US20170225234A1 - A preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials - Google Patents

A preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials Download PDF

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US20170225234A1
US20170225234A1 US14/901,780 US201414901780A US2017225234A1 US 20170225234 A1 US20170225234 A1 US 20170225234A1 US 201414901780 A US201414901780 A US 201414901780A US 2017225234 A1 US2017225234 A1 US 2017225234A1
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rare earth
tungsten
earth oxide
dispersion strengthened
preparation
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Jinglian Fan
Yong Han
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Central South University
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Central South University
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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
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/0003—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • 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
    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/25—Oxide
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/04—Nanocrystalline

Definitions

  • the invention relates to field of nanomaterials and powder metallurgy field, especially a preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials by nano-composite technology.
  • Tungsten has characteristics such as high melting point, high hardness, good high temperature strength, thermal conductivity, electrical conductivity, low thermal expansion coefficient low sputtering and plasma effect, does not react with H, low H + retention, is a very important high temperature structural materials and functional materials and is widely used as a plasma facing material and divertor component material in the nuclear fusion field.
  • pure tungsten material is a widely used, typical high temperature materials.
  • tungsten grain size is about 100 microns
  • the ductile to brittle transition temperature (DBTT) is about 300 ⁇ 350 ⁇
  • the recrystallization temperature is of 1300 ⁇ 1350 ⁇
  • room temperature tensile strength is more than 500 MPa
  • high temperature tensile strength at 1000 ⁇ is about 400 MPa.
  • this material exists defects such as coarse grain, fiber microstructure, high DBTT, low recrystallization temperature, high brittleness.
  • the present invention adopts the heterogeneous precipitation—spray drying—calcining—thermal reduction—conventional sintering technology to prepare high performance rare-earth oxide dispersion strengthened fine grain tungsten materials, its density is close to full density (98.5% or higher), and the rare earth oxides particles evenly distribute in tungsten intracrystalline or grain boundary, its grain size is uniform and very fine (average in about 10 microns or less), with good room temperature and high temperature performance as well as high thermal loading shock resistance.
  • a rare earth oxide dispersion strengthened fine grain tungsten material its character is that includes: rare earth oxides referred to any one or more of Y 2 O 3 , La 2 O 3 , or in CeO 2 , the mass percent of the rare earth oxide is of 0.1 ⁇ 2%, and the rest ingredient is W.
  • The-mass percent of the rare earth oxide is of 0.1 ⁇ 2%, and the rest ingredient is W.
  • the coprecipitation coating particle colloidal is spray-dried at 350 ⁇ 450 ⁇ forming tungsten and rare earth oxide compound precursor powder, which is then calcined at 300 ⁇ 600 ⁇ for 1 ⁇ 4 h. After deaggregation and sieving, the calcined powder is hydrogen reduced at 600 ⁇ 850° C. for 2 ⁇ 6 h, ultrafine or nanoscale tungsten powder with particle size of 50 ⁇ 500 nm is obtained.
  • Rare earth oxides referred to any one or more of Y 2 O 2 , La 2 O 3 , or in CeO 2 ;
  • the ultrafine/nanoscale tungsten powder containing trace rare earth oxide prepared in step (1) is compression molded under 150 ⁇ 300 MPa using mold pressing or cold isostatic pressing;
  • the described tungstate is ammonium metatungstate, ammonium paratungstate or ammonium tungstate.
  • the described rare earth salts are nitrate, oxalate, carbonate, chloride or sulfate of Y, La or Ce.
  • the described stirring speed is 1000 ⁇ 5000 revolutions per minute.
  • the described spray drying nozzle rotating speed is 20000 ⁇ 30000 revolutions per minute.
  • reaction dispersant are stearic acid, polyethylene glycol (PEG), area, N, N-dimethyl formamide, OP emulsifier, twain-20 or sodium dodecyl sulfate, the mass fraction of reaction dispersant is of 0.1 ⁇ 1.5% of rare earth salt solution or tungstate solution.
  • the described acid is hydrochloric acid (HCl), nitric acid (HNO 3 ) or oxalic acid (H 2 C 2 O 4 ), the described alkali is sodium hydroxide (NaOH), potassium hydroxide (KOH), or aqueous ammonia (NH 3 ⁇ H 2 O).
  • heterogeneous precipitation—spray drying” adding rare earth oxide in tungsten matrix improves the compatibility of tungsten and rare earth oxides particles surface, spray drying achieves the uniformity of composition, microstructure in powder and alloy, so rare earth elements in tungsten matrix distribute more uniform, and do not introduce impurities.
  • ultrafine tungsten composite powder containing trace rare earth oxides prepared by “heterogeneous precipitation—spray drying—calcining—hydrogen reduction” method has much higher sintering activity;
  • the powder of this invention can reach more than 98.5% density sintered at 1800 ⁇ 2000 ⁇ by conventional sintering, grain size for sintered body is about 5 ⁇ 10 microns, and microstructure more evenly, excellent toughness at room temperature and high temperature.
  • the invention adopts the conventional sintering method preparation of rare earth oxide dispersion strengthened fine grain tungsten materials, the technological process is simple and suitable for engineering preparation.
  • the coprecipitated coating particle colloidal is spray-dried at 360 ⁇ , spray drying nozzle rotating speed is 20000 revolutions per minute, forming tungsten and rare earth oxide compound precursor powder,
  • the precursor powder is then calcined at 350 ⁇ for 2 h. After desegregation and sieving, the calcined powder is hydrogen reduced at 780° C. for 4 h, ultrafine tungsten powder containing 0.1 wt % Y 2 O 3 is obtained.
  • the ultrafine tungsten powder containing trace rare earth oxide is compression molded using mold pressing.
  • the pressing molded compaction is subjected to pre-sintering and then high temperature sintered at 1950 ⁇ for 2 h and W-0.1 wt %Y 2 O 3 material is obtained, its density is above 99.2%, its microstructure is uniform and very fine, average grain size is less than 10 microns.
  • This materials can bear 200 MW/m 2 high heat flux loading without surface crack appearing.
  • the coprecipitated coating particle colloidal is spray-dried at 400 ⁇ , spray drying nozzle rotating speed is 20000 revolutions per minute, forming tungsten and rare earth lanthanum oxide compound precursor powder.
  • the precursor powder is then calcined at 350 ⁇ for 2 h. After deaggregation and sieving, the calcined powder is hydrogen reduced at 780° C. for 4 h, ultrafine tungsten powder containing 0.3 wt % La 2 O 3 is obtained.
  • the ultrafine tungsten powder containing trace rare earth lanthanum oxide is compression molded using mold pressing.
  • the pressing molded compaction is subjected to pre-sintering and then high temperature sintered at 1950 ⁇ for 2 h and W-0.3 wt % La 2 O 3 material is obtained, its density is above 99.1%, its microstructure is uniform and very fine, average grain size is less than 8 microns.
  • This materials can bear 200 MW/m 2 high heat flux loading without surface crack appearing.
  • the coprecipitated coating particle colloidal is spray-dried at 400 ⁇ , spray drying nozzle rotating speed is 25000 revolutions per minute, forming tungsten and rare earth cerium oxide compound precursor powder.
  • the precursor powder is then calcined at 400 ⁇ for 2 h. After deaggregation and sieving, the calcined powder is two-step hydrogen reduced at 600 ⁇ for 2 h subsequent with 800 ⁇ for 2 h, ultrafine tungsten powder containing 0.5 wt % CeO 2 is obtained.
  • the ultrafine tungsten powder containing trace rare earth cerium oxide is compression molded using cold isostatic pressing.
  • the pressing molded compaction is subjected to pre-sintering and then high temperature sintered at 1950 ⁇ for 4 h and W-0.5 wt % CeO 2 material is obtained, its density is above 99.3%, its microstructure is uniform and very fine, average grain size is less than 8 microns.
  • This materials can bear 200 MW/m 2 high heat flux loading without surface crack appearing.
  • the coprecipitated coating particle colloidal is spray-dried at 450 ⁇ , spray drying nozzle rotating speed is 25000 revolutions per minute, forming tungsten and rare earth yttrium and lanthanum oxide compound precursor powder.
  • the precursor powder is then calcined at 400 ⁇ for 3 h. After disaggregation and sieving, the calcined powder is hydrogen reduced at 800 ⁇ for 3 h, ultrafine tungsten powder containing 0.3 wt % Y 2 O 3 +0.3 wt % La 2 O 3 is obtained.
  • the ultrafine tungsten powder containing trace rare earth yttrium and lanthanum oxide is compression molded using mold pressing.
  • the pressing molded compaction is subjected to pre-sintering at 1000 ⁇ for 2 h and then high temperature sintered at 1920 ⁇ for 3 h and W-0.3 wt % Y 2 +3.0 wt % La 2 O 3 material is obtained, its density is above 99.4%, its microstructure is uniform and very fine, average grain size is less than 6 microns. This materials can bear 300 MW/m 2 high heat flux loading without surface crack appearing.
  • the coprecipitated coating particle colloidal is spray-dried at 450 ⁇ , spray drying nozzle rotating speed is 30000 revolutions per minute, forming tungsten and rare earth yttrium+lanthanum+cerium oxide compound precursor powder.
  • the precursor powder is then calcined at 500 ⁇ for 3 h. After deaggregation and sieving, the calcined powder is two-step hydrogen reduced at 600 ⁇ for 2 h subsequent with 800 ⁇ for 4 h, ultrafine tungsten powder containing 0.3 wt % Y 2 O 3 -0.3 wt %La 2 O 3 0.3 wt %CeO 2 is obtained.
  • the ultrafine tungsten powder containing trace rare earth yttrium and lanthanum oxide is compression molded using mold pressing.
  • the pressing molded compaction is subjected to pre-sintering and then high temperature sintered at 1950 ⁇ for 4 h and W-0.3 wt %Y 2 O 3 -0.3 wt %La 2 O 3 -0.3 wt %CeO 2 material is obtained, its density is above 99.1%, its microstructure is uniform and very fine, average grain size is less than 5 microns.
  • This materials can bear 300 MW/m 2 high heat flux loading without surface crack appearing.

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