CN112853191A - High-toughness high-entropy alloy forming material for 3D printing and preparation method - Google Patents
High-toughness high-entropy alloy forming material for 3D printing and preparation method Download PDFInfo
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- CN112853191A CN112853191A CN202110020227.2A CN202110020227A CN112853191A CN 112853191 A CN112853191 A CN 112853191A CN 202110020227 A CN202110020227 A CN 202110020227A CN 112853191 A CN112853191 A CN 112853191A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- 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
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- 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
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- 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
- B33Y80/00—Products made by additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- 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 relates to a high-toughness high-entropy alloy, in particular to a high-toughness high-entropy alloy for 3D printing and a preparation method of a high-entropy alloy forming material. The high-toughness high-entropy alloy for 3D printing comprises the following raw materials in atomic percentage: ti: 17-25 at%, V: 8-15 at%, Nb: 11-18 at%, Mo: 7-15 at%, Ta: 20-25 at%, W: 15-18 at%, the sum of atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%. The high-entropy alloy forming material obtained by determining the components and the content of the corresponding high-entropy alloy raw material and combining the preparation process parameters of the SLM has good high-temperature toughness.
Description
Technical Field
The invention relates to a high-toughness high-entropy alloy, in particular to a high-toughness high-entropy alloy for 3D printing and a preparation method of a high-toughness high-entropy alloy forming material.
Background
Compared with high polymer materials and ceramic materials, the metal materials have better strength and toughness and good safety as structural materials. The high-entropy alloy has different structural characteristics from the traditional metal material due to the multi-component effect of the high-entropy alloy, so that the high-entropy alloy has some unique properties and excellent performances in various aspects, such as high hardness, high strength, oxidation resistance and thermal stability. In the case of the conventional preparation method, the more complex the shape of the prepared object is, the higher the production cost is, the more waste in the conventional metal processing is, and some fine production even causes 80% waste of raw materials.
At present, the traditional high-entropy alloy preparation method has high cost for producing parts with complex shapes, and is difficult to simultaneously consider the strength and the toughness under a high-temperature use environment, and the problems can be solved by a Selective Laser Melting (SLM) laser 3D printing technology.
Disclosure of Invention
In view of the problems of the prior art, it is an object of the present invention to provide a high-toughness high-entropy alloy for 3D printing; the second purpose of the invention is to provide a preparation method of the high-toughness high-entropy alloy forming material, which is used for reducing the cost and simultaneously considering the strength and the toughness under the high-temperature use environment.
In order to achieve the purpose, the invention adopts the following technical scheme: a high-toughness high-entropy alloy for 3D printing is characterized in that the high-entropy alloy comprises the following raw materials in atomic percentage: ti: 17-25 at%, V: 8-15 at%, Nb: 11-18 at%, Mo: 7-15 at%, Ta: 20-25 at%, W: 15-18 at%, the sum of atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%.
According to the forming material of the high-toughness high-entropy alloy for 3D printing, preferably, the tensile strength of the high-entropy alloy forming material is 1300-1550MPa, the yield strength is 920-1030MPa, and the elongation is 20-28% in a use environment at 800 ℃; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%. The high-entropy alloy forming material has good toughness and matching property under a high-temperature use environment.
Nb is beneficial to the formation of a BCC phase and is beneficial to improving the high-temperature strength and the hardness of the alloy. V, Ta can improve the high temperature strength of the alloy, but too much brittle and hard phase is formed, which causes the toughness to be reduced and is difficult to meet the requirement. Ti and Mo can improve the strength and toughness of the alloy, W can improve the high-temperature strength, and W is excessive to cause the toughness to be reduced.
Preferably, the atomic percentages of Ti, Nb and Mo are 3: 2: (1-1.5), in which the alloy has excellent high-temperature toughness.
The invention also relates to a preparation method of the high-toughness high-entropy alloy forming material, which comprises the following steps:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 17-25 at%, V: 8-15 at%, Nb: 11-18 at%, Mo: 7-15 at%, Ta: 20-25 at%, W: 15-18 at%, the sum of atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 10-25um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. Setting the laser power of the 3D printing equipment to be 180-240W, the scanning speed to be 1000-1300mm/s and the scanning interval to be 20-50um, and obtaining the high-toughness high-entropy alloy forming material suitable for the high-temperature environment.
The SLM forming process is affected by laser power, scanning speed, scanning pitch, etc., so that the structure, high temperature mechanical properties, etc. of the forming material are different and may not meet the standard required by the forming material. The higher the laser power is, the less inclusions are generated, the excellent high-temperature performance of the molding material is, but the too high laser power causes defects such as air holes and the like, and the high-temperature performance of the molding material is reduced. The scanning speed is too high, which may affect that the powder can not be completely melted, and the formed piece is easy to generate air holes and inclusions. The scan spacing is closely related to the heat distribution of the laser beam and is an important process parameter for shaping.
Preferably, the laser power is 200-210W, and the high-temperature performance of the forming material is excellent.
Preferably, the scanning speed is 1200-1250mm/s, and the high-temperature performance of the forming material is excellent.
Preferably, the scanning interval is 25-30um, and the formed material has good quality and excellent high-temperature performance.
Tests show that under the use environment of 800 ℃, the tensile strength of the high-entropy alloy forming material is 1300-1550MPa, the yield strength is 920-1030MPa, and the elongation is 20-28%; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%. The high-entropy alloy forming material has good toughness and matching property under a high-temperature use environment.
The invention has the beneficial effects that:
1. the invention provides a high-toughness high-entropy alloy for 3D printing, which can be used for 3D printing, further reduce the cost for preparing complex parts, and ensure excellent high-temperature comprehensive properties of a forming material, such as high toughness, high strength and the like.
2. The invention provides a preparation method of a high-toughness high-entropy alloy forming material, which is characterized in that proper SLM (selective laser melting) process parameters are determined according to components and contents of high-entropy alloy powder, so that the high-temperature performance of the high-entropy alloy forming material is excellent.
3. Under the use environment of 800 ℃, the tensile strength of the high-entropy alloy forming material is 1300-1550MPa, the yield strength is 920-1030MPa, and the elongation is 20-28%; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%. The high-entropy alloy forming material has good toughness and matching property under a high-temperature use environment.
Detailed Description
The present invention will be described in further detail with reference to the following examples. The specific embodiments are to be considered as illustrative and not restrictive in character.
Embodiment 1, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 25 at%, V: 15 at%, Nb: 11 at%, Mo: 7 at%, Ta: 25 at%, W: 17at percent, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100 percent, and the purity of the raw materials is more than or equal to 99.99 percent.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 10um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 180W, the scanning speed is 1300mm/s, and the scanning interval is 30um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Embodiment 2, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 20 at%, V: 8 at%, Nb: 18 at%, Mo: 15 at%, Ta: 21 at%, W: 18at percent, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100 percent, and the purity of the raw materials is more than or equal to 99.99 percent.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 25um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 240W, the scanning speed is 1000mm/s, and the scanning interval is 50um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Embodiment 3, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 17 at%, V: 15 at%, Nb: 18 at%, Mo: 15 at%, Ta: 20 at%, W: 15at percent, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100 percent, and the purity of the raw materials is more than or equal to 99.99 percent.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 20um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 200W, the scanning speed is 1250mm/s, and the scanning interval is 30um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Embodiment 4, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 21 at%, V: 15 at%, Nb: 14 at%, Mo: 10 at%, Ta: 25 at%, W: 15at percent, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100 percent, and the purity of the raw materials is more than or equal to 99.99 percent.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 20um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 200W, the scanning speed is 1250mm/s, and the scanning interval is 30um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Comparative example 1, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 25 at%, V: 15 at%, Nb: 18 at%, Ta: 25 at%, W: 17 at%, the sum of atomic percentages of Ti, V, Nb, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 10um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 180W, the scanning speed is 1300mm/s, and the scanning interval is 30um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Comparative example 2, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 30 at%, V: 15 at%, Nb: 11 at%, Mo: 7 at%, Ta: 25 at%, W: 12 at%, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 10um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 180W, the scanning speed is 1300mm/s, and the scanning interval is 30um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
Comparative example 3, a method for preparing a high-toughness high-entropy alloy forming material, comprising the steps of:
weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 20 at%, V: 8 at%, Nb: 18 at%, Mo: 15 at%, Ta: 21 at%, W: 18at percent, the sum of the atomic percentages of Ti, V, Nb, Mo, Ta and W is 100 percent, and the purity of the raw materials is more than or equal to 99.99 percent.
Mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 25um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm so as to prevent the alloy powder from being oxidized. The laser power of the 3D printing equipment is set to be 330W, the scanning speed is 800mm/s, and the scanning interval is 70um, so that the high-toughness and high-entropy alloy forming material suitable for the high-temperature environment can be obtained.
The invention performs performance tests on examples 1-4 and comparative examples 1-3, and the test results are shown in Table 1.
TABLE 1 test Properties of high-toughness high-entropy alloy forming materials at different temperatures
From table 1, it can be seen that: the high-entropy alloy forming material obtained by determining the components and the content of the corresponding high-entropy alloy raw materials and combining the preparation process parameters of the SLM has the tensile strength of 1300-1550MPa, the yield strength of 920-1030MPa and the elongation of 20-28% in the 800 ℃ use environment; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%. The high-entropy alloy forming material has good toughness and matching property under a high-temperature use environment.
The foregoing examples are set forth to illustrate the present invention more clearly and should not be construed as limiting the scope of the present invention, which is intended to be limited thereby, and all such changes and modifications that can be made without departing from the scope of the present invention are intended to be within the scope of the present invention.
Claims (9)
1. A high-toughness high-entropy alloy for 3D printing is characterized in that the high-entropy alloy comprises the following raw materials in atomic percentage: ti: 17-25 at%, V: 8-15 at%, Nb: 11-18 at%, Mo: 7-15 at%, Ta: 20-25 at%, W: 15-18 at%, the sum of atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%.
2. The high toughness high entropy alloy for 3D printing according to claim 1, wherein atomic percentages of Ti, Nb, and Mo are 3: 2: (1-1.5).
3. A high-toughness high-entropy alloy for 3D printing as claimed in claim 2, wherein the forming material of the high-toughness high-entropy alloy for 3D printing has a tensile strength of 1300-1550MPa, a yield strength of 920-1030MPa and an elongation of 20-28% in an operating environment at 800 ℃; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%.
4. A preparation method of a high-toughness high-entropy alloy forming material comprises the following steps: weighing raw materials of the high-entropy alloy, wherein the content of the raw materials of the high-entropy alloy is as follows by atomic percentage: ti: 17-25 at%, V: 8-15 at%, Nb: 11-18 at%, Mo: 7-15 at%, Ta: 20-25 at%, W: 15-18 at%, the sum of atomic percentages of Ti, V, Nb, Mo, Ta and W is 100%, and the purity of the raw materials is more than or equal to 99.99%; mixing the raw materials, preparing into alloy powder, screening out the alloy powder with the diameter of 10-25um for SLM forming, putting the screened alloy powder into 3D printing equipment of an SLM, and controlling the oxygen content in the preparation process within 150ppm to prevent the alloy powder from being oxidized; setting the laser power of the 3D printing equipment to be 180-240W, the scanning speed to be 1000-1300mm/s and the scanning interval to be 20-50um, and obtaining the high-toughness high-entropy alloy forming material suitable for the high-temperature environment.
5. The method for preparing a high-toughness high-entropy alloy forming material according to claim 4, wherein the atomic percentages of Ti, Nb, and Mo are 3: 2: (1-1.5).
6. A method for preparing a high-toughness high-entropy alloy forming material according to claim 4 or 5, wherein the laser power is 200-210W.
7. A method for preparing a high-toughness high-entropy alloy forming material according to any one of claims 4 to 6, wherein the scanning speed is 1200-1250 mm/s.
8. A method for the preparation of a high toughness high entropy alloy forming material according to any one of claims 4 to 7, wherein the scanning interval is 25-30 um.
9. The preparation method of the high-toughness high-entropy alloy forming material as claimed in any one of claims 4 to 8, wherein the high-toughness high-entropy alloy forming material has a tensile strength of 1300-1550MPa, a yield strength of 920-1030MPa and an elongation of 20-28% in a use environment at 800 ℃; under the use environment of 1000 ℃, the tensile strength of the high-entropy alloy forming material is 1230-1480MPa, the yield strength is 880-960MPa, and the elongation is 32-41%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117230336A (en) * | 2023-09-19 | 2023-12-15 | 上海大学 | Method for preparing high-entropy alloy |
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| CN104308153A (en) * | 2014-10-27 | 2015-01-28 | 西安交通大学 | High-entropy alloy hot-end part manufacturing method of turbine engine on basis of selective laser melting |
| CN105950944A (en) * | 2016-06-29 | 2016-09-21 | 华南理工大学 | High-melting-point high-entropy alloy NbMoTaWVTi and preparation method thereof |
| KR20170027520A (en) * | 2015-09-02 | 2017-03-10 | 한국과학기술원 | Hight-entropy multioelement alloy with single phase and process for preparing the same |
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| CN104308153A (en) * | 2014-10-27 | 2015-01-28 | 西安交通大学 | High-entropy alloy hot-end part manufacturing method of turbine engine on basis of selective laser melting |
| KR20170027520A (en) * | 2015-09-02 | 2017-03-10 | 한국과학기술원 | Hight-entropy multioelement alloy with single phase and process for preparing the same |
| CN105950944A (en) * | 2016-06-29 | 2016-09-21 | 华南理工大学 | High-melting-point high-entropy alloy NbMoTaWVTi and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117230336A (en) * | 2023-09-19 | 2023-12-15 | 上海大学 | Method for preparing high-entropy alloy |
| CN117230336B (en) * | 2023-09-19 | 2024-05-03 | 上海大学 | Method for preparing high-entropy alloy |
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