WO2022156216A1 - 一种合金线材及其制备方法与应用 - Google Patents

一种合金线材及其制备方法与应用 Download PDF

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WO2022156216A1
WO2022156216A1 PCT/CN2021/114939 CN2021114939W WO2022156216A1 WO 2022156216 A1 WO2022156216 A1 WO 2022156216A1 CN 2021114939 W CN2021114939 W CN 2021114939W WO 2022156216 A1 WO2022156216 A1 WO 2022156216A1
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alloy wire
alloy
tungsten
wire
powder
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PCT/CN2021/114939
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English (en)
French (fr)
Inventor
汤闵枫
方毅金
吕晟
郭东红
吴先月
彭福生
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厦门虹鹭钨钼工业有限公司
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Priority to EP21920595.2A priority Critical patent/EP4212641A4/en
Priority to US18/248,592 priority patent/US20230374634A1/en
Priority to JP2023528201A priority patent/JP2023551646A/ja
Publication of WO2022156216A1 publication Critical patent/WO2022156216A1/zh
Priority to ZA2023/04296A priority patent/ZA202304296B/en

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    • 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
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F1/16—Metallic particles coated with a non-metal
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/12—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23D—PLANING; SLOTTING; SHEARING; BROACHING; SAWING; FILING; SCRAPING; LIKE OPERATIONS FOR WORKING METAL BY REMOVING MATERIAL, NOT OTHERWISE PROVIDED FOR
    • B23D61/00—Tools for sawing machines or sawing devices; Clamping devices for these tools
    • B23D61/18—Sawing tools of special type, e.g. wire saw strands, saw blades or saw wire equipped with diamonds or other abrasive particles in selected individual positions
    • B23D61/185—Saw wires; Saw cables; Twisted saw strips
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
    • B28D5/045—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with wires or closed-loop blades
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/057—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of phases other than hard compounds by solid state reaction sintering, e.g. metal phase formed by reduction reaction
    • 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
    • C22C1/059—Making alloys comprising less than 5% by weight of dispersed reinforcing phases
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D1/00—Woven fabrics designed to make specified articles
    • D03D1/0035—Protective fabrics
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/60—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the warp or weft elements other than yarns or threads
    • D03D15/67—Metal wires
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • B22F2007/066—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using impregnation
    • 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
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/20—Metallic fibres
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2501/00—Wearing apparel
    • D10B2501/04—Outerwear; Protective garments
    • D10B2501/041—Gloves

Definitions

  • the invention relates to the technical field of tungsten alloy materials, in particular to an alloy wire material and a preparation method and application thereof.
  • hardness materials include high carbon steel wire, tungsten wire and so on.
  • the tensile strength of the existing high carbon steel wire is generally below 4500MPa, but the diameter is larger than 50 ⁇ m, and has reached the processing limit, and cannot be processed to a finer diameter.
  • tungsten has unparalleled flexibility at bend radii of less than 1 mm, while stainless steel wire rope can fail due to multiple cycles of bending stress at the same extremely small bend radius; in comparison, 316 stainless steel at 2,500– Melting at 2,550°F and tungsten at 6,192°F, tungsten still performs well in mechanical rope applications where good temperature resistance and excellent tensile strength are required.
  • tungsten is gradually becoming a more performance-advantaged material for making micromechanical filaments for medical and industrial use, thanks to its two main advantages: long life and flexibility. Because tungsten is strong, flexible and resistant to high temperatures, the tungsten wire ropes made from it are strong and durable, requiring no maintenance or replacement over long periods of time. First, tungsten is one of the toughest materials known to man. Diamond has a Mohs scale of 10 and tungsten has a Mohs scale of 9, compared to about 6 for stainless steel.
  • the tensile strength of conventional tungsten wire is generally below 4000MPa, however, its toughness is poor, the production process is complex, and the processing is extremely difficult, making it difficult to achieve effective mass production. Therefore, there is no wire on the market that is suitable for mass production, and has high strength and high toughness above 4500MPa, but in the cutting of high hardness materials such as semiconductor materials sapphire, silicon carbide, silicon wafers, and magnetic materials, high In applications such as precision instruments and cables or ropes drawn by high-temperature furnaces, there is an urgent need for a filament with higher strength, toughness and fineness, so that it can meet various realistic needs in practical applications in this field.
  • the present invention provides an alloy wire, the alloy wire is made of tungsten alloy, and the tungsten
  • the alloy contains oxides of tungsten and lanthanum; the wire diameter of the alloy wire is 100 ⁇ m or less; the tensile strength of the alloy wire is 3800 MPa or more.
  • the oxide content of lanthanum in the alloy wire is 0.1 wt % to 2.0 wt %.
  • the wire diameter of the alloy wire is 60 ⁇ m or less; the push-pull core wire diameter of the alloy wire is 350 ⁇ m or less;
  • the ultimate elastic strength of the alloy wire is above 2500MPa; the tensile strength of the alloy wire is above 4200MPa.
  • the tungsten alloy also contains a metal element M, and the metal element M is selected from at least one of potassium, rhenium, molybdenum, iron, cobalt or rare earth metals.
  • the content of potassium is less than 80ppm.
  • the tungsten alloy also contains one or more rare earth oxides other than lanthanum oxides.
  • the present invention provides a method for preparing an alloy wire as described above, which includes doping powder milling, pressing, sintering, and billeting;
  • the blanking includes blanking the sintered billet by means of multi-roll rolling, so that the ratio of the oxide particles of lanthanum in the tungsten rod after rolling to the particle size of the longitudinal length of the wire material to the particle cross-section is greater than 5.
  • the doping powder milling comprises the following steps:
  • the solid-liquid doping includes drying the mixed tungsten doping solution in stages, and the staged drying includes at least two temperature stages. Heating and drying below 100°C, and then heating and drying above 100°C.
  • the staged drying in the solid-liquid doping includes a first drying stage and a second drying stage, the temperature of the first drying stage is 60-80° C., and the second drying stage The temperature of the stage is 110 to 150°C.
  • the reduction includes reducing the material obtained after solid-liquid doping into alloy powder with an average Fisher particle size of 1.0-4.0 ⁇ m.
  • the doping powder milling comprises the following steps:
  • the solid-solid doping includes mixing tungsten powder with a Fisher particle size of 1.0 ⁇ m ⁇ 4.0 ⁇ m and lanthanum oxide with particle size distribution D90 ⁇ 2.0 ⁇ m as raw materials to obtain tungsten powder doped with lanthanum oxide.
  • the lanthanum oxide particle size of the sintered billet is less than 2.5 ⁇ m.
  • the invention provides an application of an alloy wire in the field of material cutting
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • the material includes at least a hard surface material; the hard surface material at least includes a silicon wafer, a magnetic material, and a semiconductor material; and the semiconductor material at least includes sapphire and silicon carbide.
  • the invention provides the application of an alloy wire in cables/ropes
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • the cable/rope is used for medical/industrial precision instruments and high temperature furnace traction.
  • the invention provides the application of an alloy wire in the textile field
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • the alloy wire includes gloves or protective clothing made by spinning or weaving the alloy wire.
  • an alloy wire rod and a preparation method and application thereof provided by the present invention have the following beneficial effects:
  • the wire diameter is 100 ⁇ m and below, and the tensile strength is above 3800MPa;
  • the wire diameter of the alloy wire is 60 ⁇ m or less; the diameter of the push-pull core wire of the alloy wire is 350 ⁇ m or less; the elastic proof strength of the alloy wire is above 2500MPa; the tensile strength of the alloy wire is above 4200MPa .
  • FIG. 1 is a schematic structural diagram of the equipment for push-pull toughness detection provided by the present invention.
  • the invention provides an alloy wire, the alloy wire is made of tungsten alloy, and the tungsten alloy contains tungsten and rare earth oxide;
  • the wire diameter of the alloy wire is 400 ⁇ m or less
  • the tensile strength of the alloy wire is above 2800MPa.
  • the wire diameter of the alloy wire is 100 ⁇ m or less; the tensile strength of the alloy wire is 3800 MPa or more.
  • the wire diameter of the alloy wire is 60 ⁇ m or less; the diameter of the push-pull core wire of the alloy wire is 350 ⁇ m or less;
  • the ultimate elastic strength of the alloy wire is above 2500MPa; the tensile strength of the alloy wire is above 4200MPa.
  • the wire diameter of the alloy wire is 40 ⁇ m or less; the tensile strength of the alloy wire is 4800 MPa or more.
  • the wire diameter of the alloy wire is 25 ⁇ m or less; the tensile strength of the alloy wire is 5000 MPa or more.
  • the tensile strength of the alloy wire may be 2800 MPa or more.
  • the tensile strength of the alloy wire can also be above 3200MPa, can also be above 3800MPa, and can also be above 4200MPa or even 4800MPa or 5000MPa;
  • the proof strength of the alloy wire may be 2500 MPa or more.
  • the ultimate elastic strength of the alloy wire can also be above 2700MPa, and can also be above 3000MPa or even 3200MPa;
  • the wire diameter of the alloy wire may be 400 ⁇ m or less.
  • the wire diameter of the alloy wire is 400 ⁇ m, 350 ⁇ m, 300 ⁇ m, 250 ⁇ m, 200 ⁇ m, 150 ⁇ m, 100 ⁇ m, 80 ⁇ m, even 60 ⁇ m, 40 ⁇ m, 25 ⁇ m, 20 ⁇ m and 10 ⁇ m, etc.
  • the alloy wire may be uniform or not completely uniform Yes, it can also contain a difference of several percentages such as 1% according to the site.
  • the wire diameter of the alloy wire can be 60 ⁇ m or less, so the alloy wire has flexibility and is easy to bend sufficiently, and therefore, the alloy wire can be easily wound;
  • the diameter of the push-pull core wire of the alloy wire can be less than 350 ⁇ m.
  • the alloy wire also has excellent push-pull toughness.
  • the wire diameter of the alloy wire is 200 ⁇ m to 400 ⁇ m
  • the tensile strength of the alloy wire can be 2800 MPa to 4000 MPa, for example, the tensile strength can reach 3000 MPa, 3500 MPa, or even 4000 MPa;
  • the wire diameter of the alloy wire can be 100-200 ⁇ m, and the tensile strength of the alloy wire can be 3200-4800MPa, for example, the tensile strength can reach 3400MPa, can also reach 4000MPa, can also reach 4500MPa, or even reach 4800MPa;
  • the rare earth oxide is selected from dysprosium oxide, erbium oxide, neodymium oxide, yttrium oxide, europium oxide, gadolinium oxide, lanthanum oxide, praseodymium oxide, holmium oxide, cerium oxide, terbium oxide, ytterbium oxide, oxide One or more of samarium, praseodymium neodymium oxide, thulium oxide, lutetium oxide, scandium oxide, and promethium oxide.
  • common rare earth oxides include dysprosium oxide (Dy 2 O 3 ), erbium oxide (Er 2 O 3 ), neodymium oxide (Nd 2 O 3 ), yttrium oxide (Y 2 O 3 ), europium oxide (Eu 2 O 3 ), gadolinium oxide (Gd 2 O 3 ), lanthanum oxide (La 2 O 3 ), praseodymium oxide (Pr 6 O 11 ), holmium oxide (Ho 2 O 3 ), cerium oxide (CeO 2 ), Terbium oxide (Tb 4 O 7 ), ytterbium oxide (Yb 2 O 3 ), samarium oxide (Sm 2 O 3 ), praseodymium neodymium oxide ((Pr+Nd) x O y ), thulium oxide (Tm 2 O 3 ), Lutetium oxide (Lu 2 O 3 ), scandium oxide (Sc 2 O 3 ), promethium oxide (Pm 2 O 3 ), dyspro
  • the rare earth oxides are mainly distributed at the grain boundaries of the tungsten main phase (matrix phase), and also have a small amount of distribution in the grains of the matrix phase, and the rare earth oxides can be distributed in the form of lines or particle strings.
  • the rare earth oxide can also be a rare earth-metal composite oxide, such as YSZ, LSCO and the like.
  • the tungsten alloy can also contain trace amounts of carbides, other rare elements or metal and non-metallic elements, for example, the carbides include TiC, ZrC, the other rare elements include Re, etc., the non-metallic elements Elements include C, etc., and the metal elements include potassium, rhenium, molybdenum, iron, cobalt, etc.;
  • the content of K is less than 80ppm.
  • the addition of an appropriate amount of K can improve the high temperature performance of the material, but if the content is too high, it will affect the processing performance and cause cracks and broken wires;
  • the content of the tungsten is 97.0 wt % to 99.9 wt %, and the content of the rare earth oxide is 0.1 wt % to 3.0 wt %.
  • the content of the tungsten can also be more than 95wt%; preferably, the content of the tungsten is 97.0wt% ⁇ 99.9wt%, such as 97.5wt%, 98wt%, 98.5wt%, 99wt%, 99.5wt% and many more;
  • the content of the rare earth oxide may be 0.1wt% to 3.0wt%, or 0.1wt% to 2wt%, or 0.1wt% to 1wt%, or 0.3wt% to 0.8wt% , of course, it can also be taken as 0.1wt%, 0.3wt%, 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, 2wt%, etc.
  • the tungsten alloy further includes a metal element, and the metal element is at least one of potassium, rhenium, molybdenum, iron, and cobalt.
  • the potassium content is less than 80 ppm.
  • the tungsten alloy further includes carbon.
  • the present invention provides a method for preparing an alloy wire as described above, which includes doping powder milling, pressing, sintering, and billeting. , so that the ratio of the rare earth oxide particles in the tungsten rod after rolling along the longitudinal length of the wire to the particle size of the particle cross-section is >5.
  • the doping and pulverizing comprises the following steps: solid-liquid doping, reduction, and pulverizing;
  • the solid-liquid doping includes drying the mixed tungsten doping solution in stages, and the staged drying includes at least two temperature stages. Heating and drying below 100°C, and then heating and drying above 100°C. For example, heating and drying at 60°C ⁇ 80°C for 2h ⁇ 6h, and then heating and drying at 110°C ⁇ 150°C for 3h ⁇ 5h;
  • the step-by-step heating and drying adopts a drying method of first low temperature and then high temperature, that is, drying at a temperature lower than 100 ° C, so that the rare earth salt particles are slowly precipitated, and the number of nucleation is large, and then the temperature is higher than 100 ° C. Drying, the rare earth salt particles with a large number of particles have no time to merge and grow, so that the particle size can be greatly refined;
  • the staged drying includes at least two temperature stages, and the two temperature stages take 100°C as the dividing line, firstly heating and drying at 100°C, and then heating and drying above 100°C;
  • the staged drying in the solid-liquid doping includes a first drying stage and a second drying stage, the temperature of the first drying stage is 60-80° C., and the first drying stage The temperature of the second drying stage is 110-150°C.
  • heating and drying with multiple temperature gradients or multiple temperature stages can be performed respectively, for example, drying at 60°C for 2 hours, and then drying at 60°C for 2 hours. Dry at 80°C for 2h, and then heat up to 120°C for drying; of course, the above-mentioned embodiments only express several embodiments of the present invention, and for those of ordinary skill in the art, without departing from the present invention Under the premise of the concept, adjustments and changes in several temperature stages can also be made, which all belong to the protection scope of the present invention.
  • the reducing comprises reducing the material obtained after solid-liquid doping into alloy powder in a reduction furnace.
  • the average Fisher particle size of the alloy powder is 1.0-4.0 ⁇ m.
  • the doping and pulverizing comprises the following steps: liquid-liquid doping, reduction, and pulverizing;
  • the liquid-liquid doping includes mixing a tungstic acid and/or tungstate salt solution with a soluble rare earth salt solution.
  • the doping powder milling comprises the steps of: solid-solid doping
  • the solid-solid doping includes mixing tungsten powder with a Fisher particle size of 1.0 ⁇ m-4.0 ⁇ m and rare earth oxide with a particle size distribution D90 ⁇ 2.0 ⁇ m as raw materials to obtain a rare earth oxide doped tungsten powder.
  • the solid-solid doping further comprises removing coarse particles by a water precipitation method to obtain rare earth oxide fine particles;
  • rare earth oxides with D90 ⁇ 2 ⁇ m are obtained by 3-stage precipitation with a precipitation time of 30-120 minutes;
  • the rare earth oxide fine particles have a D90 ⁇ 2 ⁇ m.
  • the particle size of the rare earth oxide of the sintered billet is less than 2.5 ⁇ m.
  • steps such as reduction, milling and other steps in the above steps are preferably but not limited to the following embodiments, namely:
  • Pulverizing The alloy powder obtained after reduction is mixed, and after mixing, the alloy powder with an average Fisher particle size of 1.0-4.0 ⁇ m is placed in a powder mixer. Mix powder at a speed of 6-10 rpm for 60-90 minutes;
  • Powder compaction by isostatic pressing, the powder with the average Fibonacci particle size of 1.0 ⁇ m to 4.0 ⁇ m is pressed into a compact with a unit weight of 1.5kg to 5.0kg under a pressure of 160MPa to 260MPa, and the compaction is pressed in a hydrogen atmosphere. Pre-sintering is performed, and the temperature of the pre-sintering is preferably 1200-1400° C. to increase the strength of the compact;
  • Sintering sintering, the sintering temperature is preferably 1800-2400° C., and the sintering time is preferably 5-15 hours, to obtain a sintered billet with a density of 17.5-18.5 g/cm 3 ;
  • the use of the multi-roll mill ensures that the ratio of the rare earth oxide particles in the tungsten rod after rolling along the longitudinal length of the wire to the particle size of the particle cross-section is >5;
  • a low temperature stress relief annealing process within 1000°C can be applied to the produced alloy wire, so as to homogenize its stress distribution and improve its linearity; the process can be carried out in a heating furnace or in other equipment. , Specifically, the alloy wire can also be subjected to low temperature stress relief annealing under the protection of hydrogen;
  • the drawn wire can be electropolished and cleaned to make the surface of the wire smooth; for example, in the electropolishing process, the alloy wire and carbon rods are dipped in the electrolyte solution to immerse the opposite electrodes such as the alloy wire to the alloy wire. It is performed by energizing between the opposing electrode and the like.
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • the material includes at least a hard surface material; the hard surface material includes at least a silicon wafer, a magnetic material, and a semiconductor material; and the semiconductor material at least includes sapphire and silicon carbide.
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • the cable/rope is used for medical/industrial precision instruments and high temperature furnace traction.
  • the alloy material adopts the above-mentioned alloy wire rod or the alloy wire rod prepared by the above-mentioned alloy wire rod preparation method.
  • it includes gloves or protective clothing made by spinning or weaving the alloy wire.
  • an alloy wire is provided, the alloy wire is made of tungsten alloy, and the tungsten alloy includes oxides of tungsten and lanthanum;
  • the content of the tungsten is more than 90wt%, and the oxide content of the lanthanum is more than 0.1wt% and less than 2.0wt%;
  • the content of the tungsten can also be more than 95wt%; preferably, the content of the tungsten is 97.0wt% ⁇ 99.9wt%, such as 97.5wt%, 98wt%, 98.5wt%, 99wt%, 99.5wt% and many more;
  • the oxide content of the lanthanum can be 0.1wt% to 2wt%, or 0.1wt% to 1wt%, or 0.3wt% to 0.8wt%, of course, it can also be 0.1wt%, 0.3wt% wt%, 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, 2wt%, etc.
  • the oxide of lanthanum is preferably lanthanum oxide (La 2 O 3 ).
  • the oxides of lanthanum are mainly distributed at the grain boundaries of the tungsten main phase (matrix phase), and a small amount is also distributed in the grains of the matrix phase.
  • the oxides of lanthanum can be distributed in the form of lines or particle strings. .
  • the oxide of lanthanum may also be a lanthanum-metal composite oxide, such as LSCO and the like.
  • the tungsten alloy can also contain trace amounts of carbides, other rare elements, metals and non-metallic elements, for example, the carbides include TiC, ZrC, the other rare elements include rhenium, etc., the non-metallic elements Including C, etc., the metal elements include potassium, molybdenum, iron, cobalt, etc.;
  • the content of potassium is less than 80ppm, the addition of an appropriate amount of potassium can improve the high temperature performance of the material, but if the content is too high, it will affect the processing performance and cause cracks and broken wires;
  • an alloy wire material is provided, the alloy wire material is made of tungsten alloy, and the tungsten alloy includes oxides of tungsten and cerium;
  • the content of the tungsten is more than 90wt%, and the oxide content of the cerium is more than 0.1wt% and less than 1.5wt%;
  • the content of the tungsten can also be more than 95wt%; preferably, the content of the tungsten is 97.0wt% ⁇ 99.9wt%, such as 97.5wt%, 98wt%, 98.5wt%, 99wt%, 99.5wt% and many more;
  • the oxide content of the cerium can be 0.2wt% to 1.5wt%, or 0.2wt% to 1wt%, or 0.3wt% to 0.8wt%, of course, it can also be 0.2wt%, 0.3wt%, 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, etc.
  • the oxide of cerium is preferably cerium oxide (CeO2).
  • an alloy wire is provided, the alloy wire is made of tungsten alloy; the tungsten alloy includes oxides of tungsten and yttrium;
  • the content of the tungsten is more than 90wt%, and the oxide content of the yttrium is more than 0.1wt% and less than 1.5wt%;
  • the content of the tungsten can also be more than 95wt%; preferably, the content of the tungsten is 97.0wt% ⁇ 99.9wt%, such as 97.5wt%, 98wt%, 98.5wt%, 99wt%, 99.5wt% and many more;
  • the yttrium oxide content may be 0.2wt% to 1.5wt%, or 0.2wt% to 1wt%, or 0.3wt% to 0.8wt%, of course, it can also be 0.2wt%, 0.3wt%, 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, etc.
  • the yttrium oxide is preferably yttrium oxide (Y 2 O 3 ), and the performance of the alloy wire can be improved by increasing the oxide content of yttrium
  • the oxide content of yttrium is greater than 1.5 wt %, the difficulty of refining the alloy wire will be greatly improved.
  • the tensile strength of the alloy wire is above 3800MPa, and can also be above 4200MPa or even 4800MPa or 5000MPa;
  • the ultimate tensile strength of the alloy wire is 2500 MPa or more.
  • the ultimate elastic strength of the alloy wire can also be above 2700MPa, and can also be above 3000MPa or even 3200MPa;
  • the wire diameter of the alloy wire is 100 ⁇ m or less.
  • the wire diameter of the alloy wire is 100 ⁇ m, 80 ⁇ m, or even 60 ⁇ m, 40 ⁇ m, 25 ⁇ m, 20 ⁇ m and 10 ⁇ m, etc.
  • the diameter of the alloy wire may be uniform or not completely uniform, and may also contain, for example, 1%, etc. A difference of a few percentages.
  • the wire diameter of the alloy wire can be 60 ⁇ m or less, so the alloy wire has flexibility and is easy to bend sufficiently, and therefore, the alloy wire can be easily wound;
  • the diameter of the push-pull core wire of the alloy wire can be less than 350 ⁇ m.
  • the alloy wire also has excellent push-pull toughness.
  • the wire diameter of the alloy wire is 100 ⁇ m or less; the tensile strength of the alloy wire is 3800 MPa or more;
  • the wire diameter of the alloy wire is 60 ⁇ m or less; the tensile strength of the alloy wire is more than 4200 MPa; the elastic proof strength of the alloy wire is more than 2500 MPa, the diameter of the push-pull core wire of the alloy wire is 350 ⁇ m or less, or even Below 180 ⁇ m;
  • the wire diameter of the alloy wire is 40 ⁇ m or less; the tensile strength of the alloy wire is above 4800 MPa; the elastic proof strength of the alloy wire is above 2700 MPa, the diameter of the push-pull core wire of the alloy wire is below 350 ⁇ m, or even Below 200 ⁇ m;
  • the wire diameter of the alloy wire is 25 ⁇ m or less; the tensile strength of the alloy wire is more than 5000 MPa; the elastic proof strength of the alloy wire is more than 3000 MPa, the diameter of the push-pull core wire of the alloy wire is 350 ⁇ m or less, or even Below 250 ⁇ m;
  • the invention provides a preparation method of an alloy wire:
  • the steps of the preparation method include doping powder milling, pressing, sintering, blanking, pressure processing, etc.;
  • the doping pulverizing is divided into solid-liquid method, liquid-liquid method, solid-solid method, etc. according to different process methods;
  • the doping powder milling includes the following steps:
  • the solid-liquid doping method includes: doping an appropriate amount of soluble lanthanum salt solution into the tungsten powder, and after fully stirring, heating and drying in stages to obtain the result;
  • the step-by-step heating and drying adopts a drying method of first low temperature and then high temperature, that is, drying is performed at a temperature lower than 100 ° C, so that the salt particles of lanthanum are slowly precipitated, and the number of nuclei is large, and then the temperature is higher than 100 ° C. Under drying, the salt particles of lanthanum with a large number of particles do not have time to merge and grow, so that the particle size can be greatly refined;
  • the staged drying includes at least two temperature stages, and the two temperature stages take 100°C as the dividing line, firstly heating and drying at 100°C, and then heating and drying above 100°C; Heating and drying at 60°C ⁇ 80°C for 2h ⁇ 6h, then heating and drying at 110°C ⁇ 150°C for 3h ⁇ 5h;
  • heating and drying with multiple temperature gradients or multiple temperature stages can be performed respectively, for example, drying at 60°C for 2 hours, and then drying at 60°C for 2 hours. Dry at 80°C for 2h, and then heat up to 120°C for drying; of course, the above-mentioned embodiments only express several embodiments of the present invention, and for those of ordinary skill in the art, without departing from the present invention Under the premise of the concept, adjustments and changes in several temperature stages can also be made, which all belong to the protection scope of the present invention.
  • a proper amount of lanthanum in the form of nitrate solution is uniformly doped into blue tungsten powder, and after fully stirring, it is first heated at 60°C to 80°C for 2h to 6h, and then heated at 110°C to 150°C for 3h to 5h. ;
  • the doping powder milling includes the following steps:
  • the liquid-liquid doping method includes: doping tungstic acid and/or tungstate solution and soluble lanthanum salt solution to obtain lanthanum salt-doped tungsten powder subsequently;
  • liquid-liquid doping is performed using ammonium metatungstate solution and lanthanum salt solution as raw materials to obtain blue tungsten powder doped with lanthanum salt;
  • the doping powder milling includes the following steps: solid-solid doping;
  • the solid-solid doping method includes: using tungsten powder with a Fisher particle size of 1.0 ⁇ m to 4.0 ⁇ m and lanthanum oxide with a particle size distribution D90 ⁇ 2.0 ⁇ m as raw materials, and performing solid-solid doping and mixing to obtain lanthanum-doped lanthanum. Tungsten oxide powder;
  • the step of solid-solid doping also includes removing coarse particles by a water precipitation method to obtain fine oxide particles of lanthanum;
  • lanthanum oxides with D90 ⁇ 2 ⁇ m are obtained by 3-stage precipitation with a precipitation time of 30-120 minutes;
  • steps such as reduction, milling and other steps in the above steps are preferably but not limited to the following embodiments, namely:
  • the material obtained by doping solid-liquid and/or liquid-liquid is reduced to alloy powder at one time in a four-temperature zone reduction furnace;
  • Pulverizing The alloy powder obtained after reduction is mixed, and after mixing, the alloy powder with an average Fisher particle size of 1.0-4.0 ⁇ m is placed in a powder mixer. Mix powder at a speed of 6-10 rpm for 60-90 minutes;
  • Powder compaction by isostatic pressing, the powder with the average Fibonacci particle size of 1.0 ⁇ m to 4.0 ⁇ m is pressed into a compact with a unit weight of 1.5kg to 5.0kg under a pressure of 160MPa to 260MPa, and the compaction is pressed in a hydrogen atmosphere. Pre-sintering is performed, and the temperature of the pre-sintering is preferably 1200-1400° C. to increase the strength of the compact;
  • Sintering sintering, the sintering temperature is preferably 1800-2400° C., and the sintering time is preferably 5-15 hours, to obtain a sintered billet with a density of 17.5-18.5 g/cm 3 ;
  • the use of the multi-roll mill ensures that the ratio of the oxide particles of lanthanum in the tungsten rod after rolling along the longitudinal length of the wire to the particle size of the particle cross-section is greater than 5;
  • a low temperature stress relief annealing process within 1000°C can be applied to the produced alloy wire, so as to homogenize its stress distribution and improve its linearity; the process can be carried out in a heating furnace or in other equipment. , Specifically, the alloy wire can also be subjected to low temperature stress relief annealing under the protection of hydrogen;
  • the drawn wire can be electropolished and cleaned to make the surface of the wire smooth; for example, in the electropolishing process, the alloy wire and carbon rods are dipped in the electrolyte solution to immerse the opposite electrodes such as the alloy wire to the alloy wire. It is performed by energizing between the opposing electrode and the like.
  • the present invention Compared with the conventional tungsten alloy wire, the present invention has the following features and advantages:
  • the drying adopts a staged type of drying at a low temperature (below 100° C.) and drying at a high temperature (above 100° C.). Drying mode for drying.
  • the nitrate particles of lanthanum are slowly precipitated, and the number of nucleation is large; then the nitrate particles of lanthanum with a large number of particles are too late to merge and grow, and the particle size can be greatly refined by this drying method.
  • the nucleation and crystallization rates of lanthanum nitrate are controlled by adjusting the doping drying temperature, so that the lanthanum nitrate crystals on the doped blue tungsten particles are finer.
  • the coarse particles are removed by water precipitation.
  • the characteristics of fast precipitation of coarse particles and slow precipitation of fine particles are used to obtain lanthanum oxides with D90 ⁇ 2 ⁇ m by 3-stage precipitation with a precipitation time of 30-120 minutes;
  • the lanthanum oxide particle size on the surface of the tungsten powder particles produced by the present invention and the lanthanum oxide particle size in the sintered billet are smaller than those of the traditional method, and the lanthanum oxide particle size is less than 2.5 ⁇ m and the distribution is more uniform , the product performance is more stable;
  • the multi-roll rolling method is used to open the sintered billet.
  • the severe radial processing of the rotary forging causes the fracture of the dispersed particles of lanthanum, forcing the dispersed particles to form voids in the voids of the tungsten matrix.
  • This processing method will lead to subsequent material stress concentration and defects, and then Difficulty in subsequent processing.
  • the use of multiple rolls (three rolls/four rolls) will make the fibrous structure of the matrix of the alloy material more developed and the rate of longitudinal deformation faster, which will lead to the refinement and deformation of the dispersed particles of lanthanum oxide.
  • the cross-sectional size of the particles becomes smaller, and the axial size becomes longer, so as to ensure that the tungsten matrix and the dispersed particles have good plasticity and toughness after blanking.
  • the dispersed particles can further form a fiber-reinforced structure. Thereby improving the strength and toughness of the tungsten wire.
  • the present invention provides the following examples and comparative examples:
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 0.15wt%, and W is 99.85wt%.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 1.5 wt %, and W is 98.5 wt %.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 1.8 wt %, and W is 98.2 wt %.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high - strength and high - toughness tungsten alloy wire is prepared according to the present invention.
  • Step 1 Doping: Evenly dope an appropriate amount of lanthanum nitrate solution into the potassium-doped tungsten powder with a potassium content of 50 ppm. After fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C. drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 1 wt %, Y 2 O 3 is 0.2 wt %, and W is 98.8 wt %.
  • Step 1 Doping: Evenly dope an appropriate amount of lanthanum nitrate solution and yttrium nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C. drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • the comparative examples in this group are tungsten alloy wires produced by conventional processes, and the material element composition is the same as that of Example 1: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, after fully stirring, steam drying, the temperature is 120 ° C, and the drying time is 4 hours;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: use multi-pass rotary forging to open the 23mm diameter sintered billet into an 8.0mm alloy rod;
  • Step 7 pressure processing: then through multi-pass rotary forging and through drawing dies of different specifications for drawing processing, and repeating the drawing for many times to make alloy wires of different specifications and diameters;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, after fully stirring, steam drying, the temperature is 120 ° C, and the drying time is 4 hours;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: use multi-pass rotary forging to open the 23mm diameter sintered billet into an 8.0mm alloy rod;
  • Step 7 pressure processing: then through multi-pass rotary forging and through drawing dies of different specifications for drawing processing, and repeating the drawing for many times to make alloy wires of different specifications and diameters;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 0.07wt%, and W is 99.93wt%.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 2.2wt%, and W is 97.8wt%.
  • Step 1 Doping: uniformly dope an appropriate amount of lanthanum nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Solid-solid doping: put the lanthanum oxide powder in the aqueous solution, stir for 5 minutes, pour the upper layer solution into the secondary water tank and stir for 5 minutes, set it to settle for 10 minutes, pour the upper layer aqueous solution into the tertiary water tank Stir for another 5 minutes, leave to precipitate for 30 minutes, pour the upper layer solution into a 4-level container for precipitation for 24 hours, filter out the solution, heat to 100 degrees and dry for 24 hours to obtain D90 ⁇ 2.0 ⁇ m lanthanum oxide powder; use tungsten with an average particle size of 2.0 ⁇ m The powder and the appropriate amount of lanthanum oxide powder with D90 ⁇ 2.0 ⁇ m after water precipitation treatment are uniformly mixed for 60 minutes by powder mixing equipment;
  • Step 2 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 3 High-temperature sintering: perform high-temperature sintering to obtain a sintered billet with a density of 18.10 g/cm 3 ;
  • Step 4 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an alloy rod of 8.0mm;
  • Step 5 Press processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element composition is: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Solid-solid doping: use tungsten powder with an average particle size of 2.0 ⁇ m and an appropriate amount of lanthanum oxide powder to uniformly mix for 60 minutes through powder mixing equipment;
  • Step 2 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 3 High-temperature sintering: perform high-temperature sintering to obtain a sintered billet with a density of 18.10 g/cm 3 ;
  • Step 4 Billeting: Billeting: using multi-pass rotary forging to open the 23.0mm diameter sintered billet into an 8.0mm alloy rod;
  • Step 5 pressure processing: then through multi-pass rotary forging and through drawing dies of different specifications for drawing processing, and repeating the drawing for many times to make alloy wires of different specifications and diameters;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Solid-solid doping: use tungsten powder with an average particle size of 2.0 ⁇ m and an appropriate amount of lanthanum oxide powder to uniformly mix for 60 minutes through powder mixing equipment;
  • Step 2 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 3 High-temperature sintering: perform high-temperature sintering to obtain a sintered billet with a density of 18.10 g/cm 3 ;
  • Step 4 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an alloy rod of 8.0mm;
  • Step 5 Press processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: La 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Solid-solid doping: put an appropriate amount of lanthanum oxide powder in the aqueous solution, stir for 5 minutes, pour the upper layer solution into the secondary water tank, stir for 5 minutes, and put the upper layer aqueous solution into the tertiary water tank after settling for 10 minutes Stir for 5 minutes, leave to precipitate for 30 minutes, pour the upper layer solution into a 4-level container for precipitation for 24 hours, filter out the solution, heat to 100 degrees and dry for 24 hours to obtain D90 ⁇ 2.0 ⁇ m lanthanum oxide powder; the average particle size is 2.0 ⁇ m Tungsten powder and appropriate amount of lanthanum oxide powder with D90 ⁇ 2.0 ⁇ m after water precipitation treatment are uniformly mixed for 60 minutes by powder mixing equipment;
  • Step 2 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 3 High-temperature sintering: perform high-temperature sintering to obtain a sintered billet with a density of 18.10 g/cm 3 ;
  • Step 4 Billeting: Billeting: using multi-pass rotary forging to open the 23mm diameter sintered billet into an 8.0mm alloy rod;
  • Step 5 pressure processing: then through multi-pass rotary forging and through drawing dies of different specifications for drawing processing, and repeating the drawing for many times to make alloy wires of different specifications and diameters;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: CeO 2 is 1wt%, and W is 99wt%.
  • Step 1 Doping: uniformly dope an appropriate amount of cerium nitrate solution into the blue tungsten powder, and after fully stirring, first dry at a low temperature of 80 °C for 4 hours, and then dry at a high temperature of 120 °C for drying;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm3;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a high-strength and high-toughness tungsten alloy wire is prepared according to the present invention, and its material element components are: Y 2 O 3 is 1 wt %, and W is 99 wt %.
  • Step 1 Doping: uniformly dope an appropriate amount of yttrium nitrate solution into the blue tungsten powder, after fully stirring, first dry at a low temperature of 80°C for 4 hours, and then dry at a high temperature of 120°C;
  • Step 2 reduction: the material obtained in step 1 is once reduced to alloy powder of suitable particle size in a four-temperature zone reduction furnace;
  • Step 3 Mixing powder: The materials obtained in step 2 are placed in a powder mixer according to different particle size compositions. Mix powder at 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powders with different particle sizes are pressed into a compact with a single weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering to obtain sintered billets with a density of 18.10 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650°C, the sintered billet with a diameter of 23.0mm is continuously rolled into an 8.0mm alloy rod;
  • Step 7 Press processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • a rhenium-tungsten alloy wire is prepared, and the material element composition of the material is that Re is 1 wt % and W is 99 wt %. Its preparation is as follows:
  • Step 1 Doping: Weigh the tungsten powder and ammonium rhenate according to the weight percentage, add an appropriate amount of deionized water and the weighed ammonium rhenate in the doping pot to fully dissolve, and then add the weighed tungsten powder, Through solid-liquid mixing and stirring, and finally drying at a temperature of 120 for 4h;
  • Step 2 reduction: put the material obtained in step 1 in a reduction furnace, and in the four-temperature zone reduction furnace, reduce it into tungsten-rhenium alloy powder at one time, and its key component is: 1.000wt% of rhenium;
  • Step 3 powder mixing: put the materials obtained in step 2 into a powder mixer according to different particle size compositions, and mix powder at a speed of 8 rpm for 80 minutes;
  • Step 4 Powder pressing: the powder in Step 4 is pressed into a compact with a unit weight of 3.0 kg by isostatic pressing under a pressure of 200 MPa, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 5 High-temperature sintering: perform high-temperature sintering on the pre-sintered billet in step 4 to obtain a sintered billet with a density of 18.2 g/cm 3 ;
  • Step 6 Billeting: Using a multi-roll mill at a heating temperature of 1650 degrees, the sintered billet with a diameter of 23mm is continuously rolled into an alloy rod of 8.0mm;
  • Step 7 Pressure processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • the comparative example in this group is to prepare conventional pure tungsten wire.
  • Step 1 Place ammonium paratungstate in a reduction furnace, reduce it to blue tungsten oxide powder in a four-temperature zone reduction furnace, and then reduce it to pure tungsten powder for the second time;
  • Step 2 powder mixing: put the materials obtained in step 1 into a powder mixer according to different particle size compositions, and mix powder at a speed of 8 rpm for 80 minutes;
  • Step 3 powder pressing: the powder in step 2 is pressed into a compact with a unit weight of 3.0 kg and a diameter of 20 mm by isostatic pressing, and the compact is pre-sintered at a low temperature in a hydrogen atmosphere to increase the strength of the compact;
  • Step 4 High-temperature sintering: perform high-temperature sintering on the pre-sintered billet in step 3 to obtain a sintered billet with a density of 17.6 g/cm 3 and a diameter of 17.5 mm;
  • Step 5 Billeting: Using a three-roll mill at a heating temperature of 1600 degrees, the sintered billet with a diameter of 17.5mm is continuously rolled into an alloy rod of 8.0mm;
  • Step 6 press processing: use multi-pass rotary forging. Then, the drawing process is carried out through wire drawing dies of different specifications, and after repeated drawing for many times, alloy wires of different specifications and diameters are made;
  • the annealing treatment is performed on the tungsten wire to eliminate the residual stress caused by plastic deformation, so that the multi-pass drawing process can be smoothly performed.
  • the tungsten powder and sintered billet obtained in Examples 1.1, 2.1 and Comparative Examples 1.1 and 2.1 were evaluated by measuring the La 2 O 3 particle size of the surface of the tungsten powder and the sintered billet by electron microscopy. The test results are shown in Table 1. Show:
  • the processing technology provided by the present invention can effectively refine the La 2 O 3 particle size in the tungsten alloy material
  • Example 1.1 Different specifications of products obtained in Example 1.1, Comparative Examples 1.1-1.3 and Comparative Examples 2.1-2.3: billets, 8.0mm, 5.0mm, 1.0mm, 0.4mm rods and wires, La 2 O 3 particles were measured by electron microscopy The particle size is evaluated, and the test results are shown in Table 2:
  • the alloy billets and wires produced by the processing technology provided by the present invention have a particle size of oxide particles on the surface far smaller than those produced by the processes used in Comparative Examples 1.1-1.3 and 2.1-2.3. Oxide particle size of alloy rods and wires.
  • the tensile strength test method use a standard tensile machine, take a tungsten wire with a length of 200mm to clamp, and load one end at a constant speed to obtain tensile strength data and elastic ultimate strength;
  • the tensile strength is calculated from the following formula (1):
  • the push-pull toughness test method wrap the tungsten wire around a straightened core wire once, and then apply a reverse force (above 8g) to the sample disc, and control the wire-winding disc by the motor to perform high-speed wire-winding.
  • the tungsten wire is wound around the core wire and moves. The smaller the diameter of the core wire, the better the toughness of the tungsten wire through the continuous wire at high speed.
  • the preferred 100 ⁇ m tungsten wire, the reverse force is 50g; the 40 ⁇ m tungsten wire, the reverse force is 12g; the 25 ⁇ m tungsten wire, the reverse force is 8g; Show.
  • the tensile strength and elastic ultimate strength of each specification of the wire produced by the invention are much higher than those of the conventionally produced tungsten wire, and higher than the rhenium-tungsten alloy wire.
  • the comprehensive performance of the tensile strength and push-pull toughness of the tungsten wire prepared by the processing technology provided by the present invention is far superior to that of the rhenium-tungsten alloy wire and the tungsten wire produced by the conventional process.
  • the tensile strength of the tungsten alloy wire prepared in Comparative Example 3 can reach more than 4500 MPa, but its push-pull performance is very poor, indicating that the toughness of the wire is much lower than that of the wire of the present invention. Therefore, the alloy wire prepared by the processing technology provided by the present invention can mass-produce alloy wires with finer specifications, higher strength and better toughness due to the addition of lanthanum oxides and other substances and processes.
  • the solid-liquid doping and multi-roll rolling billeting methods provided by the invention can effectively improve the tensile strength, elastic ultimate strength and push-pull toughness of alloy wires under various specifications, and are more conducive to producing finer specifications and higher strengths. , Alloy wire with better toughness.
  • the solid-solid doping and multi-roll rolling billeting methods provided by the invention can effectively improve the tensile strength, elastic ultimate strength and push-pull toughness of alloy wire rods under various specifications, and are more conducive to the production of finer specifications and higher strengths. , Alloy wire with better toughness.
  • the alloy wire rod provided by the present invention due to the addition of lanthanum oxide and other rare earth elements or rare earth oxides, an alloy wire rod with better performance can be obtained, and with further process optimization, mass production specifications can be realized Thinner, stronger, tougher alloy wire.
  • the alloy wire rod provided by the present invention or the alloy wire rod prepared by the preparation method provided by the present invention can be used in the field of cutting processing used by conventional tungsten wire rods, such as sawing wire, by weaving the wire rod into warp and weft to manufacture metal mesh Wait;
  • the saw wire can be used for cutting various materials, such as silicon wafers, magnetic materials, semiconductor materials and other hard-surface materials, and the semiconductor materials include cutting of sapphire, silicon carbide and other materials, or cooperate with related cutting devices
  • the metal mesh can be used for screen printing, probes for inspection, or wires for catheters, etc.
  • the alloy wire rod can be used as a bus bar, on which particles such as diamond are electroplated or brazed to be used for including silicon wafers, sapphire, silicon carbide, etc.
  • Cutting and processing of hard-surface materials such as third-generation semiconductor materials and magnetic materials;
  • Screen printing is widely used in the manufacture of printed circuit boards, thick film integrated circuits, solar cells, resistors, capacitors, piezoelectric elements, photosensitive elements, thermal elements, liquid crystal display elements, etc.
  • the metal mesh formed by the alloy wire can also be used for screen printing to replace the stainless steel wire, for example, to replace the wire mesh with a small size of 18 ⁇ m or less.
  • the alloy wire rod can be applied to the alloy wire rod in the field of medical/industrial precision instrument cables and ropes Applications such as cables/cords on various mechanical equipment, where such cables provide the highest strength and longest life, such as in minimally invasive surgical instruments or articulating systems, subject to high loads and bending load
  • the steel wire rope is used in the pulling system of the single crystal and polycrystalline silicon furnace.
  • the outer diameter of the steel wire rope used in the single crystal silicon furnace is also increased from 1.8mm to 4.5mm.
  • the traditional process uses steel wire rope, but the steel wire rope cannot be applied to In the magnetic field, the crystal direction of the finished single crystal rod will be non-parallel, and the Fe-rich and high C content of the wire rope will easily cause the main impurities of single crystal silicon to exceed the standard, which will seriously affect the high purity requirements; and with the quality of the single crystal rod.
  • the tension and life requirements of the rope under 1500 °C in the single crystal and polycrystalline silicon furnace are also getting higher and higher.
  • the alloy wire rod provided by the present invention can well meet the technical requirements of high strength, high tensile force, non-magnetic, high temperature resistance, and excellent verticality of the "pulling system" rope, so that it can be used in melting and casting, In the smelting industry such as single crystal furnace, such as high temperature furnace traction rope, etc.;
  • the alloy wire can be used as a material for the fabrication of micro-mechanical wire ropes used in modern surgical robots.
  • the above alloy wires can be used to drive the movements of human arms, elbows and wrists, and the tungsten alloy wires can be used to drive the skeletal muscle movement of the surgeon, instead of the doctor's own body as before, so that the robot can reduce the The burden of the doctor, so that the doctor will not feel tired and tired after performing multiple operations.
  • the alloy wire provided by the present invention can also be applied to technical fields such as textiles, such as cut-resistant protective gloves, protective clothing, etc., and the alloy wire is used for cutting-resistant There are great advantages in safety protection products.
  • the common specifications used to directly weave tungsten filaments and yarns into gloves are 18.5 ⁇ m, 30 ⁇ m and 40 ⁇ m, and the alloy wire provided by the present invention can also be processed to more Fine specification, the smallest can reach 3 ⁇ m, which makes the product have better softness, and is lighter and thinner.
  • the alloy wire rod provided by the present invention can meet the corresponding requirements in terms of diameter, tensile strength and toughness.
  • the above embodiments are only used to illustrate the technical solutions of the present invention, but not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: The technical solutions described in the foregoing embodiments can still be modified, or some or all of the technical features thereof can be equivalently replaced; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present invention. scope.

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Abstract

本发明涉及钨合金材料技术领域，特别涉及一种合金线材及其制备方法与应用，所述合金线材由钨合金制成，所述钨合金包含钨与镧的氧化物，所述合金线材的线径为100μm及以下; 所述合金线材的抗拉强度为3800MPa以上。所述合金线材的线径为60μm及以下: 所述合金线材的推拉芯线直径为350μm以下; 所述合金线材的弹性极限强度为2500MPa以上; 所述合金线材的抗拉强度为4200MPa以上。本发明中，通过镧的氧化物掺杂从而获得具有超高强度且具备良好韧性的合金线材。

Description

一种合金线材及其制备方法与应用 技术领域
本发明涉及钨合金材料技术领域，特别涉及一种合金线材及其制备方法与应用。
背景技术
现已知具有一定较高强度，硬度材料有高碳钢线、钨线等。但现有高碳钢线的抗拉强度一般在4500MPa以下，然而直径却大于50μm，且已达到加工极限，无法往更细的直径进行加工。
此外，钨在小于1毫米的弯曲半径下具有无与伦比的柔性，而不锈钢丝绳在同样的极小弯曲半径下可能会由于多次循环的弯曲应力而失效；相较而言，316不锈钢在2,500–2,550°F温度下就会熔化，而钨在温度达到6,192°F时才会熔化，可见钨对在要求具备良好耐温性和优异抗拉强度的机械丝绳应用中，钨的表现依然出色。
与此同时，凭借使用寿命长和柔性这两大主要优点，钨逐渐成为了制造医用和工业用微型机械丝绳的更具性能优势的材料。由于钨具有强韧、柔性和耐高温性的特质，其制成的钨丝绳坚固耐用，在长时间内无需维护或更换。首先，钨是人类已知的最强韧的材料之一。钻石的莫氏硬度为10，钨的莫氏硬度为9，而相比之下，不锈钢的莫氏硬度约为6。
常规钨丝的抗拉强度一般也在4000MPa以下，然而，其韧性差，生产工艺复杂，加工极其困难，导致难以实现有效的量产。由此，市面上还没有一种具备适用于量产，并且具备4500MPa以上的高强度高韧性的线材，而在高硬度材料-如半导体材料蓝宝石、碳化硅，硅片、磁性材料的切割，高精密器械及高温炉牵引的线缆或绳索等应用中，亟需一种兼具更高强度、韧性与细度的细丝，使得其在该领域的实际应用中满足现实的各种需求。
发明内容
为解决上述背景技术中提及的，现有的高强度钨合金线材在不同尺寸下其性能存在缺陷的问题，本发明提供一种合金线材，所述合金线材由钨合金制成，所述钨合金包含钨与镧的氧化物；所述合金线材的线径为100μm及以下；所述合金线材的抗拉强度为3800MPa以上。
进一步地，所述合金线材的镧的氧化物含量为0.1wt％～2.0wt％。
进一步地，所述合金线材的线径为60μm及以下；所述合金线材的推拉芯线直径为350μm以下；
所述合金线材的弹性极限强度为2500MPa以上；所述合金线材的抗拉强度为4200MPa以上。
进一步地，所述钨合金还包含有金属元素M，所述金属元素M选自钾、铼、钼、铁、钴或稀土金属中的至少一种。
进一步地，所述钾的含量小于80ppm。
进一步地，所述钨合金还包含有除镧的氧化物以外的其他一种或多种稀土氧化物。
本发明提供一种如上所述的合金线材的制备方法，包括掺杂制粉、压制、烧结、开坯；
所述开坯包括采用多辊轧制的方式对烧结坯条开坯，以使轧制后钨杆中镧的氧化物颗粒沿丝材纵向长 度与颗粒横截面粒径比值>5。
进一步地，所述掺杂制粉包括以下步骤：
固液掺杂、还原、制粉；
所述固液掺杂包括对混合后的钨掺杂溶液进行分阶段式烘干，所述分阶段式烘干至少包括2个温度阶段，所述2个温度阶段以100℃为分界线，先在低于100℃下加热烘干，再在100℃以上加热烘干。
进一步地，所述固液掺杂中的分阶段式烘干包括第一烘干阶段和第二烘干阶段，所述第一烘干阶段的温度为60～80℃，所述第二烘干阶段的温度为110～150℃。
进一步地，所述还原包括将固液掺杂后所制得的物料还原成平均费氏粒度为1.0～4.0μm的合金粉。
进一步地，所述掺杂制粉包括以下步骤：
固固掺杂；
所述固固掺杂包括将费氏粒度在1.0μm～4.0μm的钨粉末与粒度分布D90<2.0μm的镧的氧化物为原料，进行混合以获得掺杂镧的氧化物的钨粉。
进一步地，所述烧结坯条的镧的氧化物粒径小于2.5μm。
本发明提供一种合金线材在材料切割领域中的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
进一步地，所述材料至少包括硬面材料；所述硬面材料至少包括硅片、磁性材料、半导体材料；所述半导体材料至少包括蓝宝石、碳化硅。
本发明提供一种合金线材在线缆/绳索方面的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
进一步地，所述线缆/绳索用于医疗/工业精密器械及高温炉牵引。
本发明提供一种合金线材在纺织领域的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
进一步地，包括将所述合金线材通过纺线或编织的方式制成的手套或防护服。
本发明提供的一种合金线材及其制备方法与应用，与现有技术相比，具有以下有益效果：
1、线径在100μm及以下，抗拉强度达到3800MPa以上；
2、所述合金线材的线径为60μm及以下；所述合金线材的推拉芯线直径为350μm以下；所述合金线材的弹性极限强度为2500MPa以上；所述合金线材的抗拉强度为4200MPa以上。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作一简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1为本发明提供的推拉韧性检测的设备结构示意图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明提供一种合金线材，所述合金线材由钨合金制成,所述钨合金包含钨与稀土氧化物；
所述合金线材的线径为400μm及以下；
所述合金线材的抗拉强度为2800MPa以上。
在一些实施例中，所述合金线材的线径为100μm及以下；所述合金线材的抗拉强度为3800MPa以上。
在一些实施例中，所述合金线材的线径为60μm及以下；所述合金线材的推拉芯线直径为350μm以下；
所述合金线材的弹性极限强度为2500MPa以上；所述合金线材的抗拉强度为4200MPa以上。
在一些实施例中，所述合金线材的线径为40μm及以下；所述合金线材的抗拉强度为4800MPa以上。
在一些实施例中，所述合金线材的线径为25μm及以下；所述合金线材的抗拉强度为5000MPa以上。
所述合金线材的拉伸强度可以为2800MPa以上。例如，所述合金线材的拉伸强度也可以为3200MPa以上，也可以在3800MPa以上，还可以在4200MPa甚至4800MPa或5000MPa以上；
另外，合金线材的弹性极限强度可以为2500MPa以上。例如，所述合金线材的弹性极限强度也可以为2700MPa以上，还可以在3000MPa甚至3200MPa以上；
所述合金线材的线径可以为400μm以下。例如，合金线材的线径为400μm、350μm、300μm、250μm、200μm、150μm、100μm、80μm，甚至60μm、40μm、25μm以及20μm和10μm等；所述合金线材可以是均匀的，也可是不完全均匀的，还可以根据部位包含例如1％等几个百分比作用的差。
特别地，所述合金线材的线径可以在60μm及以下，因此合金线材具有柔软性，容易充分地使其弯曲，因此，能够将合金线材容易地卷绕；
由此，所述合金线材的推拉芯线直径可以达到350μm以下。例如230μm、200μm、180μm、160μm、130μm等，可见所述合金线材还具有极好的推拉韧性。
具体而言，所述合金线材的线径在200μm～400μm，所述合金线材的抗拉强度可以为2800MPa～4000MPa，例如抗拉强度可以达到3000MPa，也可以达到3500MPa，甚至达到4000MPa；
所述合金线材的线径可以为100～200μm，所述合金线材的抗拉强度可以为3200～4800MPa，例如抗拉强度达到3400MPa，也可以达到4000MPa，还可以达到4500MPa，甚至达到4800MPa；
在一些实施例中，所述稀土氧化物选自氧化镝、氧化铒、氧化钕、氧化钇、氧化铕、氧化钆、氧化镧、氧化镨、氧化钬、氧化铈、氧化铽、氧化镱、氧化钐、氧化镨钕、氧化铥、氧化镥、氧化钪、氧化钷中的一种或多种。
具体来说，例如，常见的稀土氧化物包括氧化镝(Dy 2O 3)、氧化铒(Er 2O 3)、氧化钕(Nd 2O 3)、氧化钇(Y 2O 3)、氧化铕(Eu 2O 3)、氧化钆(Gd 2O 3)、氧化镧(La 2O 3)、氧化镨(Pr 6O 11)、氧化钬(Ho 2O 3)、 氧化铈(CeO 2)、氧化铽(Tb 4O 7)、氧化镱(Yb 2O 3)、氧化钐(Sm 2O 3)、氧化镨钕((Pr+Nd) xO y)、氧化铥(Tm 2O 3)、氧化镥(Lu 2O 3)、氧化钪(Sc 2O 3)、氧化钷(Pm 2O 3)等，而在实际使用时，可以仅含有氧化镧(La 2O 3)、氧化钇(Y 2O 3)、氧化铈(CeO 2)、氧化钪(Sc 2O 3)等稀土氧化物中的一种，也可以同时含有氧化镧(La 2O 3)以及其他的稀土氧化物,如氧化钪(Sc 2O 3)、氧化钇(Y 2O 3)，又或者含有其他的多种稀土氧化物的组合方式，例如同时含有氧化镧(La 2O 3)和氧化铈(CeO 2)，氧化镧(La 2O 3)和氧化钇(Y 2O 3)，氧化镧(La 2O 3)和氧化钪(Sc 2O 3)，氧化铈(CeO 2)和氧化钇(Y 2O 3)等。
所述稀土氧化物主要分布于钨主相(基体相)晶界处，在基体相晶粒内也有少量分布，稀土氧化物可以呈线条状或颗粒串形态分布。
由稀土氧化物和钨构成的合金线材的线径越小，则拉伸强度相对越强；即，通过利用由稀土氧化物和钨构成的钨合金线材，能够实现线径小、并且拉伸强度高的锯线、线缆等。
此外，所述稀土氧化物还可以为稀土-金属复合氧化物，如YSZ、LSCO等。
不仅如此，所述钨合金还可以包含有微量的碳化物、其他稀有元素亦或者金属、非金属元素，例如所述碳化物包括TiC、ZrC，所述其他稀有元素包括Re等，所述非金属元素包括C等，所述金属元素包括钾、铼、钼、铁、钴等；
其中，K的含量小于80ppm，适量K的添加可以提高材料的高温性能，但是含量过高则会影响加工性能，造成裂纹断丝；
在一些实施例中，所述钨的含量为97.0wt％～99.9wt％，所述稀土氧化物的含量为0.1wt％～3.0wt％。
例如，所述钨的含量也可以是95wt％以上；较佳的，所述钨的含量在97.0wt％～99.9wt％，如97.5wt％、98wt％、98.5wt％、99wt％、99.5wt％等等；
再例如，所述稀土氧化物的含量可以取0.1wt％～3.0wt％，也可以是0.1wt％～2wt％，还或者是0.1wt％～1wt％，再或者是0.3wt％～0.8wt％，当然，也可以取0.1wt％、0.3wt％、0.5wt％、0.8wt％、1wt％、1.5wt％、2wt％等，通过提高稀土氧化物的含量可以使得金属线的性能提升，但是，在其含有率过高的情况下，所述合金线材的细化难度会大大提升。
在一些实施例中，所述钨合金还包含有金属元素，所述金属元素为钾、铼、钼、铁、钴中的至少一种。
在一些实施例中，所述钾的含量小于80ppm。
在一些实施例中，所述钨合金还包含有碳。
本发明提供一种如上所述的合金线材的制备方法，包括掺杂制粉、压制、烧结、开坯，其特征在于，所述开坯包括采用多辊轧制的方式对烧结坯条开坯，以使轧制后钨杆中稀土氧化物颗粒沿丝材纵向长度与颗粒横截面粒径比值>5。
在一些实施例中，所述掺杂制粉包括以下步骤：固液掺杂、还原、制粉；
所述固液掺杂包括对混合后的钨掺杂溶液进行分阶段式烘干，所述分阶段式烘干至少包括2个温度阶段，所述2个温度阶段以100℃为分界线，先在低于100℃下加热烘干，再在100℃以上加热烘干。例如先在60℃～80℃加热烘干2h～6h，再在110℃～150℃下加热烘干3h～5h；
所述分阶段式加热烘干采用先低温再高温的烘干方式，即在低于100℃下进行烘干，使稀土盐颗粒缓慢析出，形核数多，再在高于100℃的温度下烘干，颗粒数较多的稀土盐颗粒来不及合并长大，由此可以大幅细化颗粒粒径；
其中，所述分阶段式烘干至少包括2个温度阶段，所述2个温度阶段以100℃为分界线，先在100℃下加热烘干，再在100℃以上加热烘干；
在一些实施例中，所述固液掺杂中的分阶段式烘干包括第一烘干阶段和第二烘干阶段，所述第一烘干阶段的温度为60～80℃，所述第二烘干阶段的温度为110～150℃。
可以理解的是，在以100℃为分界线划分的该两个温度阶段内，可以分别进行多个温度梯度或多个温度阶段的加热烘干，例如先在60℃下烘干2h，再在80℃下烘干2h，进而升温至120℃进行烘干；当然，以上所述实施例仅表达了本发明的几种实施方式，而对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干温度阶段的调整和改变，这些都属于本发明的保护范围。
在一些实施例中，所述还原包括将固液掺杂后所制得的物料在还原炉中还原成合金粉。
在一些实施例中，所述合金粉的平均费氏粒度为1.0～4.0μm。
在一些实施例中，所述掺杂制粉包括以下步骤：液液掺杂、还原、制粉；
所述液液掺杂包括将钨酸和/或钨酸盐溶液与可溶性稀土盐溶液进行混合。
例如，用偏钨酸铵溶液和稀土盐溶液为原料进行液液掺杂来获得掺杂稀土盐的蓝钨粉；
在一些实施例中，所述掺杂制粉包括以下步骤：固固掺杂；
所述固固掺杂包括将费氏粒度在1.0μm-4.0μm的钨粉末与粒度分布D90<2.0μm的稀土氧化物为原料，进行混合以获得掺杂稀土氧化物的钨粉。
在一些实施例中，为了保证稀土氧化物颗粒尺寸，所述固固掺杂还包括通过水沉淀方法来去除粗颗粒以获得稀土氧化物细颗粒；
基于粗颗粒沉淀快、细颗粒沉淀慢特点，通过沉淀时间30-120分钟的3级沉淀来获得D90<2μm的稀土氧化物；
在一些实施例中，所述稀土氧化物细颗粒的D90＜2μm。
在一些实施例中，所述烧结坯条的稀土氧化物的粒径小于2.5μm。
此外，上述步骤中诸如还原、制粉等步骤，优选但不限于采用以下的实施方式，即：
还原：将固液和/或液液的方式掺杂后所制得的物料在四温区还原炉中把掺杂粉末一次还原成合金粉；
制粉：将还原后所得的合金粉进行混合，混合后组成平均费氏粒度1.0～4.0μm的合金粉置于混粉机。按6～10转/分钟的转速混粉60～90分钟；
粉末压制：采用等静压方式将平均费氏粒度在1.0μm～4.0μm搭配而成的粉末经过160MPa～260MPa压力压制成单重1.5kg～5.0kg的压坯，并在氢气气氛下对压坯进行预烧结，所述预烧结的温度优选为1200-1400℃，增加压坯强度；
烧结：进行烧结，所述烧结的温度优选为1800-2400℃，烧结时间优选为5-15小时，获得密度17.5～18.5g/cm 3的烧结坯条；
开坯：采用多辊轧机在1600～1700℃加热温度下连续轧制把直径15mm～25mm烧结坯条开坯成8.0mm～12.0mm合金杆；
其中，所述多辊轧机的使用，保证轧制后钨杆中稀土氧化物颗粒沿丝材纵向长度与颗粒横截面粒径比值>5；
压力加工：在经由多辊轧机轧制后再采用多道次旋锻，然后通过不同规格拉丝模进行拉拔加工，重 复多次拉拔后制成不同规格直径的合金线材；
接着，可以对制成的合金线材施以在1000℃以内的低温去应力退火工序，从而均匀化其应力分布并提高其直线性；所述工序可以在加热炉内进行亦或者其他装置设备内实施，具体而言，所述合金线材也可以在氢气保护下实施低温去应力退火；
再者，可以对拉拔后的线材进行电解抛光、清洗，使得线材表面变的光滑；所述电解抛光工序例如通过在电解液中浸渍所述合金线材和碳棒等对置电极，向合金线材与对置电极之间通电来进行等。
本发明提供的合金线材在材料切割领域中的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
在一些实施例中，所述材料至少包括硬面材料；所述硬面材料至少包括硅片、磁性材料、半导体材料；所述半导体材料至少包括蓝宝石、碳化硅。
本发明提供的合金线材在线缆/绳索方面的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
在一些实施例中，所述线缆/绳索用于医疗/工业精密器械及高温炉牵引。
本发明提供的合金线材在纺织领域的应用；
其中，所述合金材料采用如上所述的合金线材或者如上所述合金线材的制备方法所制备的合金线材。
在一些实施例中，包括将所述合金线材通过纺线或编织的方式制成的手套或防护服。
下面将结合本发明中的部分实施例，对本发明中的技术方案进行清楚、完整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
作为本发明的一实施例，提供一种合金线材，所述合金线材由钨合金制成，所述钨合金包含钨与镧的氧化物；
其中，所述钨的含量为90wt％以上，所述镧的氧化物含量为0.1wt％以上且2.0wt％以下；
例如，所述钨的含量也可以是95wt％以上；较佳的，所述钨的含量在97.0wt％～99.9wt％，如97.5wt％、98wt％、98.5wt％、99wt％、99.5wt％等等；
再例如，所述镧的氧化物含量可以是0.1wt％～2wt％，还或者是0.1wt％～1wt％，再或者是0.3wt％～0.8wt％，当然，也可以取0.1wt％、0.3wt％、0.5wt％、0.8wt％、1wt％、1.5wt％、2wt％等，所述镧的氧化物优选为氧化镧(La 2O 3)，通过提高镧的氧化物含量可以使得合金线材的性能提升，但是，在镧的氧化物含有率大于2wt％的情况下，所述合金线材的细化难度会大大提升。
在所述合金线材中，所述镧的氧化物主要分布于钨主相(基体相)晶界处，在基体相晶粒内也有少量分布，镧的氧化物可以呈线条状或颗粒串形态分布。
由镧的氧化物和钨构成的合金线材的线径越小，则拉伸强度相对越强；即，通过利用由镧的氧化物和钨构成的钨合金线材，能够实现线径小、并且拉伸强度高的锯线、线缆等。
此外，所述镧的氧化物还可以为镧-金属复合氧化物，如LSCO等。
不仅如此，所述钨合金还可以包含有微量的碳化物、其他稀有元素、金属、非金属元素，例如所述 碳化物包括TiC、ZrC，所述其他稀有元素包括铼等，所述非金属元素包括C等，所述金属元素包括钾、钼、铁、钴等；
其中，钾的含量小于80ppm，适量钾的添加可以提高材料的高温性能，但是含量过高则会影响加工性能，造成裂纹断丝；
作为本发明的另一实施例，提供一种合金线材，所述合金线材由钨合金制成，所述钨合金包含钨与铈的氧化物；
其中，所述钨的含量为90wt％以上，所述铈的氧化物含量为0.1wt％以上且1.5wt％以下；
例如，所述钨的含量也可以是95wt％以上；较佳的，所述钨的含量在97.0wt％～99.9wt％，如97.5wt％、98wt％、98.5wt％、99wt％、99.5wt％等等；
再例如，所述铈的氧化物含量可以是0.2wt％～1.5wt％，还或者是0.2wt％～1wt％，再或者是0.3wt％～0.8wt％，当然，也可以取0.2wt％、0.3wt％、0.5wt％、0.8wt％、1wt％、1.5wt％等，所述铈的氧化物优选为氧化铈(CeO2)，通过提高铈的氧化物含量可以使得合金线材的性能提升，但是，在铈的氧化物含有率大于1.5wt％的情况下，所述合金线材的细化难度会大大提升。
作为本发明的另一实施例，提供一种合金线材，所述合金线材由钨合金制成；所述钨合金包含钨与钇的氧化物；
其中，所述钨的含量为90wt％以上，所述钇的氧化物含量为0.1wt％以上且1.5wt％以下；
例如，所述钨的含量也可以是95wt％以上；较佳的，所述钨的含量在97.0wt％～99.9wt％，如97.5wt％、98wt％、98.5wt％、99wt％、99.5wt％等等；
再例如，所述钇的氧化物含量可以是0.2wt％～1.5wt％，还或者是0.2wt％～1wt％，再或者是0.3wt％～0.8wt％，当然，也可以取0.2wt％、0.3wt％、0.5wt％、0.8wt％、1wt％、1.5wt％等，所述钇的氧化物优选为氧化钇(Y 2O 3)，通过提高钇的氧化物含量可以使得合金线材的性能提升，但是，在钇的氧化物含有率大于1.5wt％的情况下，所述合金线材的细化难度会大大提升。
所述合金线材的拉伸强度为3800MPa以上，还可以在4200MPa甚至4800MPa或5000MPa以上；
另外，合金线材的弹性极限强度为2500MPa以上。例如，所述合金线材的弹性极限强度也可以为2700MPa以上，还可以在3000MPa甚至3200MPa以上；
所述合金线材的线径为100μm以下。例如，合金线材的线径为100μm、80μm，甚至60μm、40μm、25μm以及20μm和10μm等；所述合金线材直径可以是均匀的，也可是不完全均匀的，还可以根据部位包含例如1％等几个百分比作用的差。
特别地，所述合金线材的线径可以在60μm及以下，因此合金线材具有柔软性，容易充分地使其弯曲，因此，能够将合金线材容易地卷绕；
由此，所述合金线材的推拉芯线直径可以达到350μm以下。例如230μm、200μm、180μm、160μm、130μm等，可见所述合金线材还具有极好的推拉韧性。
具体而言，例如，所述合金线材的线径为100μm及以下；所述合金线材的抗拉强度为3800MPa以上；
所述合金线材的线径为60μm及以下；所述合金线材的抗拉强度为4200MPa以上；所述合金线材的弹性极限强度为2500MPa以上，所述合金线材的推拉芯线直径为350μm以下，甚至180μm以下；
所述合金线材的线径为40μm及以下；所述合金线材的抗拉强度为4800MPa以上；所述合金线材的 弹性极限强度为2700MPa以上，所述合金线材的推拉芯线直径为350μm以下，甚至200μm以下；
所述合金线材的线径为25μm及以下；所述合金线材的抗拉强度为5000MPa以上；所述合金线材的弹性极限强度为3000MPa以上，所述合金线材的推拉芯线直径为350μm以下，甚至250μm以下；
本发明提供一种合金线材的制备方法：
所述制备方法的步骤包括有掺杂制粉、压制、烧结、开坯、压力加工等；
掺杂、还原、混粉、
其中，所述掺杂制粉根据不同的工艺方法进行划分包括固液的方式、液液的方式以及固固的方式等；
具体来说，基于固液的方式，所述掺杂制粉包括以下步骤：
固液掺杂、还原、制粉；
所述固液掺杂的方法包括：将适量可溶性镧的盐溶液掺杂进钨粉末中，在充分搅拌后，进行分阶段式加热烘干，即得；
所述分阶段式加热烘干采用先低温再高温的烘干方式，即在低于100℃下进行烘干，使镧的盐颗粒缓慢析出，形核数多，再在高于100℃的温度下烘干，颗粒数较多的镧的盐颗粒来不及合并长大，由此可以大幅细化颗粒粒径；
其中，所述分阶段式烘干至少包括2个温度阶段，所述2个温度阶段以100℃为分界线，先在100℃下加热烘干，再在100℃以上加热烘干；例如先在60℃～80℃加热烘干2h～6h，再在110℃～150℃下加热烘干3h～5h；
可以理解的是，在以100℃为分界线划分的该两个温度阶段内，可以分别进行多个温度梯度或多个温度阶段的加热烘干，例如先在60℃下烘干2h，再在80℃下烘干2h，进而升温至120℃进行烘干；当然，以上所述实施例仅表达了本发明的几种实施方式，而对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干温度阶段的调整和改变，这些都属于本发明的保护范围。
再例如，将适量镧的硝酸盐溶液形式均匀掺杂进蓝钨粉中，在充分搅拌后，先再60℃～80℃下加热2h～6h，再在110℃～150℃下加热3h～5h；
具体来说，基于液液的方式，所述掺杂制粉包括以下步骤：
液液掺杂、还原、制粉；
所述液液掺杂的方法包括：将钨酸和/或钨酸盐溶液与可溶性镧的盐溶液进行掺杂用以后续获得掺杂镧盐的钨粉末；
例如，用偏钨酸铵溶液和镧的盐溶液为原料进行液液掺杂来获得掺杂镧盐的蓝钨粉；
具体来说，基于固固的方式，所述掺杂制粉包括以下步骤：固固掺杂；
所述固固掺杂的方法包括：采用费氏粒度在1.0μm～4.0μm的钨粉末与粒度分布D90<2.0μm的镧的氧化物为原料，进行固固掺杂混合以获得掺杂镧的氧化物钨粉；
进一步地，为了保证镧的氧化物颗粒尺寸，在固固掺杂的步骤中还包括通过水沉淀方法来去除粗颗粒以获得镧的氧化物细颗粒；
基于粗颗粒沉淀快、细颗粒沉淀慢特点，通过沉淀时间30-120分钟的3级沉淀来获得D90<2μm的镧的氧化物；
此外，上述步骤中诸如还原、制粉等步骤，优选但不限于采用以下的实施方式，即：
还原：将固液和/或液液的方式掺杂后所制得的物料在四温区还原炉中把掺杂粉末一次还原成合金 粉；
制粉：将还原后所得的合金粉进行混合，混合后组成平均费氏粒度1.0～4.0μm的合金粉置于混粉机。按6～10转/分钟的转速混粉60～90分钟；
粉末压制：采用等静压方式将平均费氏粒度在1.0μm～4.0μm搭配而成的粉末经过160MPa～260MPa压力压制成单重1.5kg～5.0kg的压坯，并在氢气气氛下对压坯进行预烧结，所述预烧结的温度优选为1200-1400℃，增加压坯强度；
烧结：进行烧结，所述烧结的温度优选为1800-2400℃，烧结时间优选为5-15小时，获得密度17.5～18.5g/cm 3的烧结坯条；
开坯：采用多辊轧机在1600～1700℃加热温度下连续轧制把直径15mm～25mm烧结坯条开坯成8.0mm～12.0mm合金杆；
其中，所述多辊轧机的使用，保证轧制后钨杆中镧的氧化物颗粒沿丝材纵向长度与颗粒横截面粒径比值>5；
压力加工：在经由多辊轧机轧制后再采用多道次旋锻，然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
接着，可以对制成的合金线材施以在1000℃以内的低温去应力退火工序，从而均匀化其应力分布并提高其直线性；所述工序可以在加热炉内进行亦或者其他装置设备内实施，具体而言，所述合金线材也可以在氢气保护下实施低温去应力退火；
再者，可以对拉拔后的线材进行电解抛光、清洗，使得线材表面变的光滑；所述电解抛光工序例如通过在电解液中浸渍所述合金线材和碳棒等对置电极，向合金线材与对置电极之间通电来进行等。
本发明与常规的钨合金线材相比，具有以下特点和优势：
第一、在本发明的掺杂工序中采用固液掺杂时，烘干采用先低温(低于100℃)下进行烘干，再在高温(高于100℃)下烘干的分阶段式烘干模式进行烘干。先使镧的硝酸盐颗粒缓慢析出，形核数多；再使颗粒数很多的镧的硝酸盐颗粒来不及合并长大，通过这种烘干方式可以大幅细化颗粒粒径。通过调整掺杂烘干温度控制镧的硝酸盐成核和析晶速度，使得掺杂蓝钨颗粒上的镧的硝酸盐晶体更加细小。
固固掺杂时，通过水沉淀方法来去除粗颗粒，同时利用粗颗粒沉淀快、细颗粒沉淀慢特点，通过沉淀时间30-120分钟的3级沉淀来获得D90<2μm的镧的氧化物；
由此，本发明生产的钨粉颗粒表面的镧的氧化物粒径和烧结坯条的镧的氧化物粒径都比传统方法要细小，其镧的氧化物粒径小于2.5μm并且分布更均匀，产品性能更稳定；
第二、本发明采用多辊轧制方式进行烧结坯条的开坯，通过对合金材料以大于2.5m/s的速度、大变形量的深度变形加工，传统的钨杆及钨丝旋锻开坯，开坯过程中因旋锻的剧烈径向加工导致镧的弥散颗粒的断裂，迫使弥散粒子的在钨基体空隙中形成空洞，这种加工方式会导致后续的材料应力集中以及缺陷产生，进而导致后续加工困难。本次采用多辊(三辊/四辊)这样会使合金材料在开坯时基体的纤维组织更发达，纵向变形的速率更快，进而带动镧的氧化物弥散颗粒的细化变形更大、颗粒横截尺寸变得更小轴向尺寸更长，从而保证钨基体以及弥散粒子在开坯后具备较好的塑性及韧性，在后续采用连续锻打时弥散粒子可以进一步形成纤维状态强化组织，从而提高钨丝的强度及韧性。
为此，本发明提供如下所示实施例和对比例：
实施例1.1
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例1.2
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为0.15wt％,W为99.85wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例1.3
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1.5wt％,W为98.5wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例1.4
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1.8wt％,W为98.2wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例1.5
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％，K为50ppm，其余为W。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进钾含量50ppm的掺钾钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例1.6
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％，Y 2O 3为0.2wt％，W为98.8wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液、钇的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例1.1
本组比较例是按常规工艺生产的钨合金线材，材料元素组分跟实施例1相同：La 2O 3为1wt％,W为99wt％。
其制备如下步骤：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，蒸汽烘干，温度120℃，烘干时间4小时；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多道次旋锻把直径23mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：再通过多道次旋锻和通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例1.2
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，蒸汽烘干，温度120℃，烘干时间4小时；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例1.3
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多道次旋锻把直径23mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：再通过多道次旋锻和通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例1.4
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为0.07wt％,W为99.93wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例1.5
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为2.2wt％, W为97.8wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量镧的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例2.1
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、固固掺杂：将氧化镧粉末至于水溶液中，搅拌5分钟后将上层溶液倒入至二级水槽中再搅拌5分钟，放置沉淀10分钟后将上层水溶液倒入至三级水槽中再搅拌5分钟，放置沉淀30分钟，将上层溶液倒入4级容器中沉淀24小时后过滤掉溶液加热至100度烘干24h获得D90<2.0μm氧化镧粉末；采用平均粒度在2.0μm的钨粉与经过水沉淀处理后D90<2.0μm的适量氧化镧粉末通过混粉设备进行60分钟均匀化混合；
步骤2、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤3、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤4、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤5、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例2.1
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W 为99wt％。
其制备步骤如下所述：
步骤1、固固掺杂：采用平均粒度在2.0μm的钨粉与适量的氧化镧粉末通过混粉设备进行60分钟均匀化混合；
步骤2、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤3、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤4、开坯：开坯：采用多道次旋锻把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤5、压力加工：再通过多道次旋锻和通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例2.2
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、固固掺杂：采用平均粒度在2.0μm的钨粉与适量的氧化镧粉末通过混粉设备进行60分钟均匀化混合；
步骤2、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤3、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤4、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤5、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例2.3
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：La 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、固固掺杂：将适量氧化镧粉末至于水溶液中，搅拌5分钟后将上层溶液倒入至二级水槽中再搅拌5分钟，放置沉淀10分钟后将上层水溶液倒入至三级水槽中再搅拌5分钟，放置沉淀30分钟，将上层溶液倒入4级容器中沉淀24小时后过滤掉溶液加热至100度烘干24h获得D90<2.0μm氧化镧粉末；采用平均粒度在2.0μm的钨粉与经过水沉淀处理后D90<2.0μm的适量氧化镧粉末通过混粉设备进行60分钟均匀化混合；
步骤2、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤3、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤4、开坯：开坯：采用多道次旋锻把直径23mm烧结坯条开坯成8.0mm合金杆；
步骤5、压力加工：再通过多道次旋锻和通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例3
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：CeO 2为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量铈的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
实施例4
本组实施例是按本发明制备一种高强度高韧性钨合金线材，其材料元素组分为：Y 2O 3为1wt％,W为99wt％。
其制备步骤如下所述：
步骤1、掺杂：将适量钇的硝酸盐溶液均匀掺杂进蓝钨粉中，在充分搅拌后，再先低温80℃烘干4小时再高温烘干120℃的模式进行烘干；
步骤2、还原：将步骤1所得的物料在四温区还原炉中把掺杂粉末一次还原成合适粒度的合金粉；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机。按8转/分钟的转速混粉80分钟；
步骤4、粉末压制：采用等静压方式将不同粒度搭配而成的粉末经过200MPa压力压制成单重 3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：进行高温烧结，获得密度18.10g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650℃加热温度下连续轧制把直径23.0mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例3
本对比例制备一种铼钨合金线材，其材料元素组分为Re为1wt％,W为99wt％。其制备如下步骤：
步骤1、掺杂：按所述重量百分比称取钨粉和铼酸铵，在掺杂锅内加入适量去离子水和称取的铼酸铵进行充分溶解，然后加入称量好的钨粉，通过固液混合搅拌，最后在120温度下烘干4h；
步骤2、还原：将步骤1所得的物料置于还原炉中，在四温区还原炉中，一次还原成钨铼合金粉，其关键组分为：铼1.000wt％；
步骤3、混粉：将步骤2所得的物料按不同粒度组成置于混粉机，按8转/分钟的转速混粉80分钟；
步骤4：粉末压制：采用等静压方式将步骤4的粉末经过200MPa压力压制成单重3.0kg的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤5、高温烧结：将步骤4的预烧结坯条进行高温烧结，获得密度18.2g/cm 3的烧结坯条；
步骤6、开坯：采用多辊轧机在1650度加热温度下连续轧制把直径23mm烧结坯条开坯成8.0mm合金杆；
步骤7、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
对比例4
本组比较例是制备常规纯钨丝。
其制备如下步骤：
步骤1、还原：将仲钨酸铵置于还原炉中，在四温区还原炉中，还原成蓝色氧化钨粉，再经过第二次还原成纯钨粉；
步骤2、混粉：将步骤1所得的物料按不同粒度组成置于混粉机，按8转/分钟的转速混粉80分钟，；
步骤3、粉末压制：采用等静压方式将步骤2的粉末经过160MPa压力压制成单重3.0kg直径20mm的压坯，并在氢气气氛下对压坯进行低温预烧结，增加压坯强度；
步骤4、高温烧结：将步骤3的预烧结坯条进行高温烧结，获得密度17.6g/cm 3直径17.5mm的烧结坯条；
步骤5、开坯：采用三辊轧机在1600度加热温度下连续轧制把直径17.5mm烧结坯条开坯成8.0mm合金杆；
步骤6、压力加工：采用多道次旋锻。然后通过不同规格拉丝模进行拉拔加工，重复多次拉拔后制成不同规格直径的合金线材；
此外，对钨丝实施退火处理，消除其因为塑性变形产生的残余应力，从而能够顺畅地实施多道拉拔加工。
需要说明的是，上述实施例中的具体参数或一些常用试剂，为本发明构思下的具体实施例或优选实施例，而非对其限制；本领域技术人员在本发明构思及保护范围内，可以进行适应性调整。
将实施例1.1、2.1和对比例1.1、2.1获得的钨粉和烧结坯条，通过电子显微镜测量钨粉表面和烧结坯条的La 2O 3颗粒粒径进行评价，其测试结果如表1所示：
表1实施例与对比例的钨粉、坯条的La 2O 3颗粒粒径
  粉末 坯条
实施例1.1 70～150nm 300～1800nm
对比例1.1 100～500nm 1000～5000nm
实施例2.1 200～2000nm 400～2500nm
对比例2.1 200～5000nm 800～6000nm
根据表1的测试结果可知，本发明提供的加工工艺可以有效细化合金钨材中的La 2O 3颗粒粒径；
将实施例1.1与对比例1.1-1.3和对比例2.1-2.3获得的不同规格产品：坯条、8.0mm、5.0mm、1.0mm、0.4mm棒材及线材，通过电子显微镜测量La 2O 3颗粒粒径进行评价，其测试结果如表2所示：
表2实施例和对比例的不同规格产品的La 2O 3颗粒粒径
Figure PCTCN2021114939-appb-000001
根据表1的测试结果可知，采用本发明提供的加工工艺生产的合金坯条及线材，其表面的氧化物颗粒粒径要远远小于对比例1.1-1.3以及对比例2.1-2.3所用工艺生产的合金棒材及线材的氧化物颗粒粒径。
将实施例及对比例获得的不同规格线材：0.1mm、0.06mm、0.04mm、0.025mm，采用下述方法对线材进行抗拉强度、弹性极限强度及推拉韧性测试。
所述抗拉强度测试方法：采用标准拉力机，，取长度200mm的钨丝夹持，一端进行恒速加载，获得抗拉强度数据和弹性极限强度；
所述抗拉强度由以下公式(1)计算获得：
σ＝F/S……(1)
其中，F为拉断力，N；S为原截面积，mm；
所述推拉韧性测试方法：将钨丝绕一根拉直的芯线一圈，然后样品盘施加反向作用力(8g以上)，通过电机控制收丝盘进行高速收丝。钨丝缠绕芯线运动，芯线的直径越小，钨丝高速通过不断丝说明韧性越好。优先100μm钨丝，反向作用力50g；40μm钨丝，反向作用力12g；25μm钨丝，反向作用力8g；所述推拉检测设备如图1所示，其测试评价结果见表3所示。
表3固液掺杂实施例及现有技术对比例性能测试表
Figure PCTCN2021114939-appb-000002
Figure PCTCN2021114939-appb-000003
需要说明的是，表3中，“/”为未进行相关测试；
根据表3的测试结果可见：
本发明生产的线材各规格抗拉强度、弹性极限强度远高于常规生产的钨线材，高于铼钨合金线材。在同等推拉韧性上，采用本发明提供的加工工艺制得的钨线材在抗拉强度和推拉韧性的综合性能远优于铼钨合金线材和常规工艺生产的钨线材。
对比例3制得的钨合金线材在抗拉强度可以达到4500MPa以上，但是其推拉性能很差，表明线材的韧性远低于本发明线材。因此，采用本发明提供的加工工艺制得的合金线材，由于加入镧的氧化物等物质和工艺，能够大批量生产规格更细、强度更高、韧性更好的合金线材。
表4固液掺杂实施例1.1和对比例1.1-1.5性能测试表
Figure PCTCN2021114939-appb-000004
Figure PCTCN2021114939-appb-000005
需要说明的是，表4中，“\”为线材规格无法进一步更细加工。
通过表4的测试结果可见:
本发明所提供的固液掺杂以及多辊轧制的开坯方式能够有效提高合金线材各规格下的抗拉强度、弹性极限强度以及推拉韧性，同时更有利于生产规格更细、强度更高、韧性更好的合金线材。
表5固液掺杂实施例2.1和对比例2.1-2.3性能测试表
Figure PCTCN2021114939-appb-000006
需要说明的是，表5中，“\”为线材规格无法进一步更细加工。
通过表5的测试结果可见:
本发明所提供的固固掺杂以及多辊轧制的开坯方式能够有效提高合金线材各规格下的抗拉强度、弹性极限强度以及推拉韧性，同时更有利于生产规格更细、强度更高、韧性更好的合金线材。
因此，采用本发明提供的合金线材，由于加入镧的氧化物以及其他稀土元素或稀土氧化物等的加入，获得性能更好的合金线材，而在进一步工艺的优化下，能够实现大批量生产规格更细、强度 更高、韧性更好的合金线材。
由此，本发明提供的合金线材或本发明提供的制备方法所制备的合金线材可以用于常规钨线材使用的切割加工领域，例如锯线、通过将线材织造为经线和纬线用以制造金属网等；
其中，所述锯线可以用于多种材料的切割，例如硅片、磁性材料、半导体材料等硬面材料，而所述半导体材料中包括蓝宝石、碳化硅等材料的切割，或者配合相关切削装置用以切断，基于其优异的性能在切割线应用方面，能有效改善其切割质量和切割效率，所述金属网可用于丝网印刷、用于检查用的探头、或导管的导线等；
需要说明的是，本发明提供的合金线材在切割领域实际应用中，所述合金线材可以作为母线，并于其上电镀或钎焊金刚石等颗粒，以用于包括硅片、蓝宝石、碳化硅等第三代半导体材料、磁性材料等硬面材料的切割加工；
基于丝网印刷被广泛地应用于印刷线路板、厚膜集成电路、太阳能电池、电阻、电容、压电元件、光敏元件、热敏元件、液晶显示元件等等的制造中，而本发明提供的合金线材所形成的金属网同样可以用于丝网印刷，用以替代不锈钢丝予以实施，例如替代小规格18μm以下的丝网等。
不仅如此，基于本发明提供的合金线材具有高抗拉强度、弹性极限强度以及推拉韧性、良好的导电性能和机械性能，所述合金线材可以适用于合金线材在医疗/工业精密器械线缆绳索领域中的应用，例如在各种机械设备上的线缆/绳索方面的应用中，此类线缆可提供最高的强度和最长的寿命，诸如在微创手术器械或铰接系统中，承受高负载和弯曲负荷
在单晶、多晶硅炉提拉系统选用钢丝绳，随着单晶、多晶硅炉吊装重量的增加，单晶硅炉上所用的钢丝绳的外径也由1.8mm增大到4.5mm，但是在以钢线切断负荷的30％以下为目标的前提下，为了提高单晶硅纯度和使用寿命，以及将“有磁场”植入单晶、多晶硅炉内，传统工艺中采用的是钢丝绳，但是钢丝绳无法应用于磁场中，会造成成品单晶棒晶体方向不平行，并且钢丝绳的富Fe性和高C含量，容易造成单晶硅主要杂质的超标，严重影响高纯度的要求；且随着单晶棒质量的不断增加，单晶、多晶硅炉内1500℃下绳的拉力和寿命要求也越来越高。
由此，本发明所提供的合金线材能够很好的满足“提拉系统”绳的高强度、高拉力、无磁性、耐高温，优良的垂直度等技术要求，使其得以应用于熔炼铸造、单晶炉等冶炼行业中，例如高温炉牵引绳索等；
同时，凭借其出色的柔韧性和耐磨性以及出色的抗拉强度和抗疲劳性，所述合金线材能够用于现代手术机器人所用微型机械丝绳的制作材料。
此外，可以将上述合金线材来驱动人类手臂、肘部和手腕的运动，由钨合金线材来驱动外科医生的骨骼肌肉运动，而不是像以往一样由医生自己的身体来驱动，这样机器人就可以减轻医生的负担，让医生在施行多台手术后也不会感到疲乏和劳累。
不仅如此，随着丝绳在医疗机器人和医疗器械的应用中承受的负荷越来越大，其结构也不断优化改进，以往常用的1×7、7×7、7×19结构已被更精密复杂的绞合丝绳(例如7×37、19×19和19×37)取代，不仅在前身的基础上提高了抗拉强度，同时也增加了高模量和出色的柔性，可满足现今外科器械更严苛的应用要求，更值得一提的是，制作直径半毫米、19×37结构的丝绳需要采用直径仅0.0005英寸＝12.7μm的细丝，这种细度几乎肉眼不可见。
此外，基于本发明所提供的合金线材具有的轻薄、高强度、高韧性等特性，还能够应用于纺织 等技术领域，例如耐切割防护手套、防护服等，而将该合金线材用于耐切割安全防护用品上有极大的优势，目前现有工艺将钨丝和纱线纺织直接编成手套所使用的常见规格为18.5μm，30μm，40μm，而本发明提供的合金线材还可以加工到更细规格，最细可达3μm，使产品具有更加优异的柔软性，且更加轻薄，在提升防护等级的同时佩戴更加舒适和灵活，适用多种劳动安全保护场合；而高强度细钨丝的强度是不锈钢丝的2倍以上，优良的设计可使防切割等级提高至少2个等级以上，使得其等级评估达到美标的A6-A9和欧标的F级的高防护等级；
而本发明所提供的合金线材无论是直径、抗拉强度还是韧性，均能符合相应的要求。最后应说明的是：以上各实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述各实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分或者全部技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (18)

  1. 一种合金线材，其特征在于：
    所述合金线材由钨合金制成，所述钨合金包含钨与镧的氧化物；
    所述合金线材的线径为100μm及以下；
    所述合金线材的抗拉强度为3800MPa以上。
  2. 根据权利要求1所述的合金线材，其特征在于：所述合金线材的镧的氧化物含量为0.1wt％～2.0wt％。
  3. 根据权利要求1所述的合金线材，其特征在于：
    所述合金线材的线径为60μm及以下；
    所述合金线材的推拉芯线直径为350μm以下；
    所述合金线材的弹性极限强度为2500MPa以上；
    所述合金线材的抗拉强度为4200MPa以上。
  4. 根据权利要求1所述的合金线材，其特征在于：所述钨合金还包含有金属元素M，所述金属元素M选自钾、铼、钼、铁、钴或稀土金属中的至少一种。
  5. 根据权利要求4所述的合金线材，其特征在于：所述钾的含量小于80ppm。
  6. 根据权利要求1所述的合金线材，其特征在于：所述钨合金还包含有除镧的氧化物以外的其他一种或多种稀土氧化物。
  7. 一种如权利要求1-6任一项所述的合金线材的制备方法，包括掺杂制粉、压制、烧结、开坯，其特征在于：
    所述开坯包括采用多辊轧制的方式对烧结坯条开坯，以使轧制后钨杆中镧的氧化物颗粒沿丝材纵向长度与颗粒横截面粒径比值>5。
  8. 根据权利要求7所述的合金线材的制备方法，其特征在于：所述掺杂制粉包括以下步骤：
    固液掺杂、还原、制粉；
    所述固液掺杂包括对混合后的钨掺杂溶液进行分阶段式烘干，所述分阶段式烘干至少包括2个温度阶段，所述2个温度阶段以100℃为分界线，先在低于100℃下加热烘干，再在100℃以上加热烘干。
  9. 根据权利要求8所述的合金线材的制备方法，其特征在于：所述固液掺杂中的分阶段式烘干包括第一烘干阶段和第二烘干阶段，所述第一烘干阶段的温度为60～80℃，所述第二烘干阶段的温度为110～150℃。
  10. 根据权利要求8所述的合金线材的制备方法，其特征在于：所述还原包括将固液掺杂后所制得的物料还原成平均费氏粒度为1.0～4.0μm的合金粉。
  11. 根据权利要求7所述的合金线材的制备方法，其特征在于，所述掺杂制粉包括以下步骤：
    固固掺杂；
    所述固固掺杂包括将费氏粒度在1.0μm～4.0μm的钨粉末与粒度分布D90<2.0μm的镧的氧化物为原料，进行混合以获得掺杂镧的氧化物的钨粉。
  12. 根据权利要求7所述的合金线材的制备方法，其特征在于：所述烧结坯条的镧的氧化物粒径小于2.5μm。
  13. 一种合金线材在材料切割领域中的应用；
    其中，所述合金线材采用如权利要求1-6任一项所述的合金线材或者如权利要求7-12任一项所述合金线材的制备方法所制备的合金线材。
  14. 根据权利要求13所述的应用，其特征在于：所述材料至少包括硬面材料；所述硬面材料至少包括硅片、磁性材料、半导体材料；所述半导体材料至少包括蓝宝石、碳化硅。
  15. 一种合金线材在线缆/绳索方面的应用；
    其中，所述合金线材采用如权利要求1-6任一项所述的合金线材或者如权利要求7-12任一项所述合金线材的制备方法所制备的合金线材。
  16. 根据权利要求15所述的应用，其特征在于：所述线缆/绳索用于医疗/工业精密器械及高温炉牵引。
  17. 一种合金线材在纺织领域的应用；
    其中，所述合金线材采用如权利要求1-6任一项所述的合金线材或者如权利要求7-12任一项所述合金线材的制备方法所制备的合金线材。
  18. 根据权利要求17所述的应用，其特征在于：包括将所述合金线材通过纺线或编织的方式制成的手套或防护服。
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