CN115007851A - Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method - Google Patents
Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method Download PDFInfo
- Publication number
- CN115007851A CN115007851A CN202210697315.0A CN202210697315A CN115007851A CN 115007851 A CN115007851 A CN 115007851A CN 202210697315 A CN202210697315 A CN 202210697315A CN 115007851 A CN115007851 A CN 115007851A
- Authority
- CN
- China
- Prior art keywords
- powder
- focusing mirror
- beam focusing
- laser
- ruthenium
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 127
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 66
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000010146 3D printing Methods 0.000 title claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 28
- 238000005507 spraying Methods 0.000 claims abstract description 26
- 150000003303 ruthenium Chemical class 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims description 38
- 239000000498 cooling water Substances 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000007664 blowing Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 239000012798 spherical particle Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- JDNQPKBFOBQRBN-UHFFFAOYSA-N ruthenium monohydride Chemical compound [RuH] JDNQPKBFOBQRBN-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 8
- 229920005862 polyol Polymers 0.000 description 8
- 150000003077 polyols Chemical class 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000013332 literature search Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Images
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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a device and a method for producing superfine spherical ruthenium powder for 3D printing by a one-step method, wherein the device comprises a high-pressure powder spraying device and a frame, the high-pressure powder spraying device is positioned at the top of the frame, a nozzle of the high-pressure powder spraying device is positioned in the frame, ultrahigh peak power lasers are arranged on two sides of the frame, a spheroidizing position is arranged below the nozzle of the high-pressure powder spraying device, laser emitters are arranged on two sides below the spheroidizing position, and the bottom of each laser emitter is connected with a positioning indicating light device. The method adopts the ultra-high peak power laser technology, adopts the hydrogenated ruthenium powder as the raw material, completes the dehydrogenation process and the spheroidization process simultaneously, and produces the superfine spherical ruthenium powder by a one-step method.
Description
Technical Field
The invention relates to the technical field of a production method of spherical ruthenium powder, in particular to a device and a method for producing superfine spherical ruthenium powder for 3D printing by a one-step method.
Background
Ruthenium (Ru) is a platinum group metal in the VIII group of the periodic table, is the cheapest metal in the platinum group metal, and the method for preparing high-purity ruthenium powder at home and abroad at present is mainly a chemical method. In recent years, the solar cell is used for manufacturing low-cost solar cells, and attention is paid to the solar cell. The ruthenium metal is hard and difficult to process, and the structural part is prepared by adopting a 3D printing technology, so that the method has great process advantages. For this reason, the production of ultra-fine spherical ruthenium powder for 3D printing is concerned, the melting point of ruthenium (2334 ℃) is high, and the spheroidizing heat source must have sufficiently high power and heating temperature.
The document search of the prior art finds that Chinese patent with publication number CN105458278B discloses a preparation method of high-purity spherical ruthenium powder, which prepares the high-purity spherical ruthenium powder by taking sponge ruthenium (99.9%) as a raw material and adopting a process of 'distillation, chemical precipitation, atomization granulation and microwave calcination', the method reduces the impurity content as much as possible and improves the sphericity and size uniformity of ruthenium particles as much as possible, but the method of the invention has the defects that: the ruthenium powder is prepared by a chemical precipitation method, so the preparation process is complex, the controllability is poor, and the method is not suitable for mass production.
It has also been found through literature search that chinese patent publication No. CN111940758A discloses a method for preparing spherical ruthenium powder by a polyol reduction method, which prepares ruthenium metal nanoparticles by using a polyol as a reducing agent, the polyol having a solubility equivalent to water and being soluble in water or ethanol, so that the polyol solution can become a solvent for metal salts; the polyalcohol has chelation and can be attached to the surface of the ruthenium metal particles to control the nucleation, growth and agglomeration of the nano ruthenium metal particles, thereby playing the role of a colloid stabilizer; when the reaction temperature is increased, the polyol can rapidly reduce the dissolved ruthenium metal ions to obtain nano ruthenium particles, and the surface of the ruthenium nanoparticles is adsorbed with part of the polyol so that the ruthenium nanoparticles can be kept stable in the rest of the polyol. However, the method has the following disadvantages: the polyol is used as a reducing agent to reduce ruthenium in the ruthenium precursor solution, and the amount of the reducing agent, the reaction time and the temperature are difficult to control.
The literature search also finds that the Chinese patent with the publication number of CN104308185A discloses a method for preparing ruthenium powder for a target material by using ruthenium trichloride, and the defects of the method are as follows: the process is complicated, the cost is high, and industrialization is not easy to realize; hydrochloric acid is used in the production process, and the raw material contains chloride ions, so that the environment is not protected; the ruthenium powder has fine particles of 2-5 microns, and is not suitable for 3D printing.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for producing superfine spherical ruthenium powder for 3D printing by a one-step method, which adopts an ultrahigh peak power laser technology, adopts hydrogenated ruthenium powder as a raw material, completes the dehydrogenation process and the spheroidization process at the same time, and produces the superfine spherical ruthenium powder by the one-step method, and the method has the advantages of simple preparation process, easy operation, strong controllability and suitability for mass production; in addition, other substances are not used in the production process, and new impurities cannot be generated, so that the method is more environment-friendly; the prepared product is more suitable for 3D printing.
In order to solve the technical problem, on one hand, the invention adopts the following technical scheme:
a device for producing superfine spherical ruthenium powder for 3D printing by a one-step method comprises a high-pressure powder spraying device and a frame, wherein the high-pressure powder spraying device is positioned at the top of the frame, a nozzle of the high-pressure powder spraying device is positioned inside the frame, ultrahigh peak power lasers are arranged on two sides of the frame, a balling position is arranged below the nozzle of the high-pressure powder spraying device, laser emitters are arranged on two sides below the balling position, and the bottom of each laser emitter is connected with a positioning indicating light device; and a constant-temperature cooling water tank is arranged below the positioning indication light device, and a powder cooling device is arranged on one side of the constant-temperature cooling water tank.
Further, the ultra-high peak power laser emits laser light in a horizontal direction and a vertically downward direction.
Furthermore, both sides of a nozzle of the high-pressure powder injection device are provided with a first beam focusing mirror, a second beam focusing mirror is arranged vertically below the ultrahigh peak power laser, and a third beam focusing mirror is arranged above the laser emitter.
Furthermore, a beam focusing mirror IV is arranged in the laser emitter.
Further, laser emitted in the horizontal direction of the ultrahigh peak power laser is projected on a first beam focusing mirror, and the laser is reflected by the first beam focusing mirror and projected on a fourth beam focusing mirror; laser emitted in the vertical direction of the ultrahigh peak power laser is projected on a second beam focusing mirror, and the laser is reflected and projected on a third beam focusing mirror and a fourth beam focusing mirror in sequence; two light beams are designed to be reflected in different directions, energy is amplified and superposed, and ultrahigh peak power laser is obtained.
Furthermore, the included angles between the first light beam focusing mirror, the second light beam focusing mirror, the third light beam focusing mirror and the fourth light beam focusing mirror and the horizontal direction are 30-45 degrees.
Further, constant temperature cooling water tank is provided with two, and the temperature is in controllable range when guaranteeing the reaction and taking place, all is provided with powder cooling device on two constant temperature cooling water tank, two powder cooling device top is provided with the tray, powder cooling device is located balling position under.
On the other hand, the application provides a method for producing superfine spherical ruthenium powder for 3D printing by a one-step method, which comprises the following steps:
(1) sampling: selecting irregular-shaped hydrogenated ruthenium powder with the granularity of 20-50 mu m;
(2) blowing: spraying and blowing the hydrogenated ruthenium powder into a spheroidizing position by a high-pressure powder spraying device;
(3) high-temperature treatment: the ultrahigh peak power laser emits horizontal laser and vertical laser, and the horizontal laser enters the emitter through the first beam focusing mirror and the fourth beam focusing mirror; the vertical laser enters the emitter through the second beam focusing mirror, the second beam focusing mirror and the fourth beam focusing mirror;
(4) positioning indication: the positioning indicating light device synchronously indicates the direction of the light path according to the descending rate of the powder, thereby realizing a high-efficiency spheroidizing process;
(5) and (3) preparing a product: in the laser high-temperature treatment process of the hydrogenated ruthenium powder, the hydrogenated ruthenium powder is decomposed into hydrogen and metal ruthenium, the hydrogen leaves a system along with argon, the metal ruthenium is melted and cooled at high temperature, and spherical particle powder is formed in the cooling process under the action of surface tension, so that the spherical ruthenium powder with the particle size of 15-45 mu m is obtained.
Further, the blowing gas is argon, and the blowing powder feeding speed is 20-30 kg/h.
Furthermore, the laser frequency emitted by the ultra-high peak power laser is 0.1Hz, and the power is 1-2 PW.
Further, the spheroidized powder is cooled by adopting high-speed fluid in the powder cooling device, so that the cooling speed is high; the constant-temperature cooling water tank adopts a closed water cavity cooling tank body, so that the temperature is in a controllable range when the reaction occurs.
Compared with the prior art, the invention has the beneficial effects that:
1. the method is simple, is easy to operate, can prepare the superfine spherical ruthenium powder by a one-step method, and is suitable for mass production; the method has the advantages of simple preparation process, easy operation and strong controllability, and is suitable for mass production.
2. The method adopts an ultrahigh peak power laser technology, adopts hydrogenated ruthenium powder as a raw material, completes the dehydrogenation process and the spheroidization process at the same time, and produces superfine spherical ruthenium powder by a one-step method; the ultrahigh peak power laser works in a low frequency range of 10Hz and below, the power exceeds 1PW, the power is high, the heating efficiency is high, even ruthenium with a high melting point can be instantly melted to form spherical liquid drops, a sphere is formed under the action of surface tension, and the cooling speed is extremely high to form regular spherical powder.
3. In the production process, other substances are not used, and new impurities cannot be generated, so that the method is more environment-friendly; the prepared product is more suitable for 3D printing.
4. The invention has simple structure, two light beams are designed to reflect in different directions, and energy is amplified and superposed to obtain the laser with ultrahigh peak power; the constant-temperature cooling water tank ensures the safe production of the device, and adopts a closed water cavity cooling tank body to ensure that the temperature is in a controllable range when the reaction occurs.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention;
FIG. 2 is a scanning electron micrograph of ruthenium powder produced by the process of the present invention;
FIG. 3 is a partially enlarged scanning electron micrograph of ruthenium powder produced by the process of the present invention.
Wherein, 1, a high-pressure powder spraying device; 2. an ultra-high peak power laser; 3. positioning an indicator light device; 4. a laser transmitter; 401. a fourth light beam focusing mirror; 5. a first light beam focusing mirror; 501. a second light beam focusing mirror; 502. a third light beam focusing mirror; 6. a powder cooling device; 601. a tray; 7. a constant temperature cooling water tank; 8. a frame.
Detailed Description
In order to make the technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following specific embodiments.
Example 1
The device for producing the superfine spherical ruthenium powder for 3D printing by the one-step method comprises a high-pressure powder spraying device 1 and a frame 8, wherein the high-pressure powder spraying device 1 is positioned at the top of the frame 8, a nozzle of the high-pressure powder spraying device 1 is positioned inside the frame 8, ultrahigh peak power lasers 2 are arranged on two sides of the frame 8, the ultrahigh peak power lasers 2 emit laser in the horizontal direction and the vertical downward direction, two light beams are designed to be reflected in different directions, energy is amplified and overlapped, and ultrahigh peak power laser is obtained.
The device comprises a high-pressure powder injection device 1, a laser emitter 4, a beam focusing mirror II 401, a beam focusing mirror III 502, a beam focusing mirror I5, a beam focusing mirror II 501, a laser emitter 4, a beam focusing mirror IV 401, a beam focusing mirror III 502, an included angle of the beam focusing mirror I5, the beam focusing mirror II 501, the beam focusing mirror III 502 and the beam focusing mirror IV 401 with the horizontal direction of 30-45 degrees, laser emitted by the ultrahigh-peak-power laser device 2 in the horizontal direction is projected on the beam focusing mirror I5, and the laser is reflected by the beam focusing mirror I5 and projected on the beam focusing mirror IV 401; the laser emitted by the ultrahigh peak power laser 2 in the vertical direction is projected on the second beam focusing mirror 501, and the laser is reflected and projected on the third beam focusing mirror 502 and the fourth beam focusing mirror 401 in sequence.
The bottom of the laser transmitter 4 is connected with a positioning indication light device 3; the below of location pilot light device 3 is provided with constant temperature cooling water tank 7, and constant temperature cooling water tank 7 guarantees device safety in production, adopts the closed water cavity cooling box, and the temperature is in controllable within range when guaranteeing that the reaction takes place, one side of constant temperature cooling water tank 7 is provided with powder cooling device 6, and constant temperature cooling water tank 7 is provided with two, all is provided with powder cooling device 6 on two constant temperature cooling water tank 7, two 6 tops of powder cooling device are provided with tray 601, powder cooling device 6 is located the balling position under.
Example 2
(1) Sampling: selecting irregular-shaped hydrogenated ruthenium powder with the granularity of 20-50 mu m;
(2) blowing: spraying ruthenium hydride powder into a spheroidizing position through a high-pressure powder spraying device 1, wherein the powder spraying speed is 20 kg/h;
(3) high-temperature treatment: the ultrahigh peak power laser 2 emits horizontal laser and vertical laser, the horizontal laser is reflected in different directions by a first beam focusing mirror 5 and a fourth beam focusing mirror 401, energy is amplified and superposed to obtain ultrahigh peak power laser, and the ultrahigh peak power laser enters a laser emitter 4; the vertical light beam enters a laser emitter 4 through a second light beam focusing mirror 501, a second light beam focusing mirror 501 and a fourth light beam focusing mirror 401, the laser frequency is 0.1Hz, and the power is 2 PW;
(4) positioning indication: the positioning indicating light device 3 synchronously indicates the direction of the light path according to the descending rate of the powder, and a high-efficiency spheroidizing process is realized;
(5) and (3) preparing a product: in the laser high-temperature treatment process of the hydrogenated ruthenium powder, the hydrogenated ruthenium powder is decomposed into hydrogen and metal ruthenium, the hydrogen leaves a system along with argon, the metal ruthenium is melted and cooled at high temperature, the metal ruthenium enters a powder cooling device 6, high-speed fluid cooling spheroidized powder is adopted in the device, the cooling speed is high, spherical particle powder is formed in the cooling process under the action of surface tension, 15-45 mu m spherical ruthenium powder is obtained, a constant-temperature cooling water tank 7 ensures the safe production of the device, and a closed water cavity cooling box body is adopted to ensure that the temperature is in a controllable range when the reaction occurs.
The spheroidization rate of the obtained spherical ruthenium powder is measured to be 98 percent, and the Hall flow rate is 16.5s/50 g.
Example 3
(1) Sampling: selecting irregular-shaped hydrogenated ruthenium powder with the granularity of 20-50 mu m;
(2) blowing: spraying ruthenium hydride powder into a spheroidizing position through a high-pressure powder spraying device 1, wherein the powder spraying speed is 30 kg/h;
(3) high-temperature treatment: the ultrahigh peak power laser 2 emits horizontal laser and vertical laser, the horizontal laser is reflected in different directions by a first beam focusing mirror 5 and a fourth beam focusing mirror 401, energy is amplified and superposed to obtain ultrahigh peak power laser, and the ultrahigh peak power laser enters a laser emitter 4; the vertical light beam enters the laser emitter 4 through the second light beam focusing mirror 501, the second light beam focusing mirror 501 and the fourth light beam focusing mirror 401, the laser frequency is 0.1Hz, and the power is 2 PW;
(4) positioning indication: the positioning indication light device 3 synchronously indicates the direction of the light path according to the descending rate of the powder, and realizes a high-efficiency spheroidizing process;
(5) and (3) preparing a product: in the laser high-temperature treatment process of the hydrogenated ruthenium powder, the hydrogenated ruthenium powder is decomposed into hydrogen and metal ruthenium, the hydrogen leaves a system along with argon, the metal ruthenium is melted and cooled at high temperature, the metal ruthenium enters a powder cooling device 6, high-speed fluid cooling spheroidized powder is adopted in the device, the cooling speed is high, spherical particle powder is formed in the cooling process under the action of surface tension, 15-45 mu m spherical ruthenium powder is obtained, a constant-temperature cooling water tank 7 ensures the safe production of the device, and a closed water cavity cooling box body is adopted to ensure that the temperature is in a controllable range when the reaction occurs.
The spheroidization rate of the obtained spherical ruthenium powder is measured to be 95 percent, and the Hall flow rate is 17.1s/50 g.
Example 4
(1) Sampling: selecting irregular-shaped hydrogenated ruthenium powder with the granularity of 20-50 mu m;
(2) blowing: spraying ruthenium hydride powder into a spheroidizing position through a high-pressure powder spraying device 1, wherein the powder spraying speed is 30 kg/h;
(3) high-temperature treatment: the ultrahigh peak power laser 2 emits horizontal laser and vertical laser, the horizontal laser is reflected in different directions by a first beam focusing mirror 5 and a fourth beam focusing mirror 401, energy is amplified and superposed to obtain ultrahigh peak power laser, and the ultrahigh peak power laser enters a laser emitter 4; the vertical light beam enters the laser emitter 4 through the second light beam focusing mirror 501, the second light beam focusing mirror 501 and the fourth light beam focusing mirror 401, the laser frequency is 0.1Hz, and the power is 1 PW;
(4) positioning indication: the positioning indicating light device 3 synchronously indicates the direction of the light path according to the descending rate of the powder, and a high-efficiency spheroidizing process is realized;
(5) and (3) preparing a product: in the laser high-temperature treatment process of the hydrogenated ruthenium powder, the hydrogenated ruthenium powder is decomposed into hydrogen and metal ruthenium, the hydrogen leaves a system along with argon, the metal ruthenium is melted and cooled at high temperature, the metal ruthenium enters a powder cooling device 6, high-speed fluid cooling spheroidized powder is adopted in the device, the cooling speed is high, spherical particle powder is formed in the cooling process under the action of surface tension, 15-45 mu m spherical ruthenium powder is obtained, a constant-temperature cooling water tank 7 ensures the safe production of the device, and a closed water cavity cooling box body is adopted to ensure that the temperature is in a controllable range when the reaction occurs.
The spheroidization rate of the obtained spherical ruthenium powder is measured to be 93%, and the Hall flow rate is measured to be 18.8s/50 g.
It should be understood that the detailed description and specific examples, while indicating the invention, are given by way of illustration only, since various other embodiments will become apparent to those skilled in the art upon reference to the following detailed description.
Claims (10)
1. The device for producing the superfine spherical ruthenium powder for 3D printing by the one-step method is characterized by comprising a high-pressure powder injection device (1) and a frame (8), wherein the high-pressure powder injection device (1) is positioned at the top of the frame (8), a nozzle of the high-pressure powder injection device (1) is positioned inside the frame (8), ultrahigh peak power lasers (2) are arranged on two sides of the frame (8), a balling position is arranged below the nozzle of the high-pressure powder injection device (1), laser emitters (4) are arranged on two sides below the balling position, and the bottom of each laser emitter (4) is connected with a positioning indication light device (3); a constant-temperature cooling water tank (7) is arranged below the positioning indication light device (3), and a powder cooling device (6) is arranged on one side of the constant-temperature cooling water tank (7).
2. The apparatus for one-step process for producing ultrafine spherical ruthenium powder for 3D printing according to claim 1, wherein the ultra-high peak power laser (2) emits laser light in horizontal and vertical downward directions.
3. The device for producing the superfine spherical ruthenium powder for 3D printing by the one-step method according to claim 1, wherein the first beam focusing mirror (5) is arranged on each of two sides of the nozzle of the high-pressure powder spraying device (1), the second beam focusing mirror (501) is arranged vertically below the ultrahigh-peak power laser (2), and the third beam focusing mirror (502) is arranged above the laser emitter (4).
4. The apparatus for producing ultrafine spherical ruthenium powder for 3D printing according to the claim 3 by one-step method, wherein the laser emitter (4) is internally provided with a beam focusing mirror four (401).
5. The apparatus for producing ultrafine spherical ruthenium powder for 3D printing according to claim 3 by one-step method, wherein the laser emitted from the ultra-high peak power laser (2) in horizontal direction is projected onto the first beam focusing mirror (5), and the laser is reflected by the first beam focusing mirror (5) and projected onto the fourth beam focusing mirror (401); the laser emitted by the ultrahigh peak power laser (2) in the vertical direction is projected on a second beam focusing mirror (501), and the laser is reflected and projected on a third beam focusing mirror (502) and a fourth beam focusing mirror (401) in sequence.
6. The device for producing the superfine spherical ruthenium powder for 3D printing by the one-step method according to claim 5, wherein the included angles between the first beam focusing mirror (5), the second beam focusing mirror (501), the third beam focusing mirror (502) and the fourth beam focusing mirror (401) and the horizontal direction are 30-45 degrees.
7. The device for producing the superfine spherical ruthenium powder for 3D printing by the one-step method according to claim 1, wherein the constant-temperature cooling water tanks (7) are provided in two numbers, the powder cooling devices (6) are arranged on the two constant-temperature cooling water tanks (7), a tray (601) is arranged on the tops of the two powder cooling devices (6), and the powder cooling devices (6) are positioned right below a spheroidizing position.
8. A method for producing superfine spherical ruthenium powder for 3D printing by a one-step method is characterized by comprising the following steps:
(1) sampling: selecting irregular-shaped hydrogenated ruthenium powder with the granularity of 20-50 mu m;
(2) blowing: spraying and blowing ruthenium hydride powder into a spheroidizing position by a high-pressure powder spraying device (1);
(3) high-temperature treatment: the ultrahigh peak power laser (2) emits horizontal and vertical lasers, and the horizontal lasers enter the emitter (4) through the first beam focusing mirror (5) and the fourth beam focusing mirror (401); the vertical light beam enters the emitter (4) through a second light beam focusing mirror (501), a second light beam focusing mirror (501) and a fourth light beam focusing mirror (401);
(4) positioning indication: the positioning indicating light device (3) synchronously indicates the direction of the light path according to the descending rate of the powder;
(5) and (3) preparing a product: in the laser high-temperature treatment process of the hydrogenated ruthenium powder, the hydrogenated ruthenium powder is decomposed into hydrogen and metal ruthenium, the hydrogen leaves a system along with argon, the metal ruthenium is melted and cooled at high temperature, and spherical particle powder is formed in the cooling process under the action of surface tension, so that the spherical ruthenium powder with the particle size of 15-45 mu m is obtained.
9. The method for producing ultrafine spherical ruthenium powder for 3D printing according to claim 8 by one-step process, wherein the blowing gas is argon, and the blowing powder feeding rate is 20-30 kg/h; the laser frequency emitted by the ultrahigh peak power laser (2) is 0.1Hz, and the power is 1-2 PW.
10. The one-step method for producing superfine spherical ruthenium powder for 3D printing according to claim 8, wherein the spheroidized powder is cooled in the powder cooling device (6) by using high-speed fluid; the constant temperature cooling water tank (7) adopts a closed water cavity cooling tank body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210697315.0A CN115007851B (en) | 2022-06-20 | 2022-06-20 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210697315.0A CN115007851B (en) | 2022-06-20 | 2022-06-20 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115007851A true CN115007851A (en) | 2022-09-06 |
| CN115007851B CN115007851B (en) | 2024-02-06 |
Family
ID=83074145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210697315.0A Active CN115007851B (en) | 2022-06-20 | 2022-06-20 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115007851B (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020017509A1 (en) * | 2000-08-10 | 2002-02-14 | Takashi Ishide | Laser beam machining head and laser beam machining apparatus having same |
| KR20180010372A (en) * | 2016-07-20 | 2018-01-31 | 한국원자력연구원 | Laser processing head |
| US20190061005A1 (en) * | 2017-08-30 | 2019-02-28 | General Electric Company | High Quality Spherical Powders for Additive Manufacturing Processes Along With Methods of Their Formation |
| CN110312583A (en) * | 2016-10-14 | 2019-10-08 | 普瑞玛工业股份有限公司 | By laser heat treatment, particularly pass through the laser operations machine and corresponding method for increasing material manufacturing of fusion |
| CN110756807A (en) * | 2019-11-29 | 2020-02-07 | 中国工程物理研究院材料研究所 | Laser melting deposition method of hydrogenated titanium dehydrogenated powder |
| CN111390192A (en) * | 2020-04-26 | 2020-07-10 | 中国科学院宁波材料技术与工程研究所 | Equipment and method for preparing spherical metal micro powder |
| CN111519183A (en) * | 2020-04-28 | 2020-08-11 | 苏州大学 | Laser ultra-high-speed cladding head, laser ultra-high-speed cladding system and laser ultra-high-speed cladding method |
| AU2020103465A4 (en) * | 2020-11-16 | 2021-01-28 | Kunming University Of Science And Technology | Method for preparing high-purity spherical ruthenium powder by microwave one-step method |
| CN112654444A (en) * | 2018-06-19 | 2021-04-13 | 6K有限公司 | Method for producing spheroidized powder from raw material |
| WO2021129468A1 (en) * | 2019-12-26 | 2021-07-01 | 西安铂力特增材技术股份有限公司 | Dual-spot-based slm forming system and method |
| CN214768946U (en) * | 2021-04-21 | 2021-11-19 | 苏州工业职业技术学院 | Three-beam wire powder mixed laser cladding system |
| CN215033627U (en) * | 2021-05-11 | 2021-12-07 | 苏州大学 | Annular hollow partial-focus laser cladding device |
| CN114260454A (en) * | 2021-12-24 | 2022-04-01 | 四川大学 | Preparation method of high-quality spherical metal powder |
-
2022
- 2022-06-20 CN CN202210697315.0A patent/CN115007851B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020017509A1 (en) * | 2000-08-10 | 2002-02-14 | Takashi Ishide | Laser beam machining head and laser beam machining apparatus having same |
| KR20180010372A (en) * | 2016-07-20 | 2018-01-31 | 한국원자력연구원 | Laser processing head |
| CN110312583A (en) * | 2016-10-14 | 2019-10-08 | 普瑞玛工业股份有限公司 | By laser heat treatment, particularly pass through the laser operations machine and corresponding method for increasing material manufacturing of fusion |
| CN111093866A (en) * | 2017-08-30 | 2020-05-01 | 通用电气公司 | High quality spherical powder for additive manufacturing processes and methods of forming the same |
| US20190061005A1 (en) * | 2017-08-30 | 2019-02-28 | General Electric Company | High Quality Spherical Powders for Additive Manufacturing Processes Along With Methods of Their Formation |
| CN112654444A (en) * | 2018-06-19 | 2021-04-13 | 6K有限公司 | Method for producing spheroidized powder from raw material |
| CN110756807A (en) * | 2019-11-29 | 2020-02-07 | 中国工程物理研究院材料研究所 | Laser melting deposition method of hydrogenated titanium dehydrogenated powder |
| WO2021129468A1 (en) * | 2019-12-26 | 2021-07-01 | 西安铂力特增材技术股份有限公司 | Dual-spot-based slm forming system and method |
| CN111390192A (en) * | 2020-04-26 | 2020-07-10 | 中国科学院宁波材料技术与工程研究所 | Equipment and method for preparing spherical metal micro powder |
| CN111519183A (en) * | 2020-04-28 | 2020-08-11 | 苏州大学 | Laser ultra-high-speed cladding head, laser ultra-high-speed cladding system and laser ultra-high-speed cladding method |
| AU2020103465A4 (en) * | 2020-11-16 | 2021-01-28 | Kunming University Of Science And Technology | Method for preparing high-purity spherical ruthenium powder by microwave one-step method |
| CN214768946U (en) * | 2021-04-21 | 2021-11-19 | 苏州工业职业技术学院 | Three-beam wire powder mixed laser cladding system |
| CN215033627U (en) * | 2021-05-11 | 2021-12-07 | 苏州大学 | Annular hollow partial-focus laser cladding device |
| CN114260454A (en) * | 2021-12-24 | 2022-04-01 | 四川大学 | Preparation method of high-quality spherical metal powder |
Non-Patent Citations (1)
| Title |
|---|
| 邹宇;廖先杰;赖奇;刘翘楚;: "3D打印用球形钛粉制备技术研究现状", 中国材料进展, no. 11, pages 1092 - 1099 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115007851B (en) | 2024-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103846447B (en) | The aerosolization preparation method of a kind of superfine spherical titanium or titanium alloy powder | |
| US7534410B1 (en) | Method for making silica nanoparticles by flame spray pyrolysis adopting two-fluid nozzle | |
| CN101182043B (en) | Method for preparing spherical cobaltous oxide | |
| WO2019165958A1 (en) | Method for preparing nano-quantum dot, nano-quantum dot material, application and quantum dot article | |
| TWI233321B (en) | Method for producing nano oxide powder using D.C. plasma thermo-reaction | |
| TW558471B (en) | Method and device for manufacturing metallic particulates and manufactured metallic particulates | |
| CN101239391B (en) | Method for coating metal nano granule by laser synthesizing carbon | |
| CN101376174A (en) | Method for preparing superfine spherical cobalt powder | |
| Hu et al. | Preparation of hollow alumina nanospheres via surfactant-assisted flame spray pyrolysis | |
| Malekzadeh et al. | Laser pyrolysis synthesis of zinc-containing nanomaterials using low-cost ultrasonic spray delivery of precursors | |
| CN113636531A (en) | Preparation method of nano-scale hollow iron phosphide particles | |
| Cao et al. | Fabrication and application of CeO2 nanostructure with different morphologies: a review | |
| CN115007851A (en) | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method | |
| Zhang et al. | Au catalyst decorated silica spheres: Synthesis and high-performance in 4-nitrophenol reduction | |
| CN110184488A (en) | A kind of method that short route prepares metal dispersion-strengthened Cu | |
| JP2007314867A (en) | Manufacturing method of nickel powder | |
| CN111515408B (en) | NiTi alloy powder and preparation method and application thereof | |
| TW570851B (en) | Method and device for producing metal powder | |
| KR101501164B1 (en) | Platinum-based bimetallic catalyst using successive solution plasma process and device for manufacturing and synthesis method thereof | |
| CN102432183B (en) | Nanomicro-grade titanium oxide glass spheres and preparation method thereof | |
| CN109081694B (en) | Yttrium aluminum composite oxide nano powder synthesized by precursor liquid and high-temperature atomized flame and preparation method thereof | |
| CN116352094A (en) | Preparation method of superfine alloy powder | |
| Bensebaa | Dry production methods | |
| Luo | Nanoparticles inks | |
| US20150093325A1 (en) | Method for preparation of an alane-etherate complex and alane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |