CN114875274A - High gamma' phase nickel-based high-temperature alloy powder for 3D printing and preparation process thereof - Google Patents
High gamma' phase nickel-based high-temperature alloy powder for 3D printing and preparation process thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 147
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 49
- 239000000956 alloy Substances 0.000 title claims abstract description 49
- 238000010146 3D printing Methods 0.000 title claims abstract description 47
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910000601 superalloy Inorganic materials 0.000 claims abstract description 72
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 18
- 238000007639 printing Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 48
- 238000002844 melting Methods 0.000 claims description 34
- 230000008018 melting Effects 0.000 claims description 34
- 229910052751 metal Inorganic materials 0.000 claims description 30
- 239000002184 metal Substances 0.000 claims description 30
- 238000003723 Smelting Methods 0.000 claims description 21
- 238000000889 atomisation Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 238000012216 screening Methods 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000007873 sieving Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
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- 239000000203 mixture Substances 0.000 claims description 5
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- 238000005516 engineering process Methods 0.000 description 22
- 239000010936 titanium Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 10
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- 238000009826 distribution Methods 0.000 description 6
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- 229910052715 tantalum Inorganic materials 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 229910001005 Ni3Al Inorganic materials 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 4
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- 101000912561 Bos taurus Fibrinogen gamma-B chain Proteins 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
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- 239000010935 stainless steel Substances 0.000 description 1
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- 238000009461 vacuum packaging Methods 0.000 description 1
Images
Classifications
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- 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
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- B33Y10/00—Processes of additive manufacturing
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides high gamma' phase nickel-based superalloy powder for 3D printing, which comprises the following chemical components in percentage by weight: 8.0-13.0% of Cr, 8.0-10.0% of Co, 8.5-10.0% of W, 0.4-0.6% of Mo, 2.5-4.0% of Ta, 2.5-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements. The invention also provides a corresponding preparation method. The high gamma' phase nickel-based high-temperature alloy powder for 3D printing meets the mechanical property requirement of a 3D printing high-temperature alloy product and avoids the cracking problem during printing.
Description
Technical Field
The invention relates to high gamma 'phase nickel-based superalloy powder for 3D printing and a preparation process thereof, in particular to high gamma' phase nickel-based superalloy powder for a Selective Laser Melting (SLM) metal 3D printing technology and a preparation process thereof.
Background
The 3D printing technology, also called additive manufacturing technology, is one of the most interesting subversive technologies in the field of manufacturing industry because it can rapidly manufacture complex structures and obtain new design space. The Selective Laser Melting (SLM) technology is one of the most widely used metal additive manufacturing technologies at present, and a layer of metal powder which is paved in advance is rapidly melted by adopting a precisely focused laser spot, so that functional parts with any shapes and complete metallurgical bonding can be almost directly obtained. The SLM manufacturing technology can be used for preparing high-performance, high-density and high-precision complex precision parts, and is widely applied to the preparation of stainless steel, titanium alloy, high-temperature alloy and aluminum alloy parts in the fields of aerospace, medical treatment, automobiles and the like.
In recent years, with the rapid development of metal 3D printing technologies such as SLM manufacturing technologies, rapid manufacturing of nickel-based superalloy components has been advanced, and direct manufacturing of nickel-based superalloy components can be realized.
For example, patent document CN113201667A discloses that a nickel-based superalloy is prepared by an additive manufacturing process, and the content of alloying elements for promoting the precipitation of the γ' -Ni3Al second phase in the nickel-based superalloy satisfies the following requirements: the volume fraction of a gamma' -Ni3Al second phase in the nickel-based superalloy is 45-60%, and the content of Ti in the nickel-based superalloy is 0-4 wt%; wherein, the alloy element for promoting the second phase precipitation of the gamma' -Ni3Al in the nickel-based superalloy comprises Al element, preferably Ti and/or Ta element. According to the patent, the content of a gamma '-Ni 3Al second phase in the nickel-based superalloy is used as a key parameter for balancing high-temperature mechanical property and additive manufacturing formability, and the content of the gamma' -Ni3Al phase is controlled within a range of 45-60% so as to give consideration to both the mechanical property and the formability of the nickel-based superalloy.
Also as patent document CN105296806B discloses a nickel-based superalloy powder, wherein said superalloy powder has a chemical composition allowing establishment of a gamma prime precipitation content of 60-70 vol% in said superalloy under heat treatment conditions. Characterized in that the powder has a powder size distribution of 10-100 μm and a spherical morphology and the content (wt%) ratios of the alloying elements C, B, Hf, Zr, Si are as follows: C/B is 10-32; C/Hf is greater than 2; C/Zr > 8; C/Si > 1. One preferred embodiment consists of the following chemical components (in weight%): 7.7-8.3 Cr; 5.0-5.25 Co; 2.0-2.1 Mo; 7.8-8.3W; 5.8-6.1 Ta; 4.7-5.1 Al; 1.1-1.4 Ti; 0.08-0.16C; 0.005-0.008B; 0-0.04 Hf; 0-0.01 Zr; 0-0.08 Si; the balance being Ni and unavoidable impurities.
However, compared with the traditional powder metallurgy, the 3D printing technology has higher requirements on alloy powder, the powder is required to meet the requirements of uniform components, narrow particle size distribution, low oxygen content, high sphericity, good fluidity and the like, and few researches are carried out on the nickel-based high-temperature alloy powder preparation technology for the 3D printing technology at present, and the main problems of difficulty in preparing fine-particle-size powder, low powder yield, high oxygen and other impurity contents and the like exist.
Disclosure of Invention
The invention mainly aims to provide high gamma' -phase nickel-based superalloy powder for 3D printing and a preparation process thereof, and aims to solve the problems in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a high γ' phase nickel-based superalloy powder for 3D printing, comprising a chemical composition, in weight percent: 8.0-13.0% of Cr, 8.0-10.0% of Co, 8.5-10.0% of W, 0.4-0.6% of Mo, 2.5-4.0% of Ta, 2.5-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
Preferably, the chemical components comprise, by weight: 8.0-10.0% of Cr, 8.5-9.5% of Co, 9-10.0% of W, 0.4-0.6% of Mo, 3.0-4.0% of Ta, 4.0-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
Preferably, the chemical components comprise, by weight: 9.78% of Cr, 8.72% of Co, 9.35% of W, 0.58% of Mo, 3.56% of Ta, 4.22% of Al, 0.65% of Ti, 0.09% of C, 0.015% of B, 0.008% of Zr, 0.002% of Mn, less than or equal to 0.04% of Si, less than or equal to 0.01% of P, 0.0004% of S, 0.0087% of O, and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm.
Preferably, the particle size of the superalloy powder is 15-53 μm.
Preferably, the sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method of preparing the above high γ' phase nickel-based superalloy powder for 3D printing, characterized in that the superalloy powder is prepared using an atomization method.
Preferably, the atomization method is a vacuum induction melting atomization method.
Preferably, the method comprises a blank melting step and an atomization pulverization step,
in the billet melting step, obtaining molten metal;
and in the atomization powder preparation step, atomizing the molten metal and preparing the high-temperature alloy powder.
Preferably, the billet melting step includes a vacuum degree control step, a heating step and a melting step,
in the vacuum degree control step, controlling the vacuum degree of a smelting chamber and replacing the air remained in the smelting chamber with inert gas;
in the heating step, the blank is heated to a preset temperature and is kept warm;
in the smelting step, the molten metal with uniform components is obtained.
Preferably, in the vacuum degree control step, the vacuum degree of the melting chamber is 10Pa or less, and the inert gas is argon gas having a purity of 99.999%.
Preferably, in the heating step, the predetermined temperature is 1520-1580 ℃, the heating rate is 40-60 ℃/min, and the heat preservation time is 5-15 min.
Preferably, in the smelting step, electromagnetic stirring is used to make the composition of the molten metal uniform.
Preferably, in the atomization powdering step, the molten metal is sprayed from a nozzle, so that the molten metal is impacted by high-pressure gas to form the high-temperature alloy powder.
Preferably, the nozzle is a conical nozzle, and the outlet diameter of the nozzle is 3-5 mm.
Preferably, the high-pressure gas is inert gas, and the pressure of the high-pressure gas is 3-4 MPa.
Preferably, before the billet melting step, an alloy billet preparation step is further included,
in the alloy blank preparation step, smelting to obtain a high-temperature alloy blank;
in the billet melting step, the high-temperature alloy billet is melted to obtain the molten metal.
Preferably, after the atomization pulverizing step, a powder sieving step is further included, in the powder sieving step, the high-temperature alloy powder in the target particle size range is sieved, the powder sieving step comprises a coarse powder sieving step and an ultra-fine powder sieving step,
in the coarse powder screening step, removing powder with a particle size larger than the target particle size range;
in the ultrafine powder screening step, powder having a particle size smaller than the target particle size range is removed.
Preferably, the target particle size ranges from 3 to 100 μm.
Preferably, the target particle size ranges from 15 to 53 μm.
By applying the technical scheme of the invention, at least the following beneficial effects are obtained:
1. the invention designs and develops a brand-new high gamma' phase high-temperature alloy, meets the requirement of mechanical property and solves the problem of cracking during printing;
2. according to the invention, by optimizing technical parameters of vacuum induction melting atomization powder preparation, the prepared high gamma' phase alloy powder has the performance characteristics of uniform components, low oxygen content, low impurity content, high sphericity, good fluidity, uniform particle size distribution and the like, and can be well suitable for a selective laser melting technology;
3. the particle size of the powder is reasonably selected through the screening step, so that the control of the pore size of the product is facilitated, and the powder spreading effect is improved;
4. the invention adopts the high-purity smelting atomization technology to ensure that the oxygen content of the finished product powder reaches below 100ppm and the yield of the target powder reaches above 40 percent.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a graph of the particle size distribution of a high gamma prime superalloy powder of the present invention;
FIG. 2 is a photograph of the morphology of the high gamma prime superalloy powder of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
The present invention is described in further detail below with reference to specific examples, which are not to be construed as limiting the scope of the invention as claimed.
Example 1
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 8.0-13.0% of Cr, 8.0-10.0% of Co, 8.5-10.0% of W, 0.4-0.6% of Mo, 2.5-4.0% of Ta, 2.5-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
Preferably, the chemical components comprise, by weight: 8.0-10.0% of Cr, 8.5-9.5% of Co, 9-10.0% of W, 0.4-0.6% of Mo, 3.0-4.0% of Ta, 4.0-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
More preferably, the chemical components comprise, by weight percent: 9.78% of Cr, 8.72% of Co, 9.35% of W, 0.58% of Mo, 3.56% of Ta, 4.22% of Al, 0.65% of Ti, 0.09% of C, 0.015% of B, 0.008% of Zr, 0.002% of Mn, less than or equal to 0.04% of Si, less than or equal to 0.01% of P, 0.0004% of S, 0.0087% of O, and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
Example 2
This example provides a method of preparing the high gamma' -phase nickel-based superalloy powder for 3D printing of example 1 using a vacuum induction melting atomization process. Specifically, the preparation method comprises an alloy blank preparation step, a blank melting step, an atomization powder preparation step and a powder screening step.
S1 alloy blank preparation step
In the alloy billet preparation step, a high-temperature alloy billet is obtained by smelting.
Specifically, the high gamma' phase alloy components in the designed embodiment 1 are proportioned, the raw materials are put into a vacuum induction furnace for smelting, then alloy bar stock is obtained by casting under the vacuum condition, and cylindrical alloy bar stock with the diameter range of 50-100 mm and the length of less than 1000mm is obtained by head cutting, tail removing and surface peeling treatment. More specifically, a cylindrical alloy bar stock with the diameter of 70mm and the length of 650mm is obtained through head cutting, tail removing and surface peeling treatment.
S2, blank melting step
In the billet melting step, a high-temperature alloy billet is melted to obtain molten metal. The blank melting step comprises a vacuum degree control step, a heating step and a melting step.
S2-1, vacuum degree control step
In the vacuum degree controlling step. Controlling the vacuum degree of the smelting chamber and replacing the air remained in the smelting chamber by using inert gas. Preferably, in the vacuum degree control step, the vacuum degree of the melting chamber is 10Pa or less, and the inert gas is argon gas having a purity of 99.999%.
Specifically, the alloy bar obtained in the alloy blank preparation step is placed into an alumina crucible of a vacuum atomization induction melting chamber, then the melting chamber is vacuumized, the vacuum degree is controlled to be below 10Pa, then high-purity argon is adopted for replacement operation, the purity of the argon adopted for replacement treatment is 99.999%, and the replacement operation frequency is 1-2 times. More specifically, the number of replacement operations is 2.
S2-2, heating step
In the heating step, the billet is heated to a predetermined temperature and kept warm. Preferably, in the heating step, the predetermined temperature is 1520-1580 ℃, the heating rate is 40-60 ℃/min, and the heat preservation time is 5-15 min.
Specifically, the crucible is heated, the alloy is heated to a certain temperature above the melting point of the alloy at a proper heating rate, the temperature is kept for a certain time, the heating temperature is controlled to be 40-60 ℃/min, the smelting temperature is controlled to be 1520-1580 ℃, and the temperature is kept for 5-15 min. More specifically, the alloy was heated to 1550 ℃ at a ramp rate of 50 ℃/min and held for 15 min.
S2-3, smelting step
In the smelting step, the molten metal with uniform components is obtained. Preferably, in the smelting step, electromagnetic stirring is used to make the composition of the molten metal uniform.
Specifically, in the smelting process, the smelting crucible needs to be properly tilted, and electromagnetic stirring is carried out, so that the components of molten metal are uniform.
S3, atomizing to prepare powder
And in the atomization powder preparation step, atomizing the molten metal and preparing the high-temperature alloy powder. Preferably, the molten metal is ejected from a nozzle such that the molten metal is impacted by a high pressure gas to form the superalloy powder.
Specifically, after the molten metal reaches the tapping temperature, the melting crucible is inclined, the furnace is poured, the molten metal enters the tundish and then flows through the spray plate through the guide pipe to be atomized and powdered, and the molten metal is crushed by high-pressure argon gas, flies and condenses to form metal powder. The temperature in the middle drain ladle is controlled to be 1320-1380 ℃. The nozzle is a conical nozzle, and the diameter of an outlet of the nozzle is 3-5 mm. The pressure of the high-pressure argon is 3-4 MPa. More specifically, the temperature in the tundish was controlled at 1350 ℃ and the nozzle size was 4.0mm, and the molten metal was impinged with argon gas at a pressure of 3.5 MPa.
S4, powder screening step
In the powder sieving step, the superalloy powder is sieved to obtain a target particle size range. Preferably, the target particle size ranges from 3 to 100 μm. More preferably, the target particle size ranges from 15 to 53 μm.
Specifically, after the powder is cooled, the powder is sieved by using a vibrating sieving machine, a gas sieving machine and other equipment under the protection of inert atmosphere.
The powder screening step comprises a coarse powder screening step and an ultrafine powder screening step, and in the coarse powder screening step, powder with the particle size larger than the target particle size range is removed; in the ultrafine powder screening step, the powder having a particle size smaller than the target particle size range is removed.
S4-1, coarse powder screening step
In the coarse powder screening step, screening is performed using a vibratory screening machine.
Specifically, the screen mesh number of the vibratory screen was 270 mesh, leaving 53 μm or less of fine powder.
S4-2, ultra-fine powder screening step
In the ultrafine powder screening step, a gas sieving machine is used for sieving.
Specifically, the fine powder with the particle size less than or equal to 53 mu m is subjected to air flow classification, particles with the particle size less than 15 mu m are sorted out, finished product powder with the particle size of 15-53 mu m is obtained, and finally vacuum packaging is carried out.
The high gamma' phase high-temperature alloy powder for 3D printing prepared by the process has uniform chemical components, meets the design requirements, has the sphericity of 93.2 percent, uniform particle size distribution, oxygen content of 0.0087wt percent, fluidity of 15.5s/50g, hollow powder rate of 0.31 percent and apparent density of 4.57g/cm3, achieves the yield of target powder of 43 percent, and meets the requirements of the 3D printing technology in the laser selection area.
Example 3
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 12.3 percent of Cr, 9.50 percent of Co, 8.74 percent of W, 0.42 percent of Mo, 2.91 percent of Ta, 2.98 percent of Al, 0.53 percent of Ti, 0.06 percent of C, 0.013 percent of B, 0.008 percent of Zr, 0.002 percent of Mn, less than or equal to 0.04 percent of Si, less than or equal to 0.01 percent of P, 0.0004 percent of S, 0.0087 percent of O, and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
The high-temperature alloy powder is prepared by the preparation process in the embodiment 2, and can still meet various index requirements of the laser selective 3D printing technology.
Example 4
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 8.0 percent of Cr, 8.0 percent of Co, 8.5 percent of W, 0.4 percent of Mo, 2.5 percent of Ta, 2.5 percent of Al, 0.5 percent of Ti, 0.05 percent of C, 0.013 percent of B, 0.008 percent of Zr, 0.002 percent of Mn, less than or equal to 0.04 percent of Si, less than or equal to 0.01 percent of P, 0.0004 percent of S, 0.009 percent of O, and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
The high-temperature alloy powder is prepared by the preparation process in the embodiment 2, and can still meet various index requirements of the laser selective 3D printing technology.
Example 5
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 13 percent of Cr, 10 percent of Co, 10 percent of W, 0.6 percent of Mo, 4 percent of Ta, 6 percent of Al, 1 percent of Ti, 0.1 percent of C, 0.02 percent of B, 0.02 percent of Zr, 0.01 percent of Mn, less than or equal to 0.05 percent of Si, less than or equal to 0.01 percent of P, 0.002 percent of S, 0.015 percent of O and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
The high-temperature alloy powder is prepared by the preparation process in the embodiment 2, and can still meet various index requirements of the laser selective 3D printing technology.
Example 6
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 8.0 percent of Cr, 8.5 percent of Co, 9 percent of W, 0.4 percent of Mo, 3 percent of Ta, 4 percent of Al, 0.5 percent of Ti, 0.05 percent of C, 0.013 percent of B, 0.008 percent of Zr, 0.002 percent of Mn, less than or equal to 0.04 percent of Si, less than or equal to 0.01 percent of P, 0.0005 percent of S, 0.009 percent of O and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
The high-temperature alloy powder is prepared by the preparation process in the embodiment 2, and can still meet various index requirements of the laser selective 3D printing technology.
Example 7
The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight: 10 percent of Cr, 9.5 percent of Co, 10 percent of W, 0.6 percent of Mo, 4 percent of Ta, 6 percent of Al, 1 percent of Ti, 0.1 percent of C, 0.02 percent of B, 0.02 percent of Zr, 0.01 percent of Mn, less than or equal to 0.05 percent of Si, less than or equal to 0.01 percent of P, 0.002 percent of S, 0.015 percent of O, and the balance of Ni and other impurity elements.
Preferably, the particle size of the superalloy powder is 3-100 μm. More preferably, the particle size of the superalloy powder is 15-53 μm, as shown in FIGS. 1 and 2. The sphericity of the high-temperature alloy powder is more than or equal to 90 percent, and the Hall flow rate is less than or equal to 25s/50 g.
The high-temperature alloy powder is prepared by the preparation process in the embodiment 2, and can still meet various index requirements of the laser selective 3D printing technology.
From the above description, it can be seen that the above-described embodiments of the present invention achieve at least the following technical effects:
1. the invention designs and develops a brand-new high gamma' phase high-temperature alloy, meets the requirement of mechanical property and solves the problem of cracking during printing;
2. according to the invention, by optimizing technical parameters of vacuum induction melting atomization powder preparation, the prepared high gamma' phase alloy powder has the performance characteristics of uniform components, low oxygen content, low impurity content, high sphericity, good fluidity, uniform particle size distribution and the like, and can be well suitable for a selective laser melting technology;
3. the particle size of the powder is reasonably selected through the screening step, so that the control of the pore size of the product is facilitated, and the powder spreading effect is improved;
4. the invention adopts the high-purity smelting atomization technology to ensure that the oxygen content of the finished product powder reaches below 100ppm and the yield of the target powder reaches above 40 percent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (20)
1. The high gamma' phase nickel-based superalloy powder for 3D printing is characterized by comprising the following chemical components in percentage by weight:
8.0-13.0% of Cr, 8.0-10.0% of Co, 8.5-10.0% of W, 0.4-0.6% of Mo, 2.5-4.0% of Ta, 2.5-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
2. The high gamma prime nickel-based superalloy powder for 3D printing according to claim 1, wherein the high gamma prime nickel-based superalloy powder comprises the following chemical components in percentage by weight: 8.0-10.0% of Cr, 8.5-9.5% of Co, 9-10.0% of W, 0.4-0.6% of Mo, 3.0-4.0% of Ta, 4.0-6.0% of Al, 0.5-1.0% of Ti, 0.05-0.10% of C, less than or equal to 0.02% of B, less than or equal to 0.02% of Zr, less than or equal to 0.01% of Mn, less than or equal to 0.05% of Si, less than or equal to 0.01% of P, less than or equal to 0.002% of S, less than or equal to 0.15% of O, and the balance of Ni and other impurity elements.
3. The high gamma prime nickel-based superalloy powder for 3D printing according to claim 1, wherein the high gamma prime nickel-based superalloy powder comprises the following chemical components in percentage by weight: 9.78% of Cr, 8.72% of Co, 9.35% of W, 0.58% of Mo, 3.56% of Ta, 4.22% of Al, 0.65% of Ti, 0.09% of C, 0.015% of B, 0.008% of Zr, 0.002% of Mn, less than or equal to 0.04% of Si, less than or equal to 0.01% of P, 0.0004% of S, 0.0087% of O, and the balance of Ni and other impurity elements.
4. The high gamma prime nickel-based superalloy powder for 3D printing according to any of claims 1 to 3, wherein the particle size of the superalloy powder is 3 to 100 μm.
5. The high gamma prime nickel-based superalloy powder for 3D printing according to claim 4, wherein the superalloy powder has a particle size of 15-53 μ ι η.
6. The high gamma' -phase nickel-based superalloy powder for 3D printing according to any of claims 1 to 3, wherein the sphericity of the superalloy powder is equal to or greater than 90%, and the Hall flow rate is equal to or less than 25s/50 g.
7. A method of preparing a high gamma prime nickel-based superalloy powder for 3D printing according to any of claims 1 to 6, wherein the superalloy powder is prepared using an atomization method.
8. The method for preparing the high gamma' -phase nickel-based superalloy powder for 3D printing according to claim 7, wherein the atomization method is a vacuum induction melting atomization method.
9. The method for preparing high gamma' -phase nickel-base superalloy powder for 3D printing according to claim 7, comprising a billet melting step and an atomization milling step,
in the billet melting step, obtaining molten metal;
and in the atomization powder preparation step, atomizing the molten metal and preparing the high-temperature alloy powder.
10. The method for preparing high gamma' -phase nickel-base superalloy powder for 3D printing according to claim 9, wherein the billet melting step includes a vacuum degree control step, a heating step, and a melting step,
in the vacuum degree control step, controlling the vacuum degree of a smelting chamber and replacing the air remained in the smelting chamber with inert gas;
in the heating step, the blank is heated to a preset temperature and is kept warm;
in the smelting step, the molten metal with uniform components is obtained.
11. The method of preparing a high γ' phase nickel-based superalloy powder for 3D printing according to claim 10, wherein in the vacuum degree controlling step, the vacuum degree of the melting chamber is 10Pa or less, and the inert gas is argon having a purity of 99.999%.
12. The method for preparing the high gamma prime nickel-based superalloy powder for 3D printing according to claim 10, wherein in the heating step, the predetermined temperature is 1520-1580 ℃, the temperature rise rate is 40-60 ℃/min, and the holding time is 5-15 min.
13. The method for preparing the high gamma' -phase nickel-base superalloy powder for 3-D printing according to claim 10, wherein in the melting step, electromagnetic stirring is used to make the composition of the molten metal uniform.
14. The method for preparing high γ' phase nickel-based superalloy powder for 3D printing according to claim 9, wherein in the atomizing pulverization step, the molten metal is ejected from a nozzle, so that the molten metal is impacted by high pressure gas to form the superalloy powder.
15. The method for preparing the high gamma prime nickel-based superalloy powder for 3D printing according to claim 14, wherein the nozzle is a tapered nozzle, and an outlet diameter of the nozzle is 3 mm to 5 mm.
16. The method for preparing the high γ' phase nickel-base superalloy powder for 3D printing according to claim 15, wherein the high pressure gas is an inert gas, and a pressure of the high pressure gas is 3 to 4 MPa.
17. The method for preparing high gamma prime nickel-based superalloy powder for 3D printing according to any of claims 9 to 16, further comprising an alloy billet preparation step prior to the billet melting step,
in the alloy blank preparation step, smelting to obtain a high-temperature alloy blank;
in the billet melting step, the high-temperature alloy billet is melted to obtain the molten metal.
18. The method for preparing high gamma prime nickel-based superalloy powder for 3D printing according to any one of claims 9 to 16, further comprising a powder sieving step after the atomization milling step, wherein the superalloy powder is sieved to obtain a target particle size range, the powder sieving step comprises a coarse powder sieving step and an ultra-fine powder sieving step,
in the coarse powder screening step, removing powder with a particle size larger than the target particle size range;
in the ultrafine powder screening step, the powder having a particle size smaller than the target particle size range is removed.
19. The method of preparing a high γ' phase nickel-base superalloy powder for 3D printing according to claim 18, wherein the target particle size range is 3-100 μ ι η.
20. The method of preparing a high γ' phase nickel-base superalloy powder for 3D printing according to claim 19, wherein the target particle size range is 15-53 μ ι η.
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