CN113084181A - Preparation method of GH3230 nickel-based superalloy powder for 3D printing - Google Patents
Preparation method of GH3230 nickel-based superalloy powder for 3D printing Download PDFInfo
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- CN113084181A CN113084181A CN202110390068.5A CN202110390068A CN113084181A CN 113084181 A CN113084181 A CN 113084181A CN 202110390068 A CN202110390068 A CN 202110390068A CN 113084181 A CN113084181 A CN 113084181A
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- 239000000843 powder Substances 0.000 title claims abstract description 102
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 36
- 238000010146 3D printing Methods 0.000 title claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 64
- 230000008018 melting Effects 0.000 claims abstract description 64
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 38
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 238000009689 gas atomisation Methods 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 97
- 239000000956 alloy Substances 0.000 claims description 97
- 238000010438 heat treatment Methods 0.000 claims description 60
- 238000003723 Smelting Methods 0.000 claims description 51
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 239000003381 stabilizer Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 230000006698 induction Effects 0.000 claims description 20
- 238000006722 reduction reaction Methods 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000000889 atomisation Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 238000007605 air drying Methods 0.000 claims description 12
- 238000012216 screening Methods 0.000 claims description 11
- 238000005275 alloying Methods 0.000 claims description 9
- 238000007670 refining Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000009461 vacuum packaging Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 230000001174 ascending effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 238000010894 electron beam technology Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000000110 selective laser sintering Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010312 secondary melting process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000010313 vacuum arc remelting Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
Abstract
The invention belongs to the technical field of preparation of nickel-based superalloy powder, and particularly relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing, which adopts vacuum melting and high-pressure inert gas atomization technology, and the prepared GH3230 nickel-based superalloy powder for 3D printing has the advantages of accurate control of chemical components, stable lanthanum element yield, low powder oxygen content, high sphericity, low hollow sphere rate and good fluidity, particle size distribution meeting the requirements of 3D printing technology in a laser selection area of 15-45 mu m or 15-53 mu m, particle size distribution meeting the requirements of 3D printing technology in an electron beam selection area of 45-105 mu m or 53-105 mu m, yield of powder of 15-105 mu m reaching more than 80%, and yield of fine powder of 15-53 mu m reaching more than 30%.
Description
Technical Field
The invention belongs to the technical field of preparation of nickel-based superalloy powder, and particularly relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing.
Background
GH3230 is a Ni-Cr-W-Mo solid solution reinforced high temperature alloy reinforced by carbides, and the total content of W + Mo + Cr elements in the alloy exceeds 35%, so that the GH3230 alloy has excellent strength, fatigue resistance and high temperature oxidation resistance. In the similar products, the performance is greatly improved compared with GH3536, and the oxidation resistance and creep property of the GH5188 alloy are equivalent. Meanwhile, the alloy has good forming process performance and welding performance, is suitable for manufacturing parts such as rocket tubes of aircraft engines, and is widely applied to combustion chambers of aircraft engines, combustion chambers of ground gas turbines, high-temperature corrosion-resistant parts in the chemical industry and the like.
GH3230 contains a large amount of alloy elements, particularly trace rare earth element lanthanum, and the alloy element lanthanum is very easy to oxidize in the smelting process, so that the components can not meet the use requirements, and the GH3230 is generally produced by adopting a vacuum induction smelting and electroslag remelting or vacuum arc remelting process. However, GH3230 nickel-based superalloy parts manufactured by the traditional process have the defects of component segregation and performance deviation respectively, and cannot meet the use requirements of aerospace on materials.
The selective sintering 3D printing technology starts in the early 90 s of the 20 th century, the process difficulty is high, high-power energy beams such as laser or electron beams are mainly used as heat sources, powder materials are subjected to selective melting, a stacking layer which is strictly manufactured according to design is formed after cooling crystallization, the stacking layer is continuously formed, a final product is formed, and the defect of component segregation is overcome. The metal powder materials used in the selective laser sintering technology at present are titanium alloy, aluminum alloy, stainless steel, cobalt-based high-temperature alloy and the like. The GH3230 alloy powder for the selective laser sintering 3D printing technology is different from powder characteristics required by traditional powder metallurgy, and the powder is required to be uniform in components, narrow in particle size distribution (15-53 mu m), low in oxygen content, high in sphericity and good in flowability. At present, enterprises for producing GH3230 alloy powder at home and abroad generally use alloy ingots as parent metals, GH3230 alloy powder for 3D printing is produced in a vacuum melting and gas atomization mode, and through the processing of the parent alloy secondary melting process, secondary oxidation of alloy melt is caused by atmosphere and materials contacting the alloy melt in the melting process, the content of easily-oxidized alloy, particularly alloy lanthanum, is extremely difficult to control, and finally the composition is not enough, so that the use requirement cannot be met.
The research on GH3230 nickel-based high-temperature alloy powder for the 3D printing technology is less in China, and the GH3230 nickel-based high-temperature alloy powder is limited by the domestic powder preparation technology, so that the main problems of inaccurate component control, difficulty in preparing fine-particle-size powder, low powder yield, high oxygen and other impurity contents and the like exist, and the application of the GH3230 nickel-based high-temperature alloy powder in high-end industries such as aerospace and the like is restricted.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of GH3230 nickel-based superalloy powder for 3D printing.
The specific technical scheme is as follows:
the preparation method of the GH3230 nickel-based superalloy powder for 3D printing specifically comprises the following steps:
(1) cleaning of melting crucibles
Removing residual impurities on the inner wall of the crucible, and removing residues at the bottom of the crucible and refractory material impurities;
(2) high temperature resistant reaction stability treatment of inner walls of smelting crucible and tundish
Selecting a material which resists high-temperature molten metal corrosion, has good wettability with a crucible material and does not react with the crucible and molten metal liquid as a high-temperature reduction reaction resisting stabilizer, diluting the high-temperature reduction reaction resisting stabilizer with absolute ethyl alcohol or acetone to prepare high-temperature reduction reaction resisting stabilizer slurry, then uniformly coating the slurry on the inner wall, the bottom and the inner wall of a tundish of a smelting crucible, repeating the steps once after natural air drying, starting an induction smelting power supply of the smelting crucible and a power supply of the tundish after natural air drying, heating the smelting crucible and the tundish to 300 +/-50 ℃, preserving heat for 60-90 min, then heating to 800 +/-50 ℃, preserving heat for 120-150 min, and finally heating to 1200 +/-50 ℃, preserving heat for 120-150 min;
(3) the alloy is prepared from the following GH3230 alloy components in percentage by mass: 0.05-0.15% of C, 20.00-24.00% of Cr, 1.00-3.00% of Mo, the balance of Ni, 13.00-15.00% of W, less than or equal to 3.00% of Fe, 0.005-0.05% of La, less than or equal to 0.015% of B, 0.3-1.0% of Mn, 0.25-0.75% of Si, less than 0.03% of P, less than 0.015% of S, less than or equal to 0.5% of Cu, less than or equal to 0.10% of Ti, Al: 0.20-0.50%;
firstly, adding all raw materials except lanthanum into a melting crucible of a vacuum melting chamber, placing small-particle raw materials at the bottom of the crucible, placing high-temperature alloy in a middle high-temperature area, and tightly descending and loosely ascending; then adding lanthanum into an alloy secondary feeding bin;
(4) the smelting crucible and the tundish heating system start to be powered on and heated, meanwhile, a vacuum pump is started to carry out system vacuumizing operation, the initial heating rate of the smelting crucible is controlled within 10 ℃ and min < -1 >, the power is gradually increased after 10min, and the heating rate is increased to 20-30 ℃ and min < -1 >; the initial heating rate of the tundish is controlled within 10 ℃ and min < -1 >, and after 10min, the power is gradually increased to control the heating rate to be 25-40 ℃ and min < -1 >; starting a vacuum pump to work within 30min to enable the vacuum degrees of the smelting chamber and the atomizing chamber to reach below 1 Pa;
(5) smelting, refining and secondary feeding alloying
After the raw materials in the melting crucible are completely melted, controlling the melting temperature rise rate to be 5-10 ℃ min-1; keeping the temperature of the alloy melt in the melting crucible at 1450-1600 ℃, keeping the temperature for 10-20 min, and filling inert gas into the melting chamber and the atomizing chamber to enable the pressure of the melting chamber to reach 0.1-0.15 Mpa; opening a secondary feeding bin, adding lanthanum into a melting crucible, standing for 1-3 min to ensure that the lanthanum is completely melted, and realizing refining and secondary feeding alloying, wherein the temperature of the tundish is controlled to reach 1100-1400 ℃ in the process, and the temperature is kept for 10-30 min;
(6) adjusting the frequency of a smelting induction power supply of a smelting crucible, ensuring the temperature of a molten alloy melt to be 1500-1650 ℃, and standing for 3-5 min;
(7) pouring the molten alloy melt into a tundish, and leading the molten alloy melt into an air atomization system through a flow guide pipe at the bottom of the tundish, wherein the air atomization system consists of an annular seam type air atomization spray disc and a nozzle with a circular hole; high-pressure inert gas is sprayed out of the annular seam type gas atomization spray disc, the molten alloy melt flow flowing out of the nozzle is smashed into fine liquid drops, and the liquid drops are cooled and solidified to form spherical alloy powder in the flying process; the diameter of the circular hole of the nozzle is 3.5-6 mm, the atomization flow of the molten alloy melt is 3-10 kg/min, and the pressure of the high-pressure inert gas is 2-6 Mpa;
(8) and (3) putting the solidified and molded spherical alloy powder into a powder collecting tank, fully cooling, taking out, performing airflow classification or ultrasonic vibration screening under the protection of inert atmosphere to obtain GH3230 nickel-based high-temperature alloy powder which is suitable for 3D printing and has the particle size of 15-45 microns, 15-53 microns, 45-105 microns or 53-105 microns, and finally performing vacuum packaging on a finished product.
In the step (1), the smelting crucible is mainly made of fused magnesia or alumina, the mass percent of MgO is not less than 95%, and the mass percent of Al2O3 is not less than 95%.
The tundish in the step (2) is mainly made of alumina, Al2O3 accounts for not less than 95% by mass, and contains a small amount of Y2O3, Y2O3 accounts for 1-3% by mass, and the balance is CaO and SiO2 impurities.
The high-temperature reduction reaction resistant stabilizer in the step (2) is AlN, BN, ZrO2 or Y2O3, the purity is not less than 99% by mass, the particle size of the stabilizer is 0.05-10 mu m, and the mass ratio of the high-temperature reduction reaction resistant stabilizer to the absolute ethyl alcohol or acetone solution when the stabilizer is diluted is 0.2-1.
And (5) the inert gas is high-purity argon or high-purity nitrogen, and the gas purity is not lower than 99.99%.
In the step (7), the material of the flow guide pipe is ZrO2 or Al2O3, and the purity is not less than 99% by mass.
In the step (7), the nozzle with the round hole is made of ZrO2 or BN, and the purity is not less than 99% by mass.
In the step (8), the inert atmosphere is high-purity argon or high-purity nitrogen, and the gas purity is not lower than 99.99%.
Compared with the prior art, the invention has the following beneficial technical effects:
the GH3230 nickel-based high-temperature alloy powder for 3D printing prepared by the method is accurate in chemical component control, stable in lanthanum element yield, low in powder oxygen content, high in sphericity, low in hollow sphere rate and good in fluidity, the particle size distribution meets the requirements of a 3D printing technology in a laser selection area by 15-45 mu m or 15-53 mu m, the particle size distribution meets the requirements of the 3D printing technology in an electron beam selection area by 45-105 mu m or 53-105 mu m, the yield of the 15-105 mu m powder reaches more than 80%, and the yield of fine powder with the particle size of 15-53 mu m reaches more than 30%.
Drawings
FIG. 1 is a photograph showing the 15 μm to 53 μm morphology of GH3230 nickel-base superalloy powder prepared in example 1;
FIG. 2 is a particle size distribution of 15 μm to 53 μm for GH3230 Ni-based superalloy powder prepared in example 1;
FIG. 3 is a photograph showing the 15 μm to 53 μm morphology of GH3230 nickel-base superalloy powder prepared in example 2;
FIG. 4 is a particle size distribution of 15 μm to 53 μm for GH3230 Ni-based superalloy powder prepared in example 2;
FIG. 5 is a 15 μm to 53 μm morphology photograph of GH3230 nickel-base superalloy powder prepared in example 3;
FIG. 6 is a particle size distribution of 15 μm to 53 μm for GH3230 Ni-based superalloy powder prepared in example 3;
FIG. 7 is a 15 μm to 53 μm morphology photograph of GH3230 nickel-base superalloy powder prepared in example 4;
FIG. 8 is a graph of the particle size distribution of GH3230 nickel-base superalloy powders prepared in example 4.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited by the embodiments.
Example 1:
cleaning a smelting crucible of fused magnesia sand and a tundish of alumina, selecting AlN with the granularity of 0.05-0.5 mu m as a high-temperature reduction reaction resistant stabilizer, adding absolute ethyl alcohol, wherein the mass ratio of the AlN to the absolute ethyl alcohol is 0.2, preparing high-temperature reduction reaction resistant stabilizer slurry, then uniformly coating the slurry on the inner wall and the bottom of the smelting crucible and the inner wall of the tundish (alumina), repeating the steps once after natural air drying, starting an induction smelting power supply and the tundish power supply after natural air drying, heating to 250 ℃, keeping the temperature for 90min, then heating to 800 ℃, keeping the temperature for 130min, and finally heating to 1150 ℃, keeping the temperature for 150min for later use; proportioning according to GH3230 alloy components, and adding all alloy raw materials except lanthanum into a vacuum induction furnace for smeltingIn the crucible, lanthanum is added into an alloy secondary feeding bin; and the smelting system and the tundish heating system start to be powered on and heated, and simultaneously, a vacuum pump is started to carry out the vacuumizing operation of the system. The initial heating rate of the melting crucible is controlled at 10 ℃ min-1Within 10min, gradually increasing the power, and increasing the heating rate to 20-30 ℃ per min-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work for 20min, wherein the vacuum degrees of a smelting chamber and an atomizing chamber reach 0.8 Pa; controlling the heating rate of smelting at about 5 ℃ per minute after the raw materials in the crucible to be smelted are completely melted-1(ii) a Keeping the temperature of the alloy melt in the melting crucible at 1455 ℃ for 20min, introducing high-purity argon into the melting chamber and the atomizing chamber to make the pressure of the melting chamber reach 0.1MPa, then opening a secondary feeding bin, adding lanthanum into the melting crucible, and standing for 3 min; controlling the temperature of the tundish to 1300 ℃ in the whole refining and secondary feeding alloying process, and preserving the heat for 10 min; adjusting the frequency of a smelting induction power supply, ensuring the temperature of the molten alloy melt to be 1500 ℃, and standing for 5 min; pouring the molten alloy melt into a tundish, passing the molten alloy melt through a flow guide pipe (ZrO)2Mass) is introduced into a tightly coupled atomization system, and high-temperature alloy powder is obtained through high-pressure high-purity argon atomization treatment, wherein a nozzle in the step is BN, the aperture of the nozzle is 6mm, the flow of a molten alloy melt is 9.8kg/min, and the pressure of high-pressure inert gas is 5.5 MPa; and (3) putting the solidified and molded spherical powder into a powder collecting tank, fully cooling, taking out, performing ultrasonic vibration screening in a high-purity argon atmosphere to obtain GH3230 nickel-based high-temperature alloy powder suitable for 3D printing, and finally performing vacuum packaging on a finished product.
Through analysis, the components of the GH3230 nickel-based superalloy powder prepared in example 1 are detailed in Table 1, the components all meet the requirements of GB/T14992-2005, particularly, the lanthanum content can be accurately controlled to be 0.018%, the yield of lanthanum element reaches over 70%, the oxygen content of the powder is 0.011%, as can be seen from the graph 1, the sphericity of the powder is better, only a small amount of satellite balls exist, the yield of the powder with the particle size of 15-105 μm reaches 80.7% and the yield of the powder with the particle size of 15-53 μm reaches 31.3% through calculation after screening.
Example 2
The invention relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing, which comprises the following steps:
cleaning an aluminum oxide smelting crucible and an aluminum oxide tundish, selecting BN with the particle size of 0.05-1 mu m as a high-temperature reduction reaction resistant stabilizer, adding acetone, wherein the mass ratio of the BN to the acetone is 0.5, preparing high-temperature reduction reaction resistant stabilizer slurry, then uniformly coating the slurry on the inner wall and the bottom of the smelting crucible and the inner wall of the tundish (aluminum oxide), repeating the steps once after natural air drying, starting an induction smelting power supply after natural air drying, heating to 300 ℃, keeping the temperature for 70min, then heating to 750 ℃, keeping the temperature for 140min, and finally heating to 1200 ℃, keeping the temperature for 130min for later use; batching according to GH3230 alloy components specified in GB/T14992-2005, adding all alloy raw materials except lanthanum into a melting crucible of a vacuum induction furnace, and adding lanthanum into an alloy secondary feeding bin; and the smelting system and the tundish heating system start to be powered on and heated, and simultaneously, a vacuum pump is started to carry out the vacuumizing operation of the system. The initial heating rate of the melting crucible is controlled at 10 ℃ min-1Within 10min, gradually increasing the power, and increasing the heating rate to 20-30 ℃ per min-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work for 25min, wherein the vacuum degrees of a smelting chamber and an atomizing chamber reach 0.7 Pa; controlling the heating rate of melting at about 8 ℃ per minute after the raw materials in the melting crucible are completely melted-1(ii) a Keeping the temperature of the alloy melt in the melting crucible for 20min after the temperature reaches 1510 ℃, filling high-purity argon into the melting chamber and the atomizing chamber to ensure that the pressure of the melting chamber reaches 0.12MPa, then opening a secondary feeding bin, adding lanthanum (La rare earth metal) into the melting crucible, and standing for 2 min; controlling the temperature of the tundish to 1200 ℃ in the whole refining and secondary feeding alloying process, and preserving the heat for more than 20 min; adjusting the frequency of a smelting induction power supply, ensuring the temperature of the molten alloy melt to be 1570 ℃, and standing for 4 min; pouring the molten alloy melt into a tundish, passing the molten alloy melt through a flow guide pipe (ZrO)2Material) is introduced into a tightly coupled atomization system and is atomized by high-pressure high-purity argon to obtain high-temperature alloy powder, wherein a nozzle in the step is ZrO2The aperture of the nozzle is 4.5mm, the injection speed of the molten alloy melt is 6.5kg/min, and the pressure of the high-pressure inert gas is 4 MPa; and (3) feeding the solidified and molded spherical powder into a powder collecting tank, fully cooling, taking out, performing airflow classification screening under the atmosphere of high-purity argon to obtain GH3230 nickel-based high-temperature alloy powder suitable for 3D printing, and finally performing vacuum packaging on a finished product.
Through analysis, the components of the GH3230 nickel-based superalloy powder prepared in example 2 are detailed in Table 1, the components all meet the requirements of GB/T14992-2005, particularly, the lanthanum content can be accurately controlled to be 0.022%, the lanthanum element yield reaches 67.3%, the powder oxygen content is 0.0078%, as can be seen from FIG. 3, the powder sphericity is better, only a small amount of satellite balls are provided, and the yield of the powder with the particle size of 15-105 μm reaches 82.2% and the yield of the powder with the particle size of 15-53 μm reaches 35.7% through calculation after screening.
Example 3
The invention relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing, which comprises the following steps:
firstly, cleaning an aluminum oxide smelting crucible and an aluminum oxide tundish, and selecting ZrO with the granularity of 0.1-10 mu m2Adding acetone and ZrO as stabilizer for high-temp reduction reaction2Preparing stabilizer slurry for resisting high-temperature reduction reaction with acetone according to the mass ratio of 1, uniformly coating the slurry on the inner wall and the bottom of a melting crucible and the inner wall of a tundish (alumina), repeating the steps once after natural air drying, starting an induction melting power supply and the tundish power supply after natural air drying, heating to 350 ℃, preserving heat for 60min, then heating to 850 ℃, preserving heat for 120min, and finally heating to 1250 ℃, preserving heat for 125min for later use; batching according to GH3230 alloy components specified in GB/T14992-2005, adding all alloy raw materials except lanthanum into a melting crucible of a vacuum induction furnace, and adding lanthanum into an alloy secondary feeding bin; the smelting system and the tundish heating system start to be powered on and heated, and simultaneously, the vacuum pump is started to carry out system vacuumizing operationDo this. The initial heating rate of the melting crucible is controlled at 10 ℃ min-1Within 10min, gradually increasing the power, and increasing the heating rate to 20-30 ℃ per min-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work for 30min, wherein the vacuum degrees of a smelting chamber and an atomizing chamber reach 0.9 Pa; controlling the heating rate of melting at about 10 ℃ per minute after the raw materials in the melting crucible are completely melted-1(ii) a Keeping the temperature of the alloy melt in the melting crucible at 1600 ℃ for 10min, filling high-purity nitrogen into the melting chamber and the atomizing chamber to enable the pressure of the melting chamber to reach 0.14MPa, then opening a secondary feeding bin, adding lanthanum (La rare earth metal) into the melting crucible, and standing for 1.5 min; controlling the temperature of the tundish to 1100 ℃ in the whole refining and secondary feeding alloying process, and preserving the heat for 30 min; adjusting the frequency of a smelting induction power supply, ensuring that the temperature of the molten alloy melt is 1630 ℃, and standing for 3 min; pouring the molten alloy melt into a tundish, and passing the molten alloy melt through a flow guide pipe (Al)2O3Material) is introduced into a tightly coupled atomization system and is atomized by high-pressure high-purity nitrogen to obtain high-temperature alloy powder, wherein a nozzle in the step is ZrO2The aperture of the nozzle is 3.5mm, the flow of the molten alloy melt is 4.3kg/min, and the pressure of the high-pressure inert gas is 3 MPa; and (3) putting the solidified and molded spherical powder into a powder collecting tank, fully cooling, taking out, performing ultrasonic vibration screening in a high-purity nitrogen atmosphere to obtain GH3230 nickel-based high-temperature alloy powder suitable for 3D printing, and finally performing vacuum packaging on a finished product.
Through analysis, the components of the GH3230 nickel-based superalloy powder prepared in example 3 are detailed in Table 1, the components all meet the requirements of GB/T14992-2005, particularly, the lanthanum content can be accurately controlled to be 0.0083%, the lanthanum element yield reaches 62.5%, the powder oxygen content is 0.0082%, and as can be seen from FIG. 5, the powder sphericity is better, only a small amount of satellite balls are provided, and the yield of the powder with the particle size of 15-105 μm reaches 81.8% and the yield of the powder with the particle size of 15-53 μm reaches 41.5% through calculation after screening.
Example 4
The invention relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing, which comprises the following steps:
firstly, cleaning an aluminum oxide smelting crucible and an aluminum oxide tundish, and selecting ZrO with the granularity of 0.5-10 mu m2Adding anhydrous ethanol and ZrO as stabilizer for high-temperature reduction reaction2Preparing stabilizer slurry for resisting high-temperature reduction reaction, uniformly coating the stabilizer slurry on the inner wall and the bottom of a melting crucible and the inner wall of a tundish (alumina), naturally drying, repeating the steps once, naturally drying, starting an induction melting power supply and the tundish power supply, heating to 320 ℃, keeping the temperature for 75min, heating to 830 ℃, keeping the temperature for 135min, and finally heating to 1230 ℃, keeping the temperature for 130min for later use; batching according to GH3230 alloy components specified in GB/T14992-2005, adding all alloy raw materials except lanthanum into a melting crucible of a vacuum induction furnace, and adding lanthanum into an alloy secondary feeding bin; and the smelting system and the tundish heating system start to be powered on and heated, and simultaneously, a vacuum pump is started to carry out the vacuumizing operation of the system. The initial heating rate of the melting crucible is controlled at 10 ℃ min-1Within 10min, gradually increasing the power, and increasing the heating rate to 20-30 ℃ per min-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work for 30min, wherein the vacuum degrees of a smelting chamber and an atomizing chamber reach 0.7 Pa; controlling the heating rate of melting at about 10 ℃ per minute after the raw materials in the melting crucible are completely melted-1(ii) a Keeping the temperature of the alloy melt in the melting crucible at 1520 ℃ for 15min, introducing high-purity argon into the melting chamber and the atomizing chamber to make the pressure of the melting chamber reach 0.11MPa, then opening a secondary feeding bin, adding lanthanum (La rare earth metal) into the melting crucible, and standing for 2 min; controlling the temperature of the tundish to reach 1380 ℃ in the whole refining and secondary feeding alloying process, and keeping the temperature for 15 min; adjusting the frequency of a smelting induction power supply, ensuring the temperature of the molten alloy melt to be 1610 ℃, and standing for 4 min; pouring the molten alloy melt into a tundish, and passing the molten alloy melt through a flow guide pipe (Al)2O3Material) is introduced into a tightly coupled atomization system and high-purity high-pressureAtomizing with argon to obtain high-temperature alloy powder, wherein the nozzle in the step is ZrO2The diameter of a nozzle is 4.2mm, the flow of the molten alloy melt is 5.6kg/min, and the pressure of high-pressure inert gas is 3.6 MPa; and (3) putting the solidified and molded spherical powder into a powder collecting tank, fully cooling, taking out, performing ultrasonic vibration screening in a high-purity nitrogen atmosphere to obtain GH3230 nickel-based high-temperature alloy powder suitable for 3D printing, and finally performing vacuum packaging on a finished product.
Through analysis, the components of the GH3230 nickel-based superalloy powder prepared in example 4 are detailed in Table 1, the components all meet the requirements of GB/T14992-2005, particularly, the lanthanum content can be accurately controlled to be 0.031%, the lanthanum element yield reaches 66.4%, the powder oxygen content is 0.012%, and as can be seen from FIG. 7, the powder sphericity is good, only a small number of satellite balls are provided, and the yield of the 15-105 μm powder reaches 83.2% and the yield of the 15-53 μm powder reaches 37.8% through calculation after screening.
Example 5
The invention relates to a preparation method of GH3230 nickel-based superalloy powder for 3D printing, which comprises the following steps:
firstly, cleaning a melting crucible of fused magnesia sand and a tundish of alumina, and selecting Y with the granularity of 0.1-5 mu m2O3Adding acetone and Y as stabilizer for high-temperature reduction reaction2O3Preparing high-temperature reduction reaction resistant stabilizer slurry with the mass ratio of the slurry to acetone being 0.25, then uniformly coating the slurry on the inner wall and the bottom of a melting crucible and the inner wall of a tundish (alumina), repeating the steps once after natural air drying, starting an induction melting power supply and the tundish power supply after natural air drying, heating to 280 ℃, preserving heat for 80min, then heating to 810 ℃, preserving heat for 140min, and finally heating to 1180 ℃, preserving heat for 135min for later use; batching according to GH3230 alloy components specified in GB/T14992-2005, adding all alloy raw materials except lanthanum into a melting crucible of a vacuum induction furnace, and adding lanthanum into an alloy secondary feeding bin; and the smelting system and the tundish heating system start to be powered on and heated, and simultaneously, a vacuum pump is started to carry out the vacuumizing operation of the system. Initial heating speed of smelting crucibleThe rate is controlled at 10 ℃ min-1Within 10min, gradually increasing the power, and increasing the heating rate to 20-30 ℃ per min-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work for 20min, wherein the vacuum degrees of a smelting chamber and an atomizing chamber reach 0.6 Pa; controlling the heating rate of melting at about 10 ℃ per minute after the raw materials in the melting crucible are completely melted-1(ii) a Keeping the temperature of the alloy melt in the melting crucible at 1550 ℃ for 13min, introducing high-purity argon into the melting chamber and the atomizing chamber to enable the pressure of the melting chamber to reach 0.1MPa, then opening a secondary feeding bin, adding lanthanum (La rare earth metal) into the melting crucible, and standing for 3 min; controlling the temperature of the tundish to 1150 ℃ in the whole refining and secondary feeding alloying process, and preserving the heat for 20 min; adjusting the frequency of a smelting induction power supply, ensuring that the temperature of the molten alloy melt is 1530 ℃, and standing for 4 min; pouring the molten alloy melt into a tundish, and passing the molten alloy melt through a flow guide pipe (Al)2O3Mass) is introduced into a tightly coupled atomization system, and high-temperature alloy powder is obtained through high-pressure high-purity argon atomization treatment, wherein a nozzle in the step is BN, the aperture of the nozzle is 5mm, the flow of a molten alloy melt is 8.7kg/min, and the pressure of high-pressure inert gas is 4.6 MPa; and (3) putting the solidified and molded spherical powder into a powder collecting tank, fully cooling, taking out, performing ultrasonic vibration screening in a high-purity argon atmosphere to obtain GH3230 nickel-based high-temperature alloy powder suitable for 3D printing, and finally performing vacuum packaging on a finished product.
Through analysis, the components of the GH3230 nickel-based superalloy powder prepared in example 1 are detailed in Table 1, the components all meet the requirements of GB/T14992-2005, particularly, the lanthanum content can be accurately controlled to be 0.028%, the yield of lanthanum elements reaches over 62.6%, the oxygen content of the powder is 0.010%, the yield of powder with the particle size of 15-105 μm reaches 81.1%, and the yield of powder with the particle size of 15-53 μm reaches 32.2%.
TABLE 1 example GH3230 Nickel base superalloy powder composition/wt%
Claims (8)
1. The preparation method of the GH3230 nickel-based superalloy powder for 3D printing is characterized by comprising the following steps:
(1) cleaning of melting crucibles
Removing residual impurities on the inner wall of the crucible, and removing residues at the bottom of the crucible and refractory material impurities;
(2) high temperature resistant reaction stability treatment of inner walls of smelting crucible and tundish
Selecting a material which resists high-temperature molten metal corrosion, has good wettability with a crucible material and does not react with the crucible and molten metal liquid as a high-temperature reduction reaction resisting stabilizer, diluting the high-temperature reduction reaction resisting stabilizer with absolute ethyl alcohol or acetone to prepare high-temperature reduction reaction resisting stabilizer slurry, then uniformly coating the slurry on the inner wall, the bottom and the inner wall of a tundish of a smelting crucible, repeating the steps once after natural air drying, starting an induction smelting power supply of the smelting crucible and a power supply of the tundish after natural air drying, heating the smelting crucible and the tundish to 300 +/-50 ℃, preserving heat for 60-90 min, then heating to 800 +/-50 ℃, preserving heat for 120-150 min, and finally heating to 1200 +/-50 ℃, preserving heat for 120-150 min;
(3) the alloy is prepared from the following GH3230 alloy components in percentage by mass: 0.05-0.15% of C, 20.00-24.00% of Cr, 1.00-3.00% of Mo, the balance of Ni, 13.00-15.00% of W, less than or equal to 3.00% of Fe, 0.005-0.05% of La, less than or equal to 0.015% of B, 0.3-1.0% of Mn, 0.25-0.75% of Si, less than 0.03% of P, less than 0.015% of S, less than or equal to 0.5% of Cu, less than or equal to 0.10% of Ti, Al: 0.20-0.50%;
firstly, adding all raw materials except lanthanum into a melting crucible of a vacuum melting chamber, placing small-particle raw materials at the bottom of the crucible, placing high-temperature alloy in a middle high-temperature area, and tightly descending and loosely ascending; then adding lanthanum into an alloy secondary feeding bin;
(4) the smelting crucible and the tundish heating system start to be powered on and heated, simultaneously, a vacuum pump is started to carry out the vacuum pumping operation of the system, and the initial heating rate of the smelting crucible is controlled at 10 ℃ min-1Within 10min, the power is gradually increased and increasedThe temperature rate is increased to 20-30 ℃ per minute-1(ii) a The initial heating rate of the tundish is controlled at 10 ℃ min-1Within 10min, gradually increasing power to control the heating rate to be 25-40 ℃ per min-1(ii) a Starting a vacuum pump to work within 30min to enable the vacuum degrees of the smelting chamber and the atomizing chamber to reach below 1 Pa;
(5) smelting, refining and secondary feeding alloying
After all the raw materials in the melting crucible are melted, controlling the melting temperature rise rate to be 5-10 ℃ per minute-1(ii) a Keeping the temperature of the alloy melt in the melting crucible at 1450-1600 ℃, keeping the temperature for 10-20 min, and filling inert gas into the melting chamber and the atomizing chamber to enable the pressure of the melting chamber to reach 0.1-0.15 Mpa; opening a secondary feeding bin, adding lanthanum into a melting crucible, standing for 1-3 min to ensure that the lanthanum is completely melted, and realizing refining and secondary feeding alloying, wherein the temperature of the tundish is controlled to reach 1100-1400 ℃ in the process, and the temperature is kept for 10-30 min;
(6) adjusting the frequency of a smelting induction power supply of a smelting crucible, ensuring the temperature of a molten alloy melt to be 1500-1650 ℃, and standing for 3-5 min;
(7) pouring the molten alloy melt into a tundish, and leading the molten alloy melt into an air atomization system through a flow guide pipe at the bottom of the tundish, wherein the air atomization system consists of an annular seam type air atomization spray disc and a nozzle with a circular hole; high-pressure inert gas is sprayed out of the annular seam type gas atomization spray disc, the molten alloy melt flow flowing out of the nozzle is smashed into fine liquid drops, and the liquid drops are cooled and solidified to form spherical alloy powder in the flying process; the diameter of the circular hole of the nozzle is 3.5-6 mm, the atomization flow of the molten alloy melt is 3-10 kg/min, and the pressure of the high-pressure inert gas is 2-6 Mpa;
(8) and (3) putting the solidified and molded spherical alloy powder into a powder collecting tank, fully cooling, taking out, performing airflow classification or ultrasonic vibration screening under the protection of inert atmosphere to obtain GH3230 nickel-based high-temperature alloy powder which is suitable for 3D printing and has the particle size of 15-45 microns, 15-53 microns, 45-105 microns or 53-105 microns, and finally performing vacuum packaging on a finished product.
2. The method for 3D printing of claim 1The preparation method of the GH3230 nickel-based superalloy powder is characterized by comprising the following steps: in the step (1), the smelting crucible is mainly made of fused magnesia or alumina, the mass percent of MgO is not less than 95%, and Al2O3The mass percentage is not less than 95%.
3. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: in the step (2), the main materials of the tundish are alumina and Al2O3Not less than 95% by mass, and contains a small amount of Y2O3，Y2O31-3% of the balance of CaO and SiO2Impurities.
4. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: the high-temperature reduction reaction resistant stabilizer in the step (2) is AlN, BN or ZrO2Or Y2O3The purity is not less than 99 percent by mass, the granularity of the stabilizer is 0.05-10 mu m, and the mass ratio of the stabilizer to the absolute ethyl alcohol or acetone solution when the stabilizer is diluted for the high-temperature reduction reaction is 0.2-1.
5. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: and (5) the inert gas is high-purity argon or high-purity nitrogen, and the gas purity is not lower than 99.99%.
6. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: in the step (7), the material of the flow guide pipe is ZrO2Or Al2O3The purity is not less than 99 percent by mass.
7. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: in the step (7), the nozzle with the round hole is made of ZrO2Or BN, purity in mass percentNot less than 99%.
8. The method for preparing GH3230 nickel-base superalloy powder for 3D printing according to claim 1, wherein: in the step (8), the inert atmosphere is high-purity argon or high-purity nitrogen, and the gas purity is not lower than 99.99%.
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Application publication date: 20210709 |