CN113770366A - Method for preparing refractory metal powder for 3D printing - Google Patents
Method for preparing refractory metal powder for 3D printing Download PDFInfo
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- CN113770366A CN113770366A CN202010524799.XA CN202010524799A CN113770366A CN 113770366 A CN113770366 A CN 113770366A CN 202010524799 A CN202010524799 A CN 202010524799A CN 113770366 A CN113770366 A CN 113770366A
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- refractory metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention provides a method for preparing refractory metal powder for 3D printing, which comprises the following steps: (1) preparing materials: adding refractory metal powder into a ball milling tank, and adding a chemical reagent according to the characteristics of the refractory metal powder; (2) ball milling: performing ball milling to obtain ball-milled refractory metal powder; (3) cleaning: cleaning the ball-milled refractory metal powder, and removing a chemical reagent to obtain cleaned refractory metal powder; (4) drying: and drying the cleaned refractory metal powder. The method adopts a ball milling mode to ball mill the refractory metal powder, adds specific chemical reagents according to different refractory metal powder characteristics, then cleans, dries and screens the ball-milled powder, and then obtains the refractory metal 3D printing powder with good sphericity and good fluidity.
Description
Technical Field
The invention belongs to the field of refractory metal spherical powder for 3D printing, and particularly relates to a method for preparing refractory metal powder for 3D printing.
Background
Refractory metal 3D printing powder is the raw materials that refractory metal 3D printed, generally has the advantage that mobility is good, sphericity is high. However, because the melting point of the refractory metal is generally high, the conventional refractory metal 3D printing powder is usually manufactured in a plasma spheroidization mode, and although the refractory metal spherical powder prepared by the method has high sphericity and good fluidity, the refractory metal 3D printing powder prepared by the method has low manufacturing efficiency and high cost due to the problems of high value of related equipment and manufacturing principle.
Therefore, it is an urgent problem to provide a method for preparing low-cost metal 3D printing powder.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing refractory metal 3D printing powder.
A method of preparing a refractory metal 3D printing powder comprising the steps of:
(1) preparing materials: adding refractory metal powder into a ball milling tank, and adding a chemical reagent according to the characteristics of the refractory metal powder;
(2) ball milling: performing ball milling to obtain ball-milled refractory metal powder;
(3) cleaning: cleaning the ball-milled refractory metal powder, and removing a chemical reagent to obtain cleaned refractory metal powder;
(4) drying: drying the cleaned refractory metal powder;
(5) screening: and screening the dried refractory metal powder.
Further, the refractory metal powder is alloy powder composed of one or more of tungsten, molybdenum, niobium, tantalum and zirconium, and the particle size of the refractory metal powder is 5-150 μm.
Further, the chemical agent means a chemical agent that can dissolve the refractory metal powder.
Further, the mass ratio of the refractory metal powder, the grinding balls in the ball mill pot and the chemical reagent is 10: 3: 1.
further, the ball milling means that the edges and corners of the powder particles are removed in a mechanical mode, the ball milling speed is 50rpm to 500rpm, and the ball milling time is 10min to 300 min.
Further, the step of cleaning the ball-milled refractory metal powder comprises the following steps:
and (3) stirring and rinsing the ball-milled refractory metal powder by using cleaning water, stirring and rinsing for 10min, pouring out old water, adding new cleaning water, and repeating for 5 times.
Further, the mass ratio of the ball-milled refractory metal powder to the washing water is 1: 0.5.
further, the washing water is a liquid evaporated without residue.
Further, the drying treatment is to dry the powder in a heating mode, wherein the drying time is 30-300 min, and the drying temperature is 120-200 ℃.
Further, the screening refers to screening the particle size of the dried refractory metal powder by using a screen or an air flow classification mode to obtain the required powder particle size;
and when the particle size of the dried refractory metal powder is 1000-2500 meshes, an airflow classification mode is adopted.
The method adopts a ball milling mode to ball mill the refractory metal powder, adds specific chemical reagents according to different refractory metal powder characteristics, then cleans, dries and screens the ball-milled powder, and then obtains the refractory metal 3D printing powder with good sphericity and good fluidity.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
Fig. 1 illustrates a method of preparing a refractory metal 3D printing powder according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method of preparing a refractory metal 3D printing powder comprising the steps of:
(1) ingredients
10kg of tungsten powder with the granularity of 300 meshes is filled into a ball milling tank, and chemical reagents are added according to the characteristics of the tungsten powder2O2：NaOH：H2O10: 1: 100, wherein the mass ratio of the tungsten powder, the grinding ball and the chemical reagent is 10: 3: 1.
(2) ball mill
Ball milling is carried out for 1h at the rotating speed of 200 r/min.
(3) Cleaning of
Pouring out the chemical reagent, adding deionized water into the powder subjected to ball milling for stirring and rinsing, wherein the mass ratio of the tungsten powder subjected to ball milling to the deionized water is 1: 0.5, stirring and rinsing for 10min, pouring out the old water, adding new deionized water, repeating for 5 times, and removing the chemical reagent.
(4) Drying by baking
And putting the cleaned tungsten powder into a vacuum drying oven, and drying at 150 ℃.
(5) Sieving
The dried tungsten powder was sieved with a 300 mesh sieve to obtain about 9.5kg of 300 mesh tungsten powder.
Example 2:
a method of preparing a refractory metal 3D printing powder comprising the steps of:
(1) ingredients
10kg of tungsten powder with the granularity of 400 meshes is filled into a ball milling tank, and the chemical reagent proportion is H2O2：NaOH：H2O ═ 8: 1.5: 100, the mass ratio of tungsten powder, grinding balls and chemical reagents is 10: 3: 1.
(2) ball mill
And ball milling for 2 hours at the rotating speed of 300 r/min.
(3) Cleaning of
Pouring out the chemical reagent, adding deionized water into the tungsten powder subjected to ball milling for stirring and rinsing, wherein the mass ratio of the tungsten powder subjected to ball milling to the deionized water is 1: 0.5, stirring and rinsing for 10min, pouring out the old water, adding new deionized water, repeating for 5 times, and removing the chemical reagent.
(4) Drying by baking
And putting the cleaned tungsten powder into a vacuum drying oven, and drying at 150 ℃.
(5) Sieving
The dried tungsten powder was sieved with a 400 mesh sieve to obtain about 9kg of 400 mesh tungsten powder.
Example 3:
a method of preparing a refractory metal 3D printing powder comprising the steps of:
(1) ingredients
10kg of tantalum powder with the granularity of 200 meshes is filled into a ball milling tank, and the chemical reagent proportion is H2O2：NaOH：H2O10: 1: 100, the mass ratio of tantalum powder to grinding ball to chemical reagent is 10: 3: 1.
(2) ball mill
Ball milling is carried out for 1h at the rotating speed of 200 r/min.
(3) Cleaning of
Pouring out the chemical reagent, adding deionized water into the ball-milled tantalum powder for stirring and rinsing, wherein the mass ratio of the powder to water is 1: 0.5, stirring and rinsing for 10min, pouring out the old water, adding new deionized water, repeating for 5 times, and removing the chemical reagent.
(4) Drying by baking
And (3) putting the cleaned tantalum powder into a vacuum drying oven, and drying at 150 ℃.
(5) Sieving
The dried tantalum powder was sieved through a 200 mesh sieve to obtain about 9.7kg of tantalum powder with a particle size of 200 mesh.
Illustratively, the dried refractory metal powder is sieved by air classification when the particle size is 1500 meshes.
The method adopts a ball milling mode to ball mill the refractory metal powder, adds specific chemical reagents according to different refractory metal powder characteristics, then cleans, dries and screens the ball-milled powder, and then obtains the refractory metal 3D printing powder with good sphericity and good fluidity.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing refractory metal powder for 3D printing is characterized by comprising the following steps:
(1) preparing materials: adding refractory metal powder into a ball milling tank, and adding a chemical reagent according to the characteristics of the refractory metal powder;
(2) ball milling: performing ball milling to obtain ball-milled refractory metal powder;
(3) cleaning: cleaning the ball-milled refractory metal powder, and removing a chemical reagent to obtain cleaned refractory metal powder;
(4) drying: drying the cleaned refractory metal powder;
(5) screening: and screening the dried refractory metal powder.
2. The method of making a refractory metal 3D printing powder of claim 1, wherein: the refractory metal powder is alloy powder consisting of one or more of tungsten, molybdenum, niobium, tantalum and zirconium, and the particle size of the refractory metal powder is in a range of 5-150 mu m.
3. The method of making a refractory metal 3D printing powder of claim 1, wherein: the chemical agent is a chemical agent that can dissolve the refractory metal powder.
4. A method of preparing a refractory metal 3D printing powder according to claim 1, 2 or 3, characterized in that: the mass ratio of the refractory metal powder to the grinding balls in the ball milling pot to the chemical reagent is 10: 3: 1.
5. the method of making a refractory metal 3D printing powder of claim 1, wherein: the ball milling is to remove the edges and corners of powder particles in a mechanical mode, the ball milling speed is 50-500 rpm, and the ball milling time is 10-300 min.
6. The method of making a refractory metal 3D printing powder of claim 1, wherein: the step of cleaning the ball-milled refractory metal powder comprises the following steps:
and (3) stirring and rinsing the ball-milled refractory metal powder by using cleaning water, stirring and rinsing for 10min, pouring out old water, adding new cleaning water, and repeating for 5 times.
7. The method of making a refractory metal 3D printing powder of claim 6, wherein: the mass ratio of the ball-milled refractory metal powder to the cleaning water is 1: 0.5.
8. the method of making a refractory metal 3D printing powder of claim 1, wherein: the washing water is liquid which is evaporated without residue.
9. The method of making a refractory metal 3D printing powder of claim 1, wherein: the drying treatment is to dry the powder in a heating mode, wherein the drying time is 30-300 min, and the drying temperature is 120-200 ℃.
10. The method of making a refractory metal 3D printing powder of claim 1, wherein: the screening refers to screening the particle size of the dried refractory metal powder by adopting a screen or an air flow classification mode to obtain the required powder particle size;
and when the particle size of the dried refractory metal powder is 1000-2500 meshes, an airflow classification mode is adopted.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010524799.XA CN113770366A (en) | 2020-06-10 | 2020-06-10 | Method for preparing refractory metal powder for 3D printing |
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| CN202010524799.XA CN113770366A (en) | 2020-06-10 | 2020-06-10 | Method for preparing refractory metal powder for 3D printing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192793A (en) * | 2021-12-28 | 2022-03-18 | 河北京东管业有限公司 | Spheroidizing process for refractory metal powder |
Citations (5)
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| CN1433346A (en) * | 2000-04-24 | 2003-07-30 | 昭和电工株式会社 | Nobium powder, sintered compact thereof and capacitor |
| US20080230090A1 (en) * | 2007-02-15 | 2008-09-25 | Mclaughlin David F | Removal of niobium second phase particle deposits from pickled zirconium-niobium alloys |
| CN105834437A (en) * | 2016-05-16 | 2016-08-10 | 唐建中 | Preparing method of 3D printing metal powder |
| CN106735254A (en) * | 2016-12-28 | 2017-05-31 | 宁夏东方钽业股份有限公司 | A kind of metal dust and its preparation method and application |
| CN108637264A (en) * | 2018-06-05 | 2018-10-12 | 广东省材料与加工研究所 | A kind of ball mill improves the 3D printing method of metal powder mobility and 3D printing metal powder |
-
2020
- 2020-06-10 CN CN202010524799.XA patent/CN113770366A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1433346A (en) * | 2000-04-24 | 2003-07-30 | 昭和电工株式会社 | Nobium powder, sintered compact thereof and capacitor |
| US20080230090A1 (en) * | 2007-02-15 | 2008-09-25 | Mclaughlin David F | Removal of niobium second phase particle deposits from pickled zirconium-niobium alloys |
| CN105834437A (en) * | 2016-05-16 | 2016-08-10 | 唐建中 | Preparing method of 3D printing metal powder |
| CN106735254A (en) * | 2016-12-28 | 2017-05-31 | 宁夏东方钽业股份有限公司 | A kind of metal dust and its preparation method and application |
| CN108637264A (en) * | 2018-06-05 | 2018-10-12 | 广东省材料与加工研究所 | A kind of ball mill improves the 3D printing method of metal powder mobility and 3D printing metal powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192793A (en) * | 2021-12-28 | 2022-03-18 | 河北京东管业有限公司 | Spheroidizing process for refractory metal powder |
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Effective date of registration: 20220225 Address after: 100081 No. 76 South College Road, Beijing, Haidian District Applicant after: ADVANCED TECHNOLOGY & MATERIALS Co.,Ltd. Applicant after: ATTL ADVANCED MATERIALS Co.,Ltd. Applicant after: Aetna Tianlong (Beijing) tungsten molybdenum Technology Co.,Ltd. Address before: 100081 No. 76 South College Road, Beijing, Haidian District Applicant before: ADVANCED TECHNOLOGY & MATERIALS Co.,Ltd. Applicant before: Antai Tianlong tungsten molybdenum Technology Co., Ltd |