CN113976918B - Remelting process for metal powder return material in additive manufacturing - Google Patents
Remelting process for metal powder return material in additive manufacturing Download PDFInfo
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- CN113976918B CN113976918B CN202110866639.8A CN202110866639A CN113976918B CN 113976918 B CN113976918 B CN 113976918B CN 202110866639 A CN202110866639 A CN 202110866639A CN 113976918 B CN113976918 B CN 113976918B
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/70—Recycling
- B22F10/73—Recycling of powder
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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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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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
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Abstract
The invention relates to the field of chemical industry, and discloses a remelting process for metal powder return materials in additive manufacturing, wherein the metal powder return materials are made into briquettes; preheating and degassing the pressing block at the temperature of 200 to 600 ℃ under the vacuum condition of-0.05 to-0.1 MPa, then heating to the temperature of 700 to 1200 ℃ under the protective atmosphere of 0.01MPa to 0.2MPa, and sintering for 1 to 4 hours, and cooling to obtain a sintering block; sampling and checking the oxygen and nitrogen contents of the sintered blocks; and (3) preparing materials according to the components of the metal powder return material and the oxygen and nitrogen contents of the sintered blocks by adopting a return ratio of 30-70%, and smelting by adopting a standard master alloy vacuum smelting process to prepare the master alloy bar. The process solves the problem of residual powder recovery and remelting generated by an additive manufacturing powder manufacturing plant, and by the process, the residual powder return ratio of the high-temperature alloy can reach 30 to 70 percent, and meanwhile, the application of the master alloy in the additive manufacturing field is not influenced.
Description
Technical Field
The invention relates to the technical field of powder preparation by refining and additive manufacturing of high-temperature alloys and other special non-ferrous metal alloys, in particular to a remelting process for a metal powder return material for additive manufacturing.
Background
The additive manufacturing technology develops rapidly in recent years, thereby driving the increase of the powder manufacturing technology and production. The yield of fine powder in the conventional powder preparation method is generally 35%. Therefore, the resulting particle size does not meet the 3D printed metal powder, mostly without good utilization methods. The direct return of the remaining powder to the master alloy smelting process also has a plurality of problems: loss in the treatment process, difficult molding of the cold-pressed block or high-temperature pulverization, and equipment damage and production safety risk caused by the fact that powder is collected by a vacuum system. Therefore, the residual powder produced by the powder mill facing the additive manufacturing industry does not have a mature recycling process at present, and a large amount of residual powder inventory is accumulated by part of manufacturers. In addition, due to the powder making process such as gas atomization powder making, plasma rotating electrode and the like, the content of harmful gas elements such as oxygen and nitrogen in the high-temperature master alloy is increased by a certain amount (for example, from 40ppm to more than 100 ppm) in the powder making process, so that the amount (return ratio) of the returned remelting alloy is limited.
Disclosure of Invention
The invention aims to: aiming at the problems in the prior art, the invention provides an additive manufacturing metal powder return material remelting process, which solves the problem of residual powder recovery remelting generated in an additive manufacturing powder making plant, and by utilizing the process scheme provided by the invention, the residual powder returning ratio of high-temperature alloys (such as GH3536, GH3625 and GH 4169) can reach 30 to 70 percent, and the application of the master alloy in the field of additive manufacturing is not influenced.
The technical scheme is as follows: the invention provides an additive manufacturing metal powder return material remelting process, which comprises the following steps of: s1: preparing metal powder return materials into briquettes; s2: preheating and degassing the pressing block at the temperature of 200 to 600 ℃ under the vacuum condition of-0.05 to-0.1 MPa, then heating to the temperature of 700 to 1200 ℃ under the protective atmosphere of 0.01to 0.2MPa for sintering for 1 to 4 hours, and then cooling to obtain a sintering block; s3: sampling and checking the oxygen and nitrogen contents of the sintered blocks; s4: if the nitrogen content of the sintered blocks is less than 80ppm, blending according to the components of the metal powder return materials and the oxygen and nitrogen contents of the sintered blocks by adopting a return ratio of 30-70%, and smelting by adopting a standard master alloy vacuum smelting process to prepare master alloy bars; if the nitrogen content of the sintered blocks is larger than 80ppm in S3, the sintered blocks are subjected to pre-smelting degassing through a standard master alloy vacuum smelting process, cast into bars, then mixed according to the components of the metal powder return materials and the oxygen and nitrogen contents of the sintered blocks by adopting a return ratio of 30-70%, and smelted through a standard master alloy vacuum smelting process to prepare master alloy bars. So as to ensure that the chemical components and the mechanical properties of the final master alloy product are not influenced under the condition of using the metal powder return material.
Further, in the step S1, if the metal powder return material is not well formed in the briquetting process or the strength after forming is not enough, the metal powder return material and an additive material accounting for 5-15% of the weight of the metal powder return material are mixed to prepare a briquetting; the additive is main metal powder of the master alloy bar. In the process of cold pressing the metal powder return material into briquettes, the use or non-use of additives is determined according to the briquetting strength of the metal powder return material, generally, the briquetting is not good mainly because the alloy material is not easy to deform or the split particle size distribution range is narrow (such as more fine powder); the selected additive components are compatible with the main components of the original alloy, and the particle size of the additive components increases the particle size distribution range of the mixed powder.
Preferably, in S4, the metal powder returning material, the additive material and the sintered cake are mixed according to their oxygen and nitrogen contents.
Preferably, the pressing block is a cylindrical pressing block with the diameter of 50-100mm and the height of 30-70mm, and the pressure in the pressing forming process is 5-20MPa. The formed compact should be able to remain free of chipping or powdering during manual handling.
Preferably, the protective atmosphere is 100% argon or argon-hydrogen mixed gas mixed with 5% -20% hydrogen by volume.
Has the advantages that: in the invention, because the returned residual powder of the additive manufacturing powder making process has fine granularity, and most of the master alloy components contain Al, ti, cr and other oxygen-philic elements, the metal powder returned material is firstly made into a briquetting, then the briquetting is preheated and degassed under the environment with the vacuum pressure ranging from-0.05 MPa to-0.1 MPa and the temperature ranging from 200 ℃ to 600 ℃ to remove the residual air in the briquetting, the preheating and degassing temperature is set to be not more than 600 ℃ to ensure that the briquetting has sufficient expansion, and simultaneously avoid a possible chemical reaction high-temperature region, then the briquetting is sintered for 1 to 4 hours at 700 ℃ to 1200 ℃ under the argon protection atmosphere to soften or melt the metal structure grain boundary, so that the metal powder particles are bonded together, finally the temperature is reduced and cooled to ensure that the briquetting has sufficient strength and is not further pulverized, and the cooling process also adopts vacuum or atmosphere protection; the oxygen and nitrogen contents in the sintered blocks obtained after preheating, degassing, sintering and cooling are controlled within 80ppm; at the moment, the sintering blocks are mixed according to the return ratio of 30-70% and the components of the metal powder return materials and the oxygen and nitrogen contents of the sintering blocks, and a standard master alloy vacuum melting process is adopted for melting to prepare master alloy bars.
Compared with the prior art, the process has the following advantages:
(1) The invention does not need to use additives containing carbon or other harmful impurities for briquetting and forming, thereby ensuring the purity of the final master alloy product.
(2) The process carries out sintering pretreatment on the metal powder return material in a reducing atmosphere or vacuum and removes partial oxygen and nitrogen gas elements, so that the return powder material can be safely and effectively used as an adding raw material in the vacuum induction melting process of the high-temperature alloy of the same product.
The invention solves the problem of recovery and remelting of residual powder generated in an additive manufacturing powder manufacturing plant. By utilizing the technical scheme provided by the invention, the residual powder return ratio of high-temperature alloys (such as GH3536, GH3625 and GH 4169) can reach 30-70%, and the application of the master alloy in the field of additive manufacturing is not influenced.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Embodiment 1:
uniformly mixing the high-temperature alloy GH3536 return powder and electrolytic nickel powder accounting for 8 percent of the weight of the high-temperature alloy GH3536 return powder into mixed powder.
And (3) preparing the mixed powder into a cylindrical briquette with the diameter of 80mm and the height of 50mm by using a hydraulic machine under the working pressure of 15 MPa.
Putting the pressed block into a sintering furnace, preheating and degassing at 500 ℃ under the vacuum condition of-0.08 MPa, filling 100% argon to 0.05-0.2MPa gauge pressure, and then heating to 950 ℃ for sintering for 3 hours. And then cooling to obtain the sintered block.
The sintered cake was checked by sampling for nitrogen content of less than 80ppm.
The method comprises the steps of proportioning according to the components of GH3536 return materials, the components of electrolytic nickel powder and the oxygen and nitrogen contents of sintered blocks by adopting a return ratio of 30%, smelting in a vacuum induction furnace by adopting a standard master alloy vacuum smelting process to prepare a GH3536 master alloy bar applied to additive manufacturing, and detecting the oxygen and nitrogen contents in the GH4169 master alloy bar.
Embodiment 2:
this embodiment is substantially the same as embodiment 1, except that in this embodiment, a return ratio of 70% is adopted in the last vacuum melting step.
Otherwise, this embodiment is identical to embodiment 1, and will not be described herein.
Embodiment 3:
the high-temperature alloy GH4169 return powder and 8 wt% of reduction method iron powder are uniformly mixed.
And (3) preparing the mixed powder into a cylindrical briquette with the diameter of 80mm and the height of 50mm by using a hydraulic machine under the working pressure of 15 MPa.
And putting the pressed block into a sintering furnace, preheating and degassing at 500 ℃ under the vacuum condition of-0.08 MPa, then filling hydrogen and argon mixed protective gas containing 8 percent of hydrogen to the gauge pressure of 0.05-0.2MPa, and heating to 1100 ℃ for sintering for 3 hours. Then cooling to below 400 ℃ under the same protective atmosphere, and closing hydrogen.
Sampling and checking that the nitrogen content of the sintered cake is more than 80ppm;
100% of the obtained sintered lump material is used for melting pretreatment in a vacuum induction furnace, the melting process is the same as that of a standard product vacuum melting process, and the sintered lump material is cast into a rod, analyzed for all components and then used as a return raw material for product melting.
The method comprises the steps of proportioning according to the components of GH4169 return materials, the components of reduction iron powder and the oxygen and nitrogen contents of sinter blocks by adopting a return ratio of 30%, smelting in a vacuum induction furnace by adopting a standard master alloy vacuum smelting process to prepare a GH4169 master alloy bar applied to additive manufacturing, and detecting the oxygen and nitrogen contents in the GH4169 master alloy bar.
Embodiment 4:
this embodiment is substantially the same as embodiment 3, except that in this embodiment, a return ratio of 70% is adopted in the final vacuum melting step.
Otherwise, this embodiment is completely the same as embodiment 3, and will not be described herein.
Table 1 below shows the oxygen and nitrogen gas contents of the master alloy rods of the two superalloys of embodiments 1 to 4 using different powder return ratios:
TABLE 1
As can be seen from Table 1, by utilizing the process scheme provided by the invention, the residual powder return ratio of the high-temperature alloy (such as GH3536 and GH 4169) can reach 30-70%, and the application of the master alloy in the field of additive manufacturing is not influenced.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. A remelting process for manufacturing metal powder returns in an additive mode is characterized by comprising the following steps:
s1: cold pressing the metal powder returning charge into a pressing block, wherein the strength of the pressing block is ensured not to be cracked or pulverized in the manual carrying process;
s2: preheating and degassing the pressing block at the temperature of 200 to 600 ℃ under the vacuum condition of-0.05 to-0.1 MPa, then heating to the temperature of 700 to 1200 ℃ for sintering for 1 to 4 hours under the protective atmosphere with the pressure of 0.01MPa to 0.2MPa, and then cooling to obtain a sintering block;
s3: sampling and checking the oxygen and nitrogen contents of the sintered blocks;
s4: if the nitrogen content of the sintered blocks is less than 80ppm in the S3 test, blending according to the components of the metal powder return material and the oxygen and nitrogen contents of the sintered blocks by adopting a return ratio of 30-70%, and smelting by adopting a standard master alloy vacuum smelting process to prepare a master alloy bar;
and if the nitrogen content of the sintered blocks is greater than 80ppm in the S3 test, pre-smelting and degassing the sintered blocks by a standard master alloy vacuum smelting process, casting the sintered blocks into bars, then proportioning the bars according to the components of the metal powder return materials and the oxygen and nitrogen contents of the sintered blocks by adopting a return ratio of 30-70%, and smelting the bars by adopting a standard master alloy vacuum smelting process to prepare the master alloy bars.
2. The additive manufacturing metal powder return remelting process of claim 1,
in the S1, if the metal powder return material is not well formed in the briquetting process or the strength after forming is not enough, mixing the metal powder return material with an additive accounting for 5-15% of the weight of the metal powder return material to prepare a briquetting; the additive is main metal powder of the master alloy bar.
3. The additive manufacturing metal powder return remelting process according to claim 2, wherein in S4, the metal powder return is formulated according to the composition of the metal powder return, the composition of the additive, and the oxygen and nitrogen contents of the agglomerates.
4. The additive manufacturing metal powder return remelting process according to any one of claims 1 to 3, wherein the pressing block is a cylindrical pressing block with a diameter of 50 to 100mm and a height of 30 to 70mm, the pressure during the pressing and cold forming process is 5 to 20MPa, and the strength of the pressing block is ensured not to be cracked or pulverized during manual carrying.
5. The additive manufactured metal powder return remelting process according to any one of claims 1 to 3, wherein the protective atmosphere is 100% argon or an argon-hydrogen mixed gas mixed with 5% to 20% hydrogen by volume fraction.
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| CN114749673A (en) * | 2022-03-29 | 2022-07-15 | 中国航发北京航空材料研究院 | Method for preparing powder by recycling high-temperature alloy coarse powder return material |
| CN115852186B (en) * | 2022-12-21 | 2023-10-27 | 四川钢研高纳锻造有限责任公司 | Method for refining carbonitride in GH4169 alloy by controlling addition amount of return material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4251266A (en) * | 1978-10-25 | 1981-02-17 | Uddeholms Aktiebolag | Method for taking care of metallic waste products by remelting |
| CN101440436A (en) * | 2007-11-21 | 2009-05-27 | 中国科学院金属研究所 | Purified smelting technique for high-temperature superalloy |
| CN107617749A (en) * | 2017-08-30 | 2018-01-23 | 兰州空间技术物理研究所 | A kind of method that spherical powder is prepared using TC4 titanium alloy scraps |
| CN110106374A (en) * | 2018-12-22 | 2019-08-09 | 北京航空航天大学 | A method of high-purity high temperature alloy is prepared using material is returned |
| CN112746177A (en) * | 2020-12-28 | 2021-05-04 | 大连理工大学 | Method for refining and purifying high-temperature alloy return material by using electron beams |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4251266A (en) * | 1978-10-25 | 1981-02-17 | Uddeholms Aktiebolag | Method for taking care of metallic waste products by remelting |
| CN101440436A (en) * | 2007-11-21 | 2009-05-27 | 中国科学院金属研究所 | Purified smelting technique for high-temperature superalloy |
| CN107617749A (en) * | 2017-08-30 | 2018-01-23 | 兰州空间技术物理研究所 | A kind of method that spherical powder is prepared using TC4 titanium alloy scraps |
| CN110106374A (en) * | 2018-12-22 | 2019-08-09 | 北京航空航天大学 | A method of high-purity high temperature alloy is prepared using material is returned |
| CN112746177A (en) * | 2020-12-28 | 2021-05-04 | 大连理工大学 | Method for refining and purifying high-temperature alloy return material by using electron beams |
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