CN115041699A - Production method of spherical zirconium powder for 3D printing - Google Patents
Production method of spherical zirconium powder for 3D printing Download PDFInfo
- Publication number
- CN115041699A CN115041699A CN202210863305.XA CN202210863305A CN115041699A CN 115041699 A CN115041699 A CN 115041699A CN 202210863305 A CN202210863305 A CN 202210863305A CN 115041699 A CN115041699 A CN 115041699A
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- China
- Prior art keywords
- powder
- zirconium
- zirconium tetrachloride
- printing
- spherical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000010146 3D printing Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 56
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 46
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000006698 induction Effects 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000010923 batch production Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- 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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a production method of spherical zirconium powder for 3D printing, and relates to the technical field of 3D printing. The production method of the spherical zirconium powder for 3D printing comprises the following steps; s1, putting zirconium tetrachloride powder into a container for later use; s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder; s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 80-100 ℃, and cooling for later use; s4, filtering the zirconium tetrachloride powder in the S3 again; s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device. The method takes zirconium tetrachloride powder as a raw material, has abundant raw material amount, is suitable for batch production, can meet the requirement of industry on spherical zirconium, uses the coaxial embedded induction plasma spheroidizing device, has the center temperature of a plasma zone as high as 10000 ℃, rapidly decomposes and spheroidizes the zirconium tetrachloride at the high temperature, and greatly improves the spheroidizing efficiency.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a production method of spherical zirconium powder for 3D printing.
Background
Zirconium is a rare metal, has high melting point, good plasticity and excellent corrosion resistance, has the characteristics of high density, high activity, high volume heat value, small specific heat capacity and the like, has better corrosion resistance than titanium, is expected to replace titanium alloy in the field of 3D printing, and is widely applied in the fields of ocean engineering, biological medicine, chemical engineering and the like.
For high-performance metal 3D components, metal powder with good sphericity, high spheroidization rate and good fluidity is needed, 3D printing and powder paving operations are convenient, and in view of the high melting point (1852 ℃) of zirconium, conventional spheroidization methods such as an air atomization method and a plasma method are low in efficiency, difficult to realize high-efficiency production, and unsatisfactory in sphericity and spheroidization rate.
The document search of the prior art finds that Chinese patent with publication number CN113909479A discloses a method for preparing superfine spherical zirconium powder capable of realizing granularity classification, and the method has the following defects: the steps are complicated and the efficiency is low. Through literature search, the inventor finds that the "crucible-free smelting gas atomization technology for preparing high-purity spherical zirconium powder" is published in rare metals (2018, 8 th stage, 864-868) by the slaying-goddess et al, and the specific method comprises the following steps: the method is characterized in that a zirconium rod is used as a raw material, and the high-purity spherical zirconium powder is successfully prepared by adopting independently designed crucible-free smelting gas atomization equipment, so that the yield of fine powder can reach 40-50% only by strictly controlling the feeding speed and the atomization pressure, the batch production cannot be achieved, and the industrial requirement on the spherical zirconium powder cannot be met.
By searching the existing patents and literatures, the report of producing the spherical zirconium powder by the coaxial embedded induction plasma method technology is not found.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a production method of spherical zirconium powder for 3D printing, and solves the problems that batch production cannot be achieved and the industrial requirement on the spherical zirconium powder cannot be met.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a production method of spherical zirconium powder for 3D printing comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 80-100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
Preferably, the operation parameters in S5 are: the power is 200KW, the gas flow rate of the argon-hydrogen plasma is 0.5-0.8 m/h, and the gas flow rate for argon powder transport is 0.10-0.18 m/h.
Preferably, the argon-hydrogen plasma gas comprises 95v% argon and 5v% hydrogen.
(III) advantageous effects
The invention provides a production method of spherical zirconium powder for 3D printing. The method has the following beneficial effects:
1. compared with the prior art, the zirconium tetrachloride powder is used as the raw material, the raw material amount is rich, the method is suitable for batch production, and the requirement of the industry on spherical zirconium can be met.
2. Compared with the prior art, the invention uses the coaxial embedded induction plasma spheroidizing device, the central temperature of the plasma zone is up to 10000 ℃, and the zirconium tetrachloride is rapidly decomposed and spheroidized at the high temperature, thereby greatly improving the spheroidizing efficiency.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
The first embodiment is as follows:
the embodiment of the invention provides a production method of spherical zirconium powder for 3D printing, which comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
The operation parameter is 400KW, argon-hydrogen plasma gas flow 0.8 m/h, argon-hydrogen plasma gas contains argon 95v%, hydrogen 5v%, argon powder feeding gas flow rate is 0.10 m/h, under the plasma high temperature condition, the obtained powder is collected, and spherical zirconium powder of 15-53um is obtained.
The spheroidization rate of spherical zirconium obtained was found to be 99%, and the Hall flow rate was 24.01 (s/50 g).
Example two:
the embodiment of the invention provides a production method of spherical zirconium powder for 3D printing, which comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
Power 300KW, argon-hydrogen plasma gas flow 0.8 m/h, argon-hydrogen plasma gas contain argon 95v%, hydrogen 5v%, argon powder feeding gas flow rate is 0.18 m/h, under the plasma high temperature condition, collect the gained powder, obtain 15-53um spherical zirconium powder.
The spherical zirconium spheroidization rate was found to be 96% and the Hall flow rate was found to be 26.21 (s/50 g).
Example three:
the embodiment of the invention provides a production method of spherical zirconium powder for 3D printing, which comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
Power 200KW, argon-hydrogen plasma gas flow 0.5 m/h, argon-hydrogen plasma gas contain argon 95v%, hydrogen 5v%, argon powder feeding gas flow rate is 0.15 m/h, and under the plasma high temperature condition, the obtained powder is collected to obtain 15-53um spherical zirconium powder.
The spheroidization rate of spherical zirconium obtained was found to be 95% and the Hall flow rate was found to be 27.78 (s/50 g).
Example four
The embodiment of the invention provides a production method of spherical zirconium powder for 3D printing, which comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
Power 200KW, argon-hydrogen plasma gas flow 0.5 m/h, argon-hydrogen plasma gas contain argon 95v%, hydrogen 5v%, argon powder feeding gas flow rate is 0.10 m/h, and under the plasma high-temperature condition, the obtained powder is collected to obtain 15-53um spherical zirconium powder.
The spheroidization rate of spherical zirconium obtained was found to be 93% and the Hall flow rate was found to be 28.35 (s/50 g).
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A production method of spherical zirconium powder for 3D printing is characterized in that; the method comprises the following steps:
s1, putting zirconium tetrachloride powder into a container for later use;
s2, filtering the zirconium tetrachloride powder for three times to remove large-particle impurities in the zirconium tetrachloride powder;
s3, drying the zirconium tetrachloride powder in the S2 at the temperature of 80-100 ℃, and cooling for later use;
s4, filtering the zirconium tetrachloride powder in the S3 again;
s5, putting the zirconium tetrachloride powder with the granularity of 25um-70um in the S4 into a coaxial embedded induction plasma spheroidizing device, and setting the operation parameters of the plasma to obtain a final product.
2. The method for producing spherical zirconium powder for 3D printing according to claim 1, wherein: the operation parameters in S5 are: 400KW in power of 200-.
3. The method for producing spherical zirconium powder for 3D printing according to claim 2, wherein: the argon-hydrogen plasma gas contained 95v% argon and 5v% hydrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210863305.XA CN115041699A (en) | 2022-07-22 | 2022-07-22 | Production method of spherical zirconium powder for 3D printing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210863305.XA CN115041699A (en) | 2022-07-22 | 2022-07-22 | Production method of spherical zirconium powder for 3D printing |
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| Publication Number | Publication Date |
|---|---|
| CN115041699A true CN115041699A (en) | 2022-09-13 |
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| CN202210863305.XA Pending CN115041699A (en) | 2022-07-22 | 2022-07-22 | Production method of spherical zirconium powder for 3D printing |
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Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB628147A (en) * | 1945-02-17 | 1949-08-23 | William Justin Kroll | Improvements in the production of anhydrous zirconium tetrachloride and in the production of zirconium therefrom |
| CH595286A5 (en) * | 1975-08-26 | 1978-02-15 | Konstantin Gavrilovich Marin | |
| GB8303266D0 (en) * | 1982-06-10 | 1983-03-09 | Westinghouse Electric Corp | Process for upgrading metal powder |
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2022
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