CN111334679A - Processing method of tungsten-yttrium oxide composite material with excellent thermal stability - Google Patents

Processing method of tungsten-yttrium oxide composite material with excellent thermal stability Download PDF

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CN111334679A
CN111334679A CN202010326372.9A CN202010326372A CN111334679A CN 111334679 A CN111334679 A CN 111334679A CN 202010326372 A CN202010326372 A CN 202010326372A CN 111334679 A CN111334679 A CN 111334679A
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rolling
composite material
tungsten
deformation
composite
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CN111334679B (en
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昝祥
孙海涛
吴玉程
任大雅
王康
罗来马
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Hefei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention discloses a processing method of a tungsten-yttrium oxide composite material with excellent thermal stability, which adopts a wet chemical method to prepare W-Y2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Rolling the composite blank to obtain W-Y2O3A composite material; wherein the rolling is carried out in two steps and a recrystallization annealing is carried out between the two steps of rolling. The invention adds a recrystallization annealing process between multiple rolling, greatly reduces the storage energy existing in the tungsten-yttrium oxide composite material, thereby obviously improving the W-Y2O3Thermal stability of the composite.

Description

Processing method of tungsten-yttrium oxide composite material with excellent thermal stability
Technical Field
The invention relates to a processing method of a tungsten-based composite material, in particular to a processing method of a tungsten-yttrium oxide composite material with excellent thermal stability.
Background
Currently, energy sources available for human beings are mainly non-renewable energy sources, and most of the non-renewable energy sources such as petroleum, natural gas and the like cause serious environmental problems. The nuclear fusion energy is considered as one of important energy sources for solving the problem of human energy in the future due to sufficient fuel and no pollution. When the nuclear fusion reactor works, Plasma Facing Materials (PFM) are subjected to high thermal load, high thermal Plasma flux and high energy neutron irradiation. Therefore, high requirements are put on the performance of the PFM material.
Tungsten has the characteristics of high melting point, good thermal conductivity, low sputtering rate, low tritium retention and the like, and is considered as the most promising plasma-oriented material. However, tungsten has the problems of low-temperature brittleness, irradiation brittleness, low recrystallization temperature and the like, and recrystallization embrittlement can occur under the high-temperature service condition, so that the performance of the material is degraded. The addition of the oxide to the tungsten matrix can improve the high-temperature stability of tungsten by hindering dislocation motion and inhibiting grain growth. In addition, the rolling process is a main processing mode of the tungsten-based material, and the strength of the material can be improved and the ductile-brittle transition temperature can be reduced by rolling the tungsten-based alloy. At present, the tungsten-yttrium oxide composite material with large deformation needs to be processed by warm rolling for many times. However, after the deformation is strengthened, a large amount of stored energy exists in the material, and thus the thermal stability of the material is reduced.
Disclosure of Invention
Based on the problems of the prior art, the present invention is directed to a method for processing a tungsten-yttria composite material having excellent thermal stability. The invention is suitable for large deformation W-Y2O3Rolling of composite materialsDuring the process, a recrystallization annealing process is added between multiple times of rolling, so that the stored energy in the tungsten-yttrium oxide composite material can be greatly reduced, and the prepared W-Y2O3The composite material has excellent thermal stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a processing method of a tungsten-yttrium oxide composite material with excellent thermal stability, which adopts a wet chemical method to prepare W-Y2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Rolling the composite blank to obtain W-Y2O3A composite material; the rolling is carried out in two steps, and recrystallization annealing is carried out between the two steps of rolling. The method specifically comprises the following steps:
step 1, preparing W-Y by adopting a wet chemical method2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Compounding blanks;
step 2, for the W-Y2O3Rolling the composite blank with deformation of 45-50% to obtain a rolled plate after initial rolling;
step 3, carrying out recrystallization annealing on the initially rolled plate to obtain a recrystallized rolled plate;
step 4, taking out the recrystallized rolled plate, immediately rolling again to obtain the W-Y alloy steel sheet2O3The final deformation of the composite blank is 62-67% of the rolled plate, namely the required W-Y2O3A composite material.
Preferably, the specific method of step 1 is:
step 11, ammonium paratungstate (APT, Aladdin, purity is more than or equal to 99.95%) and yttrium nitrate (Y (NO)3)3·6H2O, Aladdin with the purity of more than or equal to 99.5%) is dissolved in deionized water to obtain a mixed solution; the precipitant oxalic acid (analytically pure, C)2H2O4·2H2O) is added into the mixed solution and is continuously stirred at the temperature of 180 ℃ and 200 ℃ until W-Y is obtained2O3Drying and grinding the precursor to obtain W-Y2O3Precursor powder; subjecting the obtained W-Y2O3Putting the precursor powder into a tube furnace, and reducing the precursor powder in a hydrogen atmosphere to obtain W-Y2O3Composite powder;
wherein: ammonium paratungstate and yttrium nitrate in a ratio of Y2O3The volume fraction of (A) is 2-3%; the mass ratio of ammonium paratungstate to precipitator oxalic acid is 4: 1; h in the hydrogen atmosphere2The content is more than or equal to 99.999 percent, the reduction temperature is 780-820 ℃, and the reduction time is 2-3 hours; W-Y obtained after reduction2O3The particle size of the composite powder is 0.5-3 μm.
Step 12, mixing the W-Y2O3Pressing the composite powder under 500-600MPa to obtain a pressed compact, then placing the pressed compact in a medium-frequency induction heating furnace, and heating in a H furnace2Sintering at 1900-2100 ℃ for 120 min under protection to obtain W-Y2O3And (5) compounding blanks.
Preferably, the rolling start temperature in step 2 is 1580-. The grain size of the rolled plate with the deformation of 62-67% obtained in step 4 is larger than that of the rolled plate with the deformation of 45-50% obtained in step 2, but has similar defect density.
W-Y obtained by the invention2O3The volume percentage of tungsten in the composite material is 97-98%, and the balance is yttrium oxide.
Compared with the prior art, the invention has the beneficial effects that:
the invention is suitable for large deformation W-Y2O3When the composite material is rolled, a recrystallization annealing process is added between multiple times of rolling, so that the storage energy existing in the tungsten-yttrium oxide composite material is greatly reduced, and the prepared W-Y2O3The composite material has excellent thermal stability. W-Y prepared by the invention2O3The relative density of the composite material reaches more than 99.0 percent, and the Vickers hardness of the RD-ND surface is HV10Is 430, and the composite material is annealed for 408 hours at 1300 ℃ in a high-temperature performance test,Annealing at 1350 ℃ for 268h, still keeping the recovery state, and the thermal stability is obviously superior to that of the existing W-Y2O3The composite material meets the performance requirements of a plasma-oriented material.
Drawings
FIGS. 1(a) and (b) are W-Y showing 50% strain obtained in step 2 of example 1 of the present invention2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3Gold phase diagram of the composite.
FIGS. 2(a) and (b) are W-Y showing 50% strain obtained in step 2 of example 1 of the present invention2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3EBSD grain boundary map of the composite.
FIGS. 3(a) and (b) are W-Y showing 50% strain obtained in step 2 of example 1 of the present invention2O3Annealing the composite material at 1300 ℃ for 42h and obtaining the W-Y with the deformation of 67 percent in the step 42O3The composite material is annealed at 1300 ℃ for 408 h.
FIG. 4 is a graph showing W-Y values of 50% strain obtained in step 2 of example 1 of the present invention2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3Time histogram of recovery and recrystallization during isothermal annealing of composite materials.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Step 1, preparing W-Y by adopting a wet chemical method2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Compounding blanks:
step 11, ammonium paratungstate (APT, Aladdin, purity is more than or equal to 99.95%) and yttrium nitrate (Y (NO)3)3·6H2O, Aladdin, the purity is more than or equal to 99.5 percent) as raw materials, the proportion of ammonium paratungstate and yttrium nitrate and the proportion of Y2O3Is 3% by volume.
Dissolving ammonium paratungstate and yttrium nitrate in deionized water to obtain a transparent mixed solution; adding precipitator oxalic acid (the mass ratio of ammonium paratungstate to oxalic acid is 4:1) into the mixed solution, and continuously stirring the mixed solution under 180 ℃ oil bath until obtaining W-Y2O3Drying and grinding the precursor to obtain W-Y2O3Precursor powder; subjecting the obtained W-Y2O3The precursor powder was placed in a tube furnace under hydrogen atmosphere (H)2Content of more than or equal to 99.999%) at 780 ℃ for 3h to obtain W-Y with particle size of 0.5 mu m2O3Composite powder;
step 12, mixing W-Y2O3Pressing the composite powder under 500MPa to obtain a pressed compact, then placing the pressed compact in a medium-frequency induction heating furnace, and heating in a furnace at H2Sintering at 1900 deg.C for 120 min under protection to obtain W-Y2O3And (5) compounding blanks.
Step 2, for W-Y2O3And rolling the composite blank at the initial rolling temperature of 1580 ℃, and performing rolling deformation for multiple times to obtain a rolled plate with the deformation of 50%, namely the plate rolled after the initial rolling.
Step 3, carrying out recrystallization annealing on the initially rolled plate, wherein the temperature of the recrystallization annealing is 1500 ℃, and the time is 30min, so as to obtain a recrystallized rolled plate;
step 4, taking out the recrystallized rolled plate, immediately rolling again to obtain the W-Y steel sheet2O3The final deformation of the composite blank is 67 percent of a rolled plate, namely the required W-Y2O3A composite material.
FIGS. 1(a) and (b) are W-Y showing 50% strain obtained in step 2 of this example2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3The gold phase diagram of the composite material can be seen: after rolling, crystal grains are elongated along the rolling direction and are in a slender fiber shape; W-Y with a deformation of 67%2O3W-Y with grain size greater than 50% of deformation2O3Grain size.
FIGS. 2(a) and (b) are graphs showing the 50% deformation obtained in step 2 of this exampleW-Y2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3According to the EBSD grain boundary diagram of the composite material, a large number of low-angle grain boundaries exist inside the rolled grains.
FIGS. 3(a) and (b) are W-Y showing 50% strain obtained in step 2 of this example2O3Annealing the composite material at 1300 ℃ for 42h and obtaining the W-Y with the deformation of 67 percent in the step 42O3The gold phase diagram of the composite material annealed at 1300 ℃ for 408h can be seen: W-Y with 50% deformation2O3After the composite material is annealed at 1300 ℃ for 42h, all the crystal grains are isometric recrystallized grains; and a deformation of 67% W-Y2O3After the composite material is annealed for 408h at 1300 ℃, the crystal grains are still slender deformed crystal grains.
FIG. 4 shows W-Y with a strain of 50% obtained in step 2 of this example2O3The composite material and the W-Y with the deformation of 67 percent obtained in the step 42O3The time histogram of the recovery and recrystallization during isothermal annealing of the composite can be seen: W-Y with 50% deformation in the long-term isothermal annealing at 1300 ℃ and 1350 ℃2O3The composite material had completely recrystallized in a short time and had a deformation of 67% W-Y2O3The composite is still in the recovery phase. W-Y with a deformation of 67%2O3The composite material is completely recrystallized only after being isothermally annealed at 1400 ℃ for 100 h.
W-Y prepared in this example2O3The relative density of the composite material reaches more than 99.0 percent, and the deformation of the composite material is 67 percent2O3The composite material has a Vickers hardness of RD-ND surface of HV10Is 430. W-Y with 67% deformation in high temperature performance test2O3The composite material still maintains the recovery state after annealing for 408h at 1300 ℃ and 268h at 1350 ℃.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (4)

1. A processing method of a tungsten-yttrium oxide composite material with excellent thermal stability is characterized in that: preparing W-Y by wet chemical method2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Rolling the composite blank to obtain W-Y2O3A composite material;
the rolling is carried out in two steps, and recrystallization annealing is carried out between the two steps of rolling.
2. The process according to claim 1, characterized in that it comprises the following steps:
step 1, preparing W-Y by adopting a wet chemical method2O3Compounding the powder, pressing and sintering to obtain W-Y2O3Compounding blanks;
step 2, for the W-Y2O3Rolling the composite blank with deformation of 45-50% to obtain a rolled plate after initial rolling;
step 3, carrying out recrystallization annealing on the initially rolled plate to obtain a recrystallized rolled plate;
step 4, taking out the recrystallized rolled plate, immediately rolling again to obtain the W-Y alloy steel sheet2O3The final deformation of the composite blank is 62-67% of the rolled plate, namely the required W-Y2O3A composite material.
3. The processing method according to claim 2, characterized in that: the initial rolling temperature of the rolling in the step 2 is 1580-1620 ℃; the temperature of the recrystallization annealing in the step 3 is 1500-1520 ℃ and the time is 30-40 min; and 4, the initial rolling temperature of the rolling in the step 4 is the temperature of the recrystallization annealing.
4. The processing method according to claim 1 or 2, characterized in that: obtaining W-Y2O3The volume percentage of tungsten in the composite material is 97-98%, and the balance is yttrium oxide.
CN202010326372.9A 2020-04-23 2020-04-23 Processing method of tungsten-yttrium oxide composite material with excellent thermal stability Active CN111334679B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111975005A (en) * 2020-08-26 2020-11-24 合肥工业大学 Tungsten-copper pipe penetrating component integrally formed by utilizing spark plasma sintering technology

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US20040238599A1 (en) * 2003-05-30 2004-12-02 General Electric Company Apparatus and method for friction stir welding of high strength materials, and articles made therefrom
EP1594645A2 (en) * 2003-01-31 2005-11-16 H.C. Starck Inc. Refractory metal annealing bands
CN107227423A (en) * 2017-06-12 2017-10-03 合肥工业大学 A kind of tungsten Yttria Composite with excellent high temperature mechanical property and preparation method thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
EP1594645A2 (en) * 2003-01-31 2005-11-16 H.C. Starck Inc. Refractory metal annealing bands
US20040238599A1 (en) * 2003-05-30 2004-12-02 General Electric Company Apparatus and method for friction stir welding of high strength materials, and articles made therefrom
CN107227423A (en) * 2017-06-12 2017-10-03 合肥工业大学 A kind of tungsten Yttria Composite with excellent high temperature mechanical property and preparation method thereof

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Title
谢卓明: "碳化物/氧化物弥散强化钨基合金的制备及性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111975005A (en) * 2020-08-26 2020-11-24 合肥工业大学 Tungsten-copper pipe penetrating component integrally formed by utilizing spark plasma sintering technology

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