coating conductor on a large scale The Perfected process of powder.
Accompanying drawing explanation
The XRD figure spectrum that in Fig. 1, example 1, Ni, W mixed-powder mechanical alloying is forward and backward
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, but the present invention is not limited in following example.
Example 1
Choose mass fraction purity be 99.99%, granularity be that the NiO powder of 3～5 μm is with mass fraction purity 99.95%, granularity is 2 μm～the WO of 3 μm3Powder, weighs NiO powder 5.463g, WO3Powder 0.892g is placed in high energy ball mill Middle ball milling 20h altogether obtains the granularity alloy powder at 300nm～500nm.Ball milling uses the tungsten-cobalt hard alloy ball of 5mm～8mm, Ball powder mass ratio is 20:1, and mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.The nanometer that will obtain Mixed-powder is placed in drying baker and is dried, and baking temperature is 50 DEG C, and drying time is 3h.It is laid in loose for dried powder Bottom porcelain boat, powder overlay thickness is at below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is 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 It is 100～110L/h.Ni, W mixed-powder obtained is placed in high energy ball mill, uses liquid nitrogen gas washing, be continually fed into liquid nitrogen Ball milling is started after 15min.Ball milling uses the tungsten-cobalt hard alloy ball of a diameter of 3～5mm, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min.After mechanical ball milling 48h, ball milling is filled to move into and stands 30min in glove box and take out, obtain granularity 500～ The alloy powder of 800nm.
Example 2
Choose mass fraction purity be 99.99%, granularity be that the NiO powder of 3～5 μm is with mass fraction purity 99.95%, granularity is 2 μm～the WO of 3 μm3Powder, weighs NiO powder 5.000g, WO3Powder 1.345g is placed in high energy ball mill Middle ball milling 20h obtains the granularity alloy powder at 300nm～500nm.Ball milling uses the tungsten-cobalt hard alloy ball of 5mm～8mm, ball Powder mass ratio is 20:1, and mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.The nanometer obtained is mixed Closing powder and be placed in drying baker dry, baking temperature is 50 DEG C, and drying time is 3h.It is laid in porcelain by loose for dried powder Bottom boat, powder overlay thickness is at below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is 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 It is 100～110L/h.Ni, W mixed-powder obtained is placed in high energy ball mill, uses liquid nitrogen gas washing, be continually fed into liquid nitrogen Ball milling is started after 15min.Ball milling uses the tungsten-cobalt hard alloy ball of a diameter of 3～5mm, and ball powder mass ratio is 20:1, and ball milling turns Speed is 300r/min.After mechanical ball milling 48h, ball milling is filled to move into and stands 30min in glove box and take out, obtain granularity 500～ The alloy powder of 800nm.
Example 3
Choose mass fraction purity be 99.99%, granularity be that the NiO powder of 3～5 μm is with mass fraction purity 99.95%, granularity is 2 μm～the WO of 3 μm3Powder, weighs NiO powder 4.816g, WO3Powder 1.533g is placed in high energy ball mill Middle ball milling 20h obtains the granularity alloy powder at 300nm～500nm.Ball milling uses the tungsten-cobalt hard alloy ball of 5mm～8mm, ball Powder mass ratio is 20:1, and mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min.The nanometer obtained is mixed Closing powder and be placed in drying baker dry, baking temperature is 50 DEG C, and drying time is 3h.It is laid in porcelain by loose for dried powder Bottom boat, powder overlay thickness is at below 1mm.Reduction reaction is carried out in hydrogen furnace, and the reaction first step is 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 It is 100～110L/h.Ni, W mixed-powder obtained is placed in high energy ball mill, uses liquid nitrogen gas washing, be continually fed into liquid nitrogen Ball milling is started after 15min.Ball milling uses the tungsten-cobalt hard alloy ball of a diameter of 3～5mm, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min.After mechanical ball milling 48h, ball milling is filled to move into and stands 30min in glove box and take out, obtain granularity 500～ The alloy powder of 800nm.

Claims (1)

1. the preparation method of a coating conductor NiW alloy base band alloy nano-powder, it is characterised in that include following step Rapid:
(1)NiO、WO3The mixing of powder and tube reducing
Choosing the NiO powder that granularity is 3～5 μm is 2 μm～the WO of 3 μm with granularity3Powder, is 5～12 by W atomic percentage conc Join powder, be placed in ball milling 20h in high energy ball mill and obtain the granularity alloy powder at 300nm～500nm；Ball milling uses 5mm～8mm Tungsten-cobalt hard alloy ball；Ball powder mass ratio is 20:1, and mechanical milling process is carried out under protective atmosphere, and rotational speed of ball-mill is 500rpm/min；
(2)NiO、WO3Two step reduction of nanometer mixed-powder
Being placed in drying baker by the nanometer mixed-powder that step (1) obtains and be dried, baking temperature is 50 DEG C, and drying time is 3h； Being laid in bottom porcelain boat by loose for dried powder, powder overlay thickness is at 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) obtains is placed in high energy ball mill, uses liquid nitrogen gas washing, be continually fed into liquid nitrogen Ball milling is started after 15min；Ball milling uses the tungsten-cobalt hard alloy ball of a diameter of 3～5mm, and ball powder mass ratio is 20: 1, and ball milling turns Speed is 300r/min；After mechanical ball milling 48h, ball milling is filled to move into and stands 30min in glove box and take out, obtain granularity 500～ The alloy powder of 800nm.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108385135A (en) * 2018-05-03 2018-08-10 北京工业大学 A kind of method of electrochemical deposition prepares coating conductor high-tungsten alloy base band billet

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