CN115889794A - Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder - Google Patents
Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder Download PDFInfo
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- CN115889794A CN115889794A CN202211422519.XA CN202211422519A CN115889794A CN 115889794 A CN115889794 A CN 115889794A CN 202211422519 A CN202211422519 A CN 202211422519A CN 115889794 A CN115889794 A CN 115889794A
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- alloy powder
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- molybdenum
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000010146 3D printing Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- MTHLBYMFGWSRME-UHFFFAOYSA-N [Cr].[Co].[Mo] Chemical compound [Cr].[Co].[Mo] MTHLBYMFGWSRME-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 230000006698 induction Effects 0.000 claims abstract description 10
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000009692 water atomization Methods 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 2
- 238000005266 casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
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Classifications
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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 discloses a preparation method of low-cost spherical cobalt chromium molybdenum 3D printing powder, which comprises the following steps: (1) The cobalt-chromium-molybdenum metal raw material is vacuum smelted after being proportioned according to the components; (2) carrying out water atomization treatment to form alloy powder; (3) Alloy powder is charged into a furnace for negative pressure deoxidation, the furnace is vacuumized to below 10Pa at room temperature, hydrogen with the purity of more than 99.99 percent is introduced, the pressure of the hydrogen is kept at 0-1.5 MPa, then the furnace is slowly heated to 550-950 ℃, the temperature is kept for 5-20 hrs, the furnace is cooled to below 50 ℃ under the condition of continuously introducing the hydrogen, and the alloy powder is discharged; (4) And (4) carrying out radio frequency induction plasma spheroidization on the alloy powder treated in the step (3). According to the technical scheme, the oxygen is reduced by adopting a mode of introducing hydrogen under negative pressure, oxygen impurities in the alloy powder are reduced, the powder forming rate of the alloy powder is greatly improved, the yield can be finally realized to be more than 80%, and the production cost is greatly reduced.
Description
Technical Field
The invention relates to the technical field of 3D printing metal powder, in particular to a preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder.
Background
The existing preparation process of cobalt-chromium-molybdenum 3D printing powder comprises the steps of proportioning metal cobalt, chromium and molybdenum according to a certain proportion, carrying out vacuum melting, casting the mixture into a bar material, and carrying out gas atomization or electrode rotation by using the bar material.
Disclosure of Invention
The invention aims to provide a preparation method of spherical cobalt-chromium-molybdenum 3D printing powder with high yield and low cost.
The invention is realized by the following technical scheme in order to achieve the purpose:
a preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder comprises the following steps: (1) cobalt, chromium and molybdenum metal raw materials are proportioned and then vacuum smelted;
(2) Carrying out water atomization treatment to form alloy powder;
(3) Charging alloy powder into a furnace for negative pressure deoxidation, vacuumizing to below 10Pa at room temperature, introducing hydrogen with the purity of more than 99.99 percent, keeping the hydrogen pressure at 0-1.5 MPa, slowly heating to 550-950 ℃, preserving heat for 5-20 hrs, cooling to below 50 ℃ under the condition of continuously introducing hydrogen, and discharging;
(4) And (4) spheroidizing the alloy powder treated in the step (3) by radio frequency induction plasma.
Further, in the step (3), the hydrogen gas flow is introduced in a mode of downward inlet and upward outlet, which means that hydrogen enters the deoxidizing furnace from an opening at the lowest end of the deoxidizing furnace, sequentially flows through the alloy powder from bottom to top, and is discharged from the highest end of the deoxidizing furnace.
Further, in the step (1), the vacuum melting temperature is 1300-1600 ℃, the vacuum degree is not more than 0.1MPa, and the melting time is 2-3h.
Further, the volume ratio of the plasma mixed gas selected by implementing the radio frequency induction plasma spheroidization in the step (4) is 65-70 v% of argon and 30-35 v% of helium; the power of the radio frequency induction plasma spheroidization is 110-140 KW, the flow rate of the plasma mixed gas is 2-4L/min, and the powder feeding rate is 8-10 kg/h.
According to the technical scheme, the oxygen is reduced by introducing the hydrogen under the negative pressure, oxygen impurities in the alloy powder are reduced, the powder yield of the alloy powder is greatly improved, the yield can be finally increased to be more than 80%, and the production cost is greatly reduced.
Drawings
FIG. 1 is a microscopic magnified view of the alloy 3D printing powder of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, the preparation method of the low-cost spherical cobalt chromium molybdenum 3D printing powder of the invention comprises the following steps: (1) batching cobalt, chromium and molybdenum metal raw materials and then carrying out vacuum melting;
(2) Carrying out water atomization powder preparation treatment to form alloy powder;
(3) Charging alloy powder into a furnace for negative pressure deoxidation, vacuumizing to below 10Pa at room temperature, introducing hydrogen with the purity of more than 99.99 percent, keeping the hydrogen pressure at 0-1.5 MPa, slowly heating to 550-950 ℃, preserving heat for 5-20 hrs, cooling to below 50 ℃ under the condition of continuously introducing hydrogen, and discharging;
(4) And (4) carrying out radio frequency induction plasma spheroidization on the alloy powder treated in the step (3).
In the invention, oxygen in the alloy powder is removed by filling hydrogen under negative pressure, preferably, in the step (3), the hydrogen gas flow adopts a mode of downward inlet and upward outlet, that is, hydrogen enters the deoxidizing furnace from an opening at the lowest end of the deoxidizing furnace, sequentially flows through the alloy powder from bottom to top, and is then discharged from the uppermost end of the deoxidizing furnace. The impurity oxygen in the alloy powder reacts with the hydrogen at high temperature to form water vapor and sinks, but under the condition of negative pressure, the hydrogen flows in a mode of introducing from bottom to top and flowing out, so that the water vapor can take away the deoxidation reaction upwards to form water molecules, the water molecules are prevented from sinking to react with the formed alloy powder, and the powder forming effect and the powder forming rate of the alloy powder are obviously improved.
Preferably, the vacuum melting temperature in the step (1) is 1300-1600 ℃, the vacuum degree is not more than 0.1MPa, and the melting time is 2-3h. Further preferably, the melting temperature may be 1400 ℃ and 1500 ℃.
Preferably, the volume ratio of the plasma mixed gas selected by implementing the radio frequency induction plasma spheroidization in the step (4) is 65-70 v% of argon and 30-35 v% of helium; the power of the radio frequency induction plasma spheroidization is 110-140 KW, the flow rate of the plasma mixed gas is 2-4L/min, and the powder feeding rate is 8-10 kg/h.
The embodiments of the present invention are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading the present specification, but the present invention is protected by patent law within the scope of the appended claims.
Claims (4)
1. A preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder is characterized by comprising the following steps: (1) batching cobalt, chromium and molybdenum metal raw materials and then carrying out vacuum melting;
(2) Carrying out water atomization powder preparation treatment to form alloy powder;
(3) Charging alloy powder into a furnace for negative pressure deoxidation, vacuumizing to below 10Pa at room temperature, introducing hydrogen with the purity of more than 99.99 percent, keeping the hydrogen pressure at 0-1.5 MPa, slowly heating to 550-950 ℃, preserving heat for 5-20 hrs, cooling to below 50 ℃ under the condition of continuously introducing hydrogen, and discharging;
(4) And (4) carrying out radio frequency induction plasma spheroidization on the alloy powder treated in the step (3).
2. The preparation method of the low-cost spherical cobalt chromium molybdenum 3D printing powder as claimed in claim 1, wherein in the step (3), the hydrogen gas flow is introduced in a downward-in-upward-out mode, specifically, the hydrogen gas enters the deoxidizing furnace from an opening at the lowest end of the deoxidizing furnace, flows through the alloy powder from bottom to top in sequence, and is discharged from the highest end of the deoxidizing furnace.
3. The preparation method of the low-cost spherical cobalt chromium molybdenum 3D printing powder according to claim 1, wherein the vacuum melting temperature in the step (1) is 1300-1600 ℃, the vacuum degree is not more than 0.1MPa, and the melting time is 2-3h.
4. The preparation method of the low-cost spherical cobalt chromium molybdenum 3D printing powder according to claim 1, wherein the volume ratio of the plasma mixed gas selected in the step (4) for implementing the radio frequency induction plasma spheroidization is 65-70 v% of argon and 30-35 v% of helium; the spheroidization power of the radio frequency induction plasma is 110-140 KW, the flow rate of the plasma mixed gas is 2-4L/min, and the powder feeding rate is 8-10 kg/h.
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| CN202211422519.XA CN115889794A (en) | 2022-11-14 | 2022-11-14 | Preparation method of low-cost spherical cobalt-chromium-molybdenum 3D printing powder |
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|---|---|---|---|---|
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| CN103752836A (en) * | 2014-01-16 | 2014-04-30 | 北京科技大学 | Method for manufacturing spherical niobium and titanium-based alloy powder with small particle size |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
| CN107598151A (en) * | 2017-08-24 | 2018-01-19 | 成都科宁达材料有限公司 | A kind of dental 3D printing vitallium powder containing Ta and preparation method thereof |
| CN109570521A (en) * | 2018-12-24 | 2019-04-05 | 南通金源智能技术有限公司 | The method that plasma spheroidization prepares metal powder |
| CN112846195A (en) * | 2021-01-08 | 2021-05-28 | 广东省科学院材料与加工研究所 | Titanium-tantalum alloy powder for additive manufacturing and preparation method thereof |
| CN113134605A (en) * | 2021-04-19 | 2021-07-20 | 山东理工大学 | Preparation method of plasma spheroidizing deoxidation 3D printing metal powder |
| CN114888281A (en) * | 2022-06-08 | 2022-08-12 | 华材(山东)新材料有限公司 | Production method of spherical hafnium powder |
| CN115194161A (en) * | 2022-08-08 | 2022-10-18 | 湖南宏承新材料科技有限公司 | Production process of high-purity tantalum powder |
-
2022
- 2022-11-14 CN CN202211422519.XA patent/CN115889794A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011082595A1 (en) * | 2010-01-05 | 2011-07-14 | 北京科技大学 | Method for preparing superfine spherical neodymium-iron-boron powder |
| CN103752836A (en) * | 2014-01-16 | 2014-04-30 | 北京科技大学 | Method for manufacturing spherical niobium and titanium-based alloy powder with small particle size |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
| CN107598151A (en) * | 2017-08-24 | 2018-01-19 | 成都科宁达材料有限公司 | A kind of dental 3D printing vitallium powder containing Ta and preparation method thereof |
| CN109570521A (en) * | 2018-12-24 | 2019-04-05 | 南通金源智能技术有限公司 | The method that plasma spheroidization prepares metal powder |
| CN112846195A (en) * | 2021-01-08 | 2021-05-28 | 广东省科学院材料与加工研究所 | Titanium-tantalum alloy powder for additive manufacturing and preparation method thereof |
| CN113134605A (en) * | 2021-04-19 | 2021-07-20 | 山东理工大学 | Preparation method of plasma spheroidizing deoxidation 3D printing metal powder |
| CN114888281A (en) * | 2022-06-08 | 2022-08-12 | 华材(山东)新材料有限公司 | Production method of spherical hafnium powder |
| CN115194161A (en) * | 2022-08-08 | 2022-10-18 | 湖南宏承新材料科技有限公司 | Production process of high-purity tantalum powder |
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