AU2020100589A4 - Method for preparing reinforced tungsten matrix composite compounding trace elements and rare earth oxide - Google Patents
Method for preparing reinforced tungsten matrix composite compounding trace elements and rare earth oxide Download PDFInfo
- Publication number
- AU2020100589A4 AU2020100589A4 AU2020100589A AU2020100589A AU2020100589A4 AU 2020100589 A4 AU2020100589 A4 AU 2020100589A4 AU 2020100589 A AU2020100589 A AU 2020100589A AU 2020100589 A AU2020100589 A AU 2020100589A AU 2020100589 A4 AU2020100589 A4 AU 2020100589A4
- Authority
- AU
- Australia
- Prior art keywords
- temperature
- composite
- precursor
- raised
- sintering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 24
- 239000010937 tungsten Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000011159 matrix material Substances 0.000 title claims abstract description 17
- 238000013329 compounding Methods 0.000 title claims abstract description 10
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 10
- 235000013619 trace mineral Nutrition 0.000 title claims abstract description 10
- 239000011573 trace mineral Substances 0.000 title claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 23
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 16
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000011946 reduction process Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000004927 fusion Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910009253 Y(NO3)3 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 2
- LBVWQMVSUSYKGQ-UHFFFAOYSA-J zirconium(4+) tetranitrite Chemical compound [Zr+4].[O-]N=O.[O-]N=O.[O-]N=O.[O-]N=O LBVWQMVSUSYKGQ-UHFFFAOYSA-J 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
Classifications
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—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
- 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
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
Abstract
METHOD FOR PREPARING REINFORCED TUNGSTEN MATRIX COMPOSITE COMPOUNDING TRACE ELEMENTS AND RARE EARTH OXIDE The present invention discloses a method for preparing a reinforced tungsten matrix composite compounding trace elements and rare earth oxide, and a W-Zr-Y203 composite is prepared by using a wet chemical method. When a W-Zr-Y 203 composite precursor is prepared, Zr element and ceramic phase Y203 can be added to make a second phase in the reduced W-Zr-Y203 composite powder become smaller. The density of the composite of the present invention reaches 98% or more, and the grain size is 1.5-2.5 tm, so that the hardness of the W-Zr-Y 203 composite reaches 490-530 HV. 2 , which is better than that of a pure tungsten material (with a grain size of about 15 m and a hardness of 340 HV.2). pm EH~ &O~kVDate.30 Aug 2019 WD =10.2 mm Mag= 10,00 KX Time:16:48:12
Description
METHOD FOR PREPARING REINFORCED TUNGSTEN MATRIX COMPOSITE COMPOUNDING TRACE ELEMENTS AND RARE EARTH OXIDE
TECHNICAL FIELD
F0001I .The present invention relates to a method for preparing a tungsten matrix composite, and in particular, to a method for preparing a reinforced tungsten matrix composite compounding trace elements and rare earth oxide.
BACKGROUND [0002] Fusion energy is one of the world’s most important energy sources. It could be a solution to the energy problems in human society at present. The Tokamak, a magnetic confinement fusion device developed through international efforts, makes fusion energy possible, but there are still some problems in actual operation. During the production and use of plasma, high thermal load is generated. Ion flux and neutron load act on plasma facing materials (PFMs), so it is useful to seek to improve the performance of the PFMs.
[0003] Tungsten is considered to be the most promising PFM at present with its high melting point, high thermal conductivity, strong sputtering resistance and other desirable characteristics. However, tungsten is still troubled by its brittleness such as low-temperature brittleness and recrystallization brittleness, mainly because impurities such as O and N are at grain boundaries, which reduces the cohesion of the grain boundaries.
[00041 .It has been found that mechanical properties of a tungsten matrix composite can be effectively improved by alloying and dispersion strengthening. For example, a small amount of active elements (such as Zr) may be added to a tungsten matrix to combine with impurities to form a compound so as to realize microalloying; the added oxides (such as Y2O3) can refine crystal grains, and a second phase disperses in the tungsten matrix, thus strengthening the material. However, the composite powder prepared by a conventional mechanical alloying method is easily doped with impurities and has certain influence on the properties of the composite obtained by subsequent sintering.
2020100589 17 Apr 2020
SUMMARY [00051 .In accordance with one aspect of the present invention, there is provided a method for preparing a reinforced tungsten matrix composite compounding trace elements and rare earth oxide, and a W-Zr-Y2O3 composite is prepared by using a wet chemical method. When a W-Zr-Y2O3 composite precursor is prepared, Zr element and ceramic phase Y2O3 can be added to make a second phase in the reduced W-Zr-Y2<D3 composite powder become smaller and evenly distributed, which lays a foundation for obtaining the highhardness W-Zr-Y2O3 composite by subsequent sintering.
[00061 In embodiments, the method further includes the following steps:
Step 1: preparation of a precursor first dissolving yttrium nitrate (Y(NO3)3 6H2O, Aladdin, with a purity greater than or equal to 99.5%), zirconium nitrate (Zr(NO3)4 5H2O, Aladdin) and triethanolamine (Ci6H22N4O3 with a purity greater than or equal to 99%) in deionized water to prepare a solution; then adding an ammonium metatungstate (AMT, Aladdin, with a purity greater than or equal to 99.95%) solution dissolved in deionized water, and fully stirring to obtain a mixed solution; finally adding oxalic acid (C2H2CU 2H2O, analytically pure) into the mixed solution, and heating and stirring until the solution is completely evaporated, the obtained precipitate being the precursor;
in step 1, the dosages of the yttrium nitrate, the zirconium nitrate, the triethanolamine and the oxalic acid are 0.5-0.7%, 0.2-0.4%, 6% and 38.9% of the weight of the ammonium metatungstate respectively.
[00071 Step 2: reduction fully grinding the precursor obtained in step 1 in a mortar, and then putting the precursor into a tube furnace for two-step reduction under hydrogen atmosphere, where in the reduction process, the purity of hydrogen is greater than or equal to 99.999%, the temperature is first raised to 545-665°C and kept for 55-75 min; and then the temperature is raised to 750-850°C and kept for 115-135 min.
[00081 Step 3: sintering placing the reduced W-Zr-Y2O3 composite powder obtained in step 2 into a graphite die, and then putting the graphite die into a discharge plasma sintering furnace for sintering. The
2020100589 17 Apr 2020 sintering process is divided into three steps: first the temperature is raised to 795-835°C and kept for 4-6 min, then the temperature is raised to 1275-1325°C and kept for 18-22 min, and finally the temperature is raised to 1775-1825°C and kept for 1-3 min. Then, the die is cooled to room temperature with the furnace, and then the \V-Zr-Y2O3 composite is obtained.
100091 .The W-Zr-Y2O3 composite prepared by the wet chemical method in the present invention has smaller grain sizes, and the second phase is uniform in the tungsten matrix composite without obvious agglomeration, which obviously improves the hardness of the WZr-Y2O3 composite.
100101 Embodiments of the present invention have the following beneficial effects:
The W-Zr-Y2O3 composite is prepared by the wet chemical method in the present invention, so that ZH+ and Y3+ are uniformly dispersed in a tungsten compound. In the W-ZrY2O3 composite obtained by subsequent sintering, carbides or oxides formed by Zr and impurities such as C and O are distributed at grain boundaries, and Y2O3 is uniformly distributed in the tungsten matrix composite. The density of the composite reaches 98% or above, and the grain size is 1.5-2.5 pm. As a result, the hardness of the \V-Zr-Y2O3 composite reaches 490-530 HV0.2, which is better than that of a pure tungsten material (with a grain size of about 15 pm and a hardness of 340 HV0.2).
BRIEF DESCRIPTION OF THE DRAWINGS room .FIG. 1 is a scanning diagram of \V-Zr-Y2O3 composite powder, according to which it can be seen that the particle size of the powder is small, the large particle size is about 200 nm, and the small particle size is below 50 nm; and
100121 FIG. 2 is a fracture morphology diagram of a W-Zr-Y2O3 composite, where it can be seen from the figure that there are almost no holes in the composite with a size of about 1.5 pm, and there are many pits on the fracture surface, indicating that the second phase with a smaller size is uniformly distributed in a tungsten matrix.
DETAILED DESCRIPTION
Example 1
100131 _A method for preparing a reinforced tungsten matrix composite compounding
2020100589 17 Apr 2020 trace elements and rare earth oxide in this example includes the following steps.
Step 1: Preparation of a precursor [00141 First dissolve yttrium nitrate (Y(NO3)s 6H2O, Aladdin, with a purity greater than or equal to 99.5%), zirconium nitrate (Zr(NOs)4 5H2O, Aladdin) and triethanolamine (C16H22N4O3 with a purity greater than or equal to 99%) in deionized water to prepare a solution; then add an ammonium metatungstate (AMT, Aladdin, with a purity greater than or equal to 99.95%) solution dissolved in deionized water, and fully stir to obtain a mixed solution; finally add oxalic acid (C2H2O4 2H2O, analytically pure) into the mixed solution, and heat and stir until the solution is completely evaporated, and the obtained precipitate is the precursor, where the dosages of the yttrium nitrate, the zirconium nitrate, the triethanolamine and the oxalic acid are 0.5%, 0.2%, 6% and 38.9% of the weight of the ammonium metatungstate respectively.
Step 2: Reduction [00151 Fully grind the precursor obtained in step 1 in a mortar, and then put the precursor into a tube furnace for two-step reduction under hydrogen atmosphere, where in the reduction process, the purity of hydrogen is greater than or equal to 99.999%, the temperature is first raised to 545°C and kept for 75 min; and then the temperature is raised to 750°C and kept for 115 min.
Step 3: Sintering [00161 Place the reduced \V-Zr-Y2O3 composite powder obtained in step 2 into a graphite die, and then put the graphite die into a discharge plasma sintering furnace for sintering. The sintering process is divided into three steps: first the temperature is raised to 795°C and kept for 4 min, then the temperature is raised to 1275°C and kept for 18 min, and finally the temperature is raised to 1775°C and kept for 1 min. Then, cool the die to room temperature with the furnace, and then obtain the \V-Zr-Y2O3 composite. The grain size of the composite was 1.5 pm and the hardness was 49OHVo.2, which were better than those of a pure tungsten material (with a grain size of about 15 pm and a hardness of 340 HV0.2).
Example 2 [00171 _A method for preparing a reinforced tungsten matrix composite compounding
2020100589 17 Apr 2020 trace elements and rare earth oxide in this example includes the following steps.
Step 1: Preparation of a precursor [00181 First dissolve yttrium nitrate (Y(NO3)3 6H2O, Aladdin, with a purity greater than or equal to 99.5%), zirconium nitrate (Zr(NO3)4 5Η3Ο, Aladdin) and triethanolamine (Ci6H22N4O3 with a purity greater than or equal to 99%) in deionized water to prepare a solution; then add an ammonium metatungstate (AMT, Aladdin, with a purity greater than or equal to 99.95%) solution dissolved in deionized water, and fully stir to obtain a mixed solution; finally add oxalic acid (C2H2O4 2H2O, analytically pure) into the mixed solution, and heat and stir until the solution is completely evaporated, and the obtained precipitate is the precursor, where the dosages of the yttrium nitrate, the zirconium nitrate, the triethanolamine and the oxalic acid are 0.6%, 0.3%, 6% and 38.9% of the weight of the ammonium metatungstate respectively.
Step 2: Reduction [00191 Fully grind the precursor obtained in step 1 in a mortar, and then put the precursor into a tube furnace for two-step reduction under hydrogen atmosphere, where in the reduction process, the purity of hydrogen is greater than or equal to 99.999%, the temperature is first raised to 605°C and kept for 65 min; and then the temperature is raised to 800°C and kept for 125 min.
Step 3: Sintering [00201 Place the reduced W-Zr-Y2O3 composite powder obtained in step 2 into a graphite die, and then put the graphite die into a discharge plasma sintering furnace for sintering. The sintering process is divided into three steps: first the temperature is raised to 815°C and kept for 5 min, then the temperature is raised to 1300°C and kept for 20 min, and finally the temperature is raised to 1800°C and kept for 2 min. Then, cool the die to room temperature with the furnace, and then obtain the W-Zr-Y2O3 composite. The grain size of the composite was 2 pm and the hardness was 510 HV0.2, which were better than those of a pure tungsten material (with a grain size of about 15 pm and a hardness of 340 HV0.2).
Example 3 [00211 _A method for preparing a reinforced tungsten matrix composite compounding
2020100589 17 Apr 2020 trace elements and rare earth oxide in this example includes the following steps.
Step 1: Preparation of a precursor [0022] First dissolve yttrium nitrate (Y(NC>3)3 6H2O, Aladdin, with a purity greater than or equal to 99.5%), zirconium nitrate (Zr(NC>3)4 5H2O, Aladdin) and triethanolamine (C16H22N4O3 with a purity greater than or equal to 99%) in deionized water to prepare a solution; then add an ammonium metatungstate (AMT, Aladdin, with a purity greater than or equal to 99.95%) solution dissolved in deionized water, and fully stir to obtain a mixed solution; finally add oxalic acid (C2H2O4 2H2O, analytically pure) into the mixed solution, and heat and stir until the solution is completely evaporated, and the obtained precipitate is the precursor, where the dosages of the yttrium nitrate, the zirconium nitrate, the triethanolamine and the oxalic acid are 0.7%, 0.4%, 6% and 38.9% of the weight of the ammonium metatungstate respectively.
Step 2: Reduction [00231 Fully grind the precursor obtained in step 1 in a mortar, and then put the precursor into a tube furnace for two-step reduction under hydrogen atmosphere, where in the reduction process, the purity of hydrogen is greater than or equal to 99.999%, the temperature is first raised to 665°C and kept for 55 min; and then the temperature is raised to 850°C and kept for 135 min.
Step 3: Sintering [0024] Place the reduced \V-Zr-Y2O3 composite powder obtained in step 2 into a graphite die, and then put the graphite die into a discharge plasma sintering furnace for sintering. The sintering process is divided into three steps: first the temperature is raised to 835°C and kept for 6 min, then the temperature is raised to 1325°C and kept for 22 min, and finally the temperature is raised to 1825°C and kept for 3 min. Then, cool the die to room temperature with the furnace, and then obtain the \V-Zr-Y2O3 composite. The grain size of the composite was 2.5 pm and the hardness was 530 HV0.2, which were better than those of a pure tungsten material (with a grain size of about 15 pm and a hardness of 340 HV0.2).
Claims (4)
- The claims defining the present invention are as follows^1. A method for preparing a reinforced tungsten matrix composite compounding trace elements and rare earth oxide, comprising the following steps:step 1: preparation of a precursor first dissolving yttrium nitrate, zirconium nitrate and triethanolamine in deionized water to prepare a solution; then adding an ammonium metatungstate solution dissolved in deionized water, and substantially fully stirring to obtain a mixed solution; finally adding oxalic acid into the mixed solution, and heating and stirring until the solution is completely evaporated, the obtained precipitate being the precursor;step 2: reduction substantially fully grinding the precursor obtained in step 1 in a mortar, and then putting the precursor into a tube furnace for two-step reduction under hydrogen atmosphere; and step 3: sintering placing the reduced \V-Zr-Y2O3 composite powder obtained in step 2 into a graphite die, then putting the graphite die into a discharge plasma sintering furnace for sintering; cooling the die to room temperature with the furnace, and then obtaining the \V-Zr-Y2O3 composite.
- 2. The preparation method according to claim 1, wherein in step 1, the dosages of the yttrium nitrate, the zirconium nitrate, the triethanolamine and the oxalic acid are 0.5-0.7%, 0.2-0.4%, 6% and 38.9% of the weight of the ammonium metatungstate respectively.
- 3. The preparation method according to claim 1 or 2, wherein in step 2, the two-step reduction comprises first raising the temperature to 545-665°C, and maintaining that temperature for 55-75 min; then raising the temperature to 750-850°C, and maintaining that temperature for 115-135 min, wherein in the reduction process, the purity of hydrogen is greater than or equal to 99.999%.
- 4. The preparation method according to any one of claims 1 to 3, wherein2020100589 17 Apr 2020 in step 3, the sintering process is divided into three steps: first the temperature is raised to 795-835°C and kept for 4-6 min, then the temperature is raised to 1275-1325°C and maintained for 18-22 min, and finally the temperature is raised to 1775-1825°C and maintained for 1-3 min.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910846229.X | 2019-09-09 | ||
| CN201910846229.XA CN110512107B (en) | 2019-09-09 | 2019-09-09 | Preparation method of trace element and rare earth oxide composite reinforced tungsten-based composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2020100589A4 true AU2020100589A4 (en) | 2020-05-28 |
Family
ID=68630398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2020100589A Active AU2020100589A4 (en) | 2019-09-09 | 2020-04-17 | Method for preparing reinforced tungsten matrix composite compounding trace elements and rare earth oxide |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN110512107B (en) |
| AU (1) | AU2020100589A4 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990374A (en) * | 2022-06-08 | 2022-09-02 | 合肥工业大学 | Rare earth oxide particle reinforced tungsten-vanadium solid solution alloy and preparation method thereof |
| CN114985752A (en) * | 2022-04-27 | 2022-09-02 | 北京工业大学 | Method for preparing tungsten alloy composite powder |
| CN115055693A (en) * | 2022-06-24 | 2022-09-16 | 合肥工业大学 | Single-phase tungsten-rhenium alloy powder and preparation method thereof |
| CN115608999A (en) * | 2022-10-17 | 2023-01-17 | 合肥工业大学 | W-Y 2 O 3 -HfO 2 Composite powder and preparation method thereof |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111057928B (en) * | 2020-01-03 | 2021-04-02 | 合肥工业大学 | WC-Co-Y with excellent comprehensive mechanical properties2O3Hard alloy and preparation method thereof |
| CN113909480B (en) * | 2020-07-08 | 2022-12-20 | 核工业西南物理研究院 | Preparation method of in-situ nano zirconium oxide particle dispersion reinforced tungsten alloy |
| CN112011703A (en) * | 2020-09-04 | 2020-12-01 | 合肥工业大学 | High-hardness composite oxide dispersion strengthening ODS tungsten alloy and preparation method thereof |
| CN113278837B (en) * | 2021-05-17 | 2022-04-26 | 合肥工业大学 | High-density Y2O3Preparation method of doped W-Re alloy |
| CN113652568B (en) * | 2021-08-06 | 2022-04-19 | 合肥工业大学 | Preparation method of rare earth oxide particle reinforced tungsten-molybdenum solid solution alloy |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1445377A (en) * | 2002-03-20 | 2003-10-01 | 哈尔滨工业大学 | Tungsten based composite material with granules of double carbide enhanced |
| KR100501674B1 (en) * | 2002-12-12 | 2005-07-20 | 성윤모 | Synthesis of Hydroxyapatite Composite Nanopowder Using Co-precipitation |
| CN103045886B (en) * | 2012-12-27 | 2015-02-11 | 大连理工大学 | Method for preparing rare-earth-tungsten electrode material |
| CN103173670A (en) * | 2013-04-09 | 2013-06-26 | 北京科技大学 | Preparation method for in-situ synthesis of carbide enhanced tungsten-based composite material |
| CN103526096B (en) * | 2013-10-25 | 2015-11-18 | 中国科学院合肥物质科学研究院 | Tungsten-zirconium-yttrium oxide Alloy And Preparation Method |
| CN105081339B (en) * | 2015-09-29 | 2017-07-28 | 河南科技大学 | A kind of preparation method of tungsten zirconium, yttrium ternary alloy powder |
| CN105441766B (en) * | 2016-01-05 | 2018-01-09 | 河南科技大学 | High-specific gravity tungsten alloy and preparation method thereof |
| CN108817387B (en) * | 2018-07-09 | 2020-02-14 | 合肥工业大学 | Preparation method of tungsten-based composite material with high hardness and high-temperature oxidation resistance |
| CN109234557B (en) * | 2018-10-24 | 2020-05-22 | 合肥工业大学 | Superfine high-hardness W-Y2O3Method for preparing composite material |
| CN109735735A (en) * | 2019-03-19 | 2019-05-10 | 合肥工业大学 | A kind of raising W-Y2O3The method of Composite Sintering compactness |
-
2019
- 2019-09-09 CN CN201910846229.XA patent/CN110512107B/en active Active
-
2020
- 2020-04-17 AU AU2020100589A patent/AU2020100589A4/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114985752A (en) * | 2022-04-27 | 2022-09-02 | 北京工业大学 | Method for preparing tungsten alloy composite powder |
| CN114990374A (en) * | 2022-06-08 | 2022-09-02 | 合肥工业大学 | Rare earth oxide particle reinforced tungsten-vanadium solid solution alloy and preparation method thereof |
| CN115055693A (en) * | 2022-06-24 | 2022-09-16 | 合肥工业大学 | Single-phase tungsten-rhenium alloy powder and preparation method thereof |
| CN115608999A (en) * | 2022-10-17 | 2023-01-17 | 合肥工业大学 | W-Y 2 O 3 -HfO 2 Composite powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110512107B (en) | 2021-11-09 |
| CN110512107A (en) | 2019-11-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU2020100589A4 (en) | Method for preparing reinforced tungsten matrix composite compounding trace elements and rare earth oxide | |
| CN107322002B (en) | Rare earth oxide doped tungsten-based composite powder and preparation method thereof | |
| CN107604186B (en) | A kind of composite rare-earth oxide reinforcing tungsten base high-specific-gravity alloy composite material and preparation method | |
| EP4156209A1 (en) | Ndfeb magnet, preparation method therefor, and application thereof | |
| CN109234557B (en) | Superfine high-hardness W-Y2O3Method for preparing composite material | |
| CN102071348B (en) | Preparation method of superfine grain nano-structure oxide dispersion strengthened steel | |
| US20220074027A1 (en) | High-hardness composite oxide dispersion-strengthened tungsten alloy and preparation method thereof | |
| CN111206164B (en) | Preparation method of high-performance ultra-fine grain molybdenum-lanthanum alloy | |
| Wu | Manufacturing of tungsten and tungsten composites for fusion application via different routes | |
| CN112030026B (en) | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material | |
| CN113652568B (en) | Preparation method of rare earth oxide particle reinforced tungsten-molybdenum solid solution alloy | |
| KR20200060444A (en) | Rare earth permanent magnet material and manufacturing method thereof | |
| CN112563013A (en) | Method for preparing high intrinsic coercivity neodymium iron boron permanent magnet material through grain boundary diffusion | |
| CN114480903B (en) | high-He-plasma-irradiation-resistance ultrafine-grained W-Y 2 O 3 Composite material and preparation method thereof | |
| CN114427062B (en) | Wide-temperature-range huge negative thermal expansion metal matrix composite material and preparation method thereof | |
| CN112435847B (en) | Preparation method of high-performance magnetic ring | |
| CN113106279A (en) | Multi-element doped oxide dispersion strengthening tungsten-based alloy and preparation method and application thereof | |
| CN110373562A (en) | A kind of magnesium-air cell AP65 magnesium-alloy anode material and its preparation method and application | |
| CN115537631B (en) | Nanometer precipitated high-strength and high-toughness low-activation FeCrVCu medium-entropy alloy and preparation method thereof | |
| CN102304646B (en) | Oxidation-resistant SmCoX-Y(SiaGebSnc)Y high-temperature permanent-magnet material for aeroengine and preparation method thereof | |
| KR20240006457A (en) | Rare earth permanent magnet and manufacturing method and application thereof | |
| CN116607037A (en) | High-strength high-conductivity Cu-Y 2 O 3 Preparation method of-Ag composite material | |
| CN103682288B (en) | Hydrogen storage electrode alloy for Ni-MH battery and preparation method thereof | |
| CN113186437A (en) | Erbium-containing oxide dispersion strengthened tungsten-based alloy and preparation method and application thereof | |
| CN111793823B (en) | High-purity gadolinium hexaboride polycrystal and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FGI | Letters patent sealed or granted (innovation patent) |