CN116352095A - Metal vapor quenching nucleation powder forming device and particle size control method - Google Patents
Metal vapor quenching nucleation powder forming device and particle size control method Download PDFInfo
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- CN116352095A CN116352095A CN202310516438.4A CN202310516438A CN116352095A CN 116352095 A CN116352095 A CN 116352095A CN 202310516438 A CN202310516438 A CN 202310516438A CN 116352095 A CN116352095 A CN 116352095A
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- 239000000843 powder Substances 0.000 title claims abstract description 166
- 238000010899 nucleation Methods 0.000 title claims abstract description 120
- 230000006911 nucleation Effects 0.000 title claims abstract description 120
- 239000002184 metal Substances 0.000 title claims abstract description 79
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 79
- 239000002245 particle Substances 0.000 title claims abstract description 36
- 238000010791 quenching Methods 0.000 title claims abstract description 24
- 230000000171 quenching effect Effects 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 198
- 239000007789 gas Substances 0.000 claims abstract description 153
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 83
- 239000000498 cooling water Substances 0.000 claims abstract description 19
- 239000002826 coolant Substances 0.000 claims description 26
- 238000000227 grinding Methods 0.000 claims description 24
- 230000035939 shock Effects 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 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
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000004033 diameter control Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002923 metal particle Substances 0.000 abstract description 17
- 238000005054 agglomeration Methods 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 10
- 239000012466 permeate Substances 0.000 abstract description 3
- 239000000112 cooling gas Substances 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 239000012808 vapor phase Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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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
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
-
- 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 utility model discloses a metal vapor quenching nucleation powder forming device and a particle size control method, wherein an outlet of a nucleation pipe is connected with a quenching powder device, the quenching powder device comprises a powder forming chamber, a gas cooling pipe positioned in the powder forming chamber and a water cooling layer II positioned on the outer wall of the powder forming chamber, and the temperature in the powder forming chamber can be controlled by controlling the temperature of cooling water of the water cooling layer II and the gas spraying state in the gas cooling pipe; when the nucleated metal vapor enters the powder forming chamber, the nucleated metal vapor can quickly permeate into the powder forming chamber to be fully mixed and contacted with cooling gas, so that metal particles in the powder forming chamber are quickly cooled, a water cooling layer II on the outer wall of the powder forming chamber and a gas cooling pipe are combined inside and outside, the temperature of each position in the powder forming chamber can be quickly controlled, the continuous growth or agglomeration of the metal particles is avoided, cooling water with different temperatures is introduced into the water cooling layer, gaseous cooling media with different temperatures are introduced into the gas cooling pipe, and the gaseous cooling media with different flow rates are introduced into the gas cooling pipe to control the temperature in the powder forming chamber.
Description
Technical Field
The utility model belongs to the field of metal vapor powder forming devices, and particularly relates to a metal vapor quenching nucleation powder forming device and a particle size control method.
Background
The physical vapor phase process for preparing superfine metal powder has been developed in recent years, and especially plasma physical vapor deposition process for preparing superfine powder has been attracting attention in recent years, the process uses excited plasma as heat source, the temperature can reach 10000 deg.c, most refractory metal can be gasified into atomic gas under normal pressure, metal vapor can form superfine metal powder after quick cooling, the whole process is completed in inert gas environment, no exhaust gas and waste water are discharged, no other impurity is introduced, and the particle size of required nickel powder can be obtained by regulating technological parameters. Physical vapor phase processes are the most commonly used methods for preparing ultra-fine metal powders.
In the preparation of refractory metal ultrafine powders using a physical vapor phase method, in order for the metal vapor to cool the vapor into metal particles of a certain particle size range, it is necessary to cool the metal vapor to a certain temperature in an extremely short time. However, in practice, a short atomic nucleation process is required after the metal vapor exits the crucible, and in order to prevent the nucleated particles from growing excessively, it is necessary to cool the particles below a certain temperature in a very short time to inhibit excessive growth and agglomeration of the powder. However, the nucleation and growth process of atomized metal vapor is very difficult to control due to the limitation of the structure of common equipment, especially the temperature control of the equipment on the metal vapor powder forming process can not be reduced to the required temperature rapidly, so that particle nucleation, growth and cooling are simultaneously carried out, bad products such as excessive growth, different sizes, agglomeration and even conjunct phenomena are easy to occur, and the metal vapor nucleation device for preparing ultrafine powder materials by a physical vapor phase method is adopted by the existing equipment in a mode of controlling the temperature or a water cooling jacket, for example, the metal vapor nucleation device for preparing ultrafine powder materials is described in Chinese patent publication No. CN216421070U, and the temperature reduction in the nucleation structure is controlled through a shell structure with a jacket and a heat preservation structure, and the metal vapor nucleation is controlled to be successfully completed by controlling the temperature range. Because the mode of controlling the temperature and the cooling speed is single, the powder is difficult to cool below a certain temperature in a very short time, and excessive growth and agglomeration of the powder are inhibited.
Disclosure of Invention
The utility model aims at: provided are a metal vapor quenching nucleation and powdering device capable of rapidly nucleating and rapidly cooling metal vapor to a certain temperature, and a method for controlling the grain size of the powder.
The technical scheme adopted by the utility model is as follows:
the utility model provides a metal vapor quenching nucleation powder device, including the nucleation pipe, nucleation pipe both ends are the feed inlet and the discharge gate respectively, the nucleation pipe includes pipeline one and the water-cooling layer one that is located pipeline one outer wall, the export of nucleation pipe is connected the shock condenser powder ware, the shock condenser powder ware includes into powder room, be located the inside gas cooling pipe of powder room, and the water-cooling layer two that is located powder room outer wall, nucleation pipe and the inside intercommunication of powder room, the powder room is connected with the discharging pipe, the discharging pipe includes pipeline two and the water-cooling layer three that is located pipeline two outer walls, the gas cooling pipe has the air inlet, and the air inlet extends to the powder room outside, the equipartition is provided with the gas spout on the gas cooling pipe; the powder forming chamber is in a bullet shell shape, one end, which is close to the nucleation pipe, is of a cylindrical structure, and the end, which is close to the discharge pipe, is of an arc-shaped funnel structure; the gas cooling pipes are arranged in the powder forming chamber in a reciprocating and uniform parallel manner along the material flow direction, and the cooling pipes which are arranged in the powder forming chamber in parallel are sequentially communicated through arc-shaped pipelines.
The further technical scheme is that an insulation layer is arranged on the outer wall of the water cooling layer, and the insulation layer is a ceramic felt insulation layer or a carbon felt insulation layer.
The technical scheme is that the first inner pipeline of the nucleation pipe is a trumpet-shaped pipeline with a large feed inlet and a small discharge outlet, the first inner pipeline of the nucleation pipe, the heat-insulating layer and the first water-cooling layer are coaxial pipelines, the ratio of the outer diameter A of the first inner pipeline to the outer diameter B of the heat-insulating layer on the same section is 1:1-4, and the ratio of the outer diameter A of the first inner pipeline to the outer diameter C of the water-cooling layer on the same section is 1:1-15. The ratio of the inner diameter of the feed inlet to the inner diameter of the discharge outlet at the two ends of the nucleation tube is 1:1-2. The ratio of the length D of the nucleation tube to the length E of the powder forming chamber of the condenser powder is 1:0.5-50, the ratio of the average diameter of the nucleation tube to the length D of the nucleation tube is 1:1-50, and the ratio of the minimum inner diameter Amin of the nucleation tube to the maximum inner diameter G of the powder forming chamber of the condenser powder is 1: 1-30.
The further technical proposal is that the number of the gas cooling pipes which are arranged in parallel in the powder forming chamber is more than 3.
The gas cooling pipe is of a double-layer pipe structure and comprises an inner pipe and an outer pipe, a water cooling layer IV is arranged inside the inner pipe, a gas flow layer is arranged between the outer pipe and the inner pipe, gas nozzles are arranged on the surface of the outer pipe, the arc of the gas nozzles on the outer pipe corresponds to the circle center angle of the outer circle of the gas flow layer to be 15-45 degrees, the ratio of the inner diameter K of the water cooling layer of the gas cooling pipe to the outer diameter H of the gas flow layer is 1:1-4, 2-4 gas nozzles are arranged on the outer pipe of the gas flow layer along the circumferential direction in the same section position, and the total number of the gas nozzles is 30-200.
The further technical proposal is that the junction of the nucleation tube and the powder forming chamber is in a horn mouth shape.
The further technical scheme is that metal steam is connected into a feeding hole of a nucleation pipe in the metal steam quenching nucleation powder forming device according to claim 7, the temperature and the cooling speed in the powder chamber are changed to be controlled to form powder particle sizes, and specifically, the temperature and the cooling speed in the powder chamber are changed to be two modes, firstly, cooling water with different temperatures is introduced into a water cooling layer, gaseous cooling media with different temperatures are introduced into a gas cooling pipe, and the gaseous cooling media with different flow rates are introduced into the gas cooling pipe to control the temperature in the powder chamber; second, adjusting the ratio of an outer diameter A of the inner pipeline to an outer diameter B of the heat insulation layer, the ratio of the outer diameter A of the inner pipeline to an outer diameter C of the water cooling layer, the ratio of the inner diameter of a feed inlet to the inner diameter of a discharge outlet at two ends of the nucleation pipe, the ratio of the length D of the nucleation pipe to the length E of a powder forming chamber of the shock condensation powder device, the ratio of the average diameter of the nucleation pipe to the length D of the nucleation pipe, and the minimum inner diameter A of the nucleation pipe min The ratio of the gas jet nozzle to the maximum inner diameter G of the powder forming chamber of the shock condenser 2, the number of the gas jet nozzles, the arc of the gas jet nozzle on the outer tube correspond to the circle center angle of the outer circle of the gas flow layer, and the ratio of the inner diameter K of the water cooling layer of the gas cooling tube to the outer diameter H of the gas flow layer.
The further technical scheme is that the gaseous cooling medium is nitrogen, argon, helium, hydrogen or mixed gas of the 2 gases.
In summary, due to the adoption of the technical scheme, the beneficial effects of the utility model are as follows:
the nucleation pipe comprises an inner pipeline I and a water cooling layer I positioned on the outer wall of the inner pipeline I, and the purpose of controlling the nucleation speed can be achieved by adjusting the temperature of cooling water of the water cooling layer I.
The outlet of the nucleation tube is connected with a shock condenser, and the temperature in the powder forming chamber can be controlled by adjusting the temperature of cooling water of the water cooling layer II.
The powder forming chamber is in the shape of a bullet shell, and the gas cooling pipes in the powder forming chamber are parallel to the flowing direction of the material flow, so that the powder forming chamber accords with the fluid principle, can reduce the residual loss of superfine metal powder in the powder forming chamber and on a pipeline, and improves the yield of the metal powder.
The first inner pipeline of the nucleation pipe is a trumpet-shaped pipeline with a large feed inlet and a small discharge outlet, accords with the fluid principle, accelerates the material flowing speed in the channel along the flowing direction, ensures that the atomic nucleation is more uniform to a certain extent, is relatively straight, can reduce the atomic nucleation time and reduces the probability of generating large metal particles.
The gas cooling pipes are uniformly provided with gas nozzles, inert gaseous cooling medium is introduced into the gas cooling pipes, and when nucleated metal vapor enters the powder forming chamber, the nucleated metal vapor can quickly permeate into the powder forming chamber and fully contacts with the low-temperature inert gaseous cooling medium sprayed by the gas cooling pipes in a mixing manner to perform heat exchange, so that metal particles in the powder forming chamber are quickly cooled, a water cooling layer II on the outer wall of the powder forming chamber and the gas cooling pipes are combined inside and outside, the temperature of each position in the powder forming chamber can be quickly controlled, the continuous growth or agglomeration of the metal particles is avoided, the particle size range of the metal particles is controlled within a certain range, the powder forming speed is higher, and the particle size is uniform; compared with the traditional single temperature control mode, the metal vapor can be quickly nucleated and quickly cooled to a certain temperature.
And the gas flow formed by the inert gaseous cooling medium sprayed out of the gas cooling pipe can further disperse the nucleated metal vapor entering the powder forming chamber, so that the temperature of the nucleated metal vapor is easier to lower, the continuous growth or agglomeration of metal particles is further avoided, and the particle size of the powder is more uniform.
The temperature inside the powder forming chamber is controlled by changing the temperature inside the powder forming chamber and the cooling speed, specifically, cooling water with different temperatures is introduced into the water cooling layer, gaseous cooling media with different temperatures are introduced into the gas cooling pipe, and gaseous cooling media with different flow rates are introduced into the gas cooling pipe, or the temperature inside the powder forming chamber or the cooling speed is controlled by changing the size proportion of the components.
Drawings
FIG. 1 is a schematic view of the overall structure of the present utility model;
FIG. 2 is a schematic view of the arrangement of the gas cooling tubes according to the present utility model;
FIG. 3 is a schematic view of a gas cooling tube according to the present utility model;
FIG. 4 is a schematic structural view of a quenching nucleation and powdering device according to the present utility model;
FIG. 5 is a schematic view of the gas cooling tube connection orientation of the present utility model;
FIG. 6 is a schematic view of the connection orientation of the gas cooling tube according to the present utility model at another view angle;
fig. 7 is a schematic structural view of the powdering device of the present utility model.
Detailed Description
The present utility model will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present utility model more apparent.
As shown in fig. 1-7.
Example 1
The utility model provides a metal vapor quenching nucleation powder device which characterized in that, including nucleation pipe 1, nucleation pipe 1 both ends are feed inlet 4 and discharge gate 5 respectively, nucleation pipe 1 includes pipeline one 11 and be located pipeline one 11 water cooling layer one 13 on the outer wall, the export of nucleation pipe 1 connects shock condenser powder ware 2, shock condenser powder ware 2 includes powder room 22, be located the inside gas cooling tube 21 of powder room 22, and be located the water cooling layer two 23 on the outer wall of powder room 22, nucleation pipe 1 and the inside intercommunication of powder room 22, powder room 22 is connected with discharging pipe 3, discharging pipe 3 includes pipeline two 32 and be located pipeline two 32 water cooling layer three 31 on the outer wall, gas cooling tube 21 has air inlet 6, and air inlet 6 extends to the outside of powder room 22, be provided with gas spout 213 on the gas cooling tube 21 equipartition. The powder forming chamber 22 is in a bullet shell shape, one end, which is close to the nucleation tube 1, is in a cylindrical structure, and one end, which is close to the discharge tube 3, is in an arc funnel structure; the gas cooling pipes 21 are arranged in parallel in the powder forming chamber 22 in a reciprocating and uniform manner along the material flow direction, and the gas cooling pipes 21 arranged in parallel in the powder forming chamber 22 are sequentially communicated through arc-shaped pipelines.
When the device is used, the outer part of the inner pipeline II 32 of the discharging pipe 3 is sequentially connected with the existing gas-solid separation and powder collecting device and an air blower, after metal steam is connected into the feed inlet 4 in the nucleation pipe 1 in the metal steam quenching nucleation powder forming device, the temperature and the cooling speed in the powder chamber 22 are changed to be controlled to be the powder particle size, the temperature and the cooling speed in the powder chamber 22 are changed to be the powder particle size, specifically, cooling water with different temperatures is introduced into the water cooling layer II 23, gaseous cooling media with different temperatures are introduced into the gas cooling pipe 21, and the temperature in the powder chamber is controlled by introducing gaseous cooling media with different flow rates into the gas cooling pipe 21, or the temperature in the powder chamber is controlled by changing the size proportion of components. The inert gaseous cooling medium in the gas cooling pipe 21 is nitrogen, argon, helium, hydrogen or a mixed gas of the 2 gases, the number of the gas nozzles 213 can be changed by replacing the gas cooling pipe, and the water cooling layer one 13, the water cooling layer two 23 and the water cooling layer three 31 are all water cooling jackets.
The outlet of the nucleation tube 1 is connected with a condenser powder 2, the condenser powder 2 comprises a powder forming chamber 22, a gas cooling tube 21 positioned in the powder forming chamber 22 and a water cooling layer II 23 positioned on the outer wall of the powder forming chamber 22, and the temperature in the powder forming chamber 22 can be controlled by controlling the temperature of cooling water of the water cooling layer II 23.
The gas cooling pipe 21 is provided with the gas inlet 6, the gas inlet 6 extends to the outside of the powder forming chamber 22, gas nozzles 213 are uniformly distributed on the gas cooling pipe 21, the gas cooling pipe 21 is filled with an inert gaseous cooling medium, when nucleated metal vapor enters the powder forming chamber 22, the nucleated metal vapor rapidly permeates into the powder forming chamber 22 and fully contacts with low-temperature inert gaseous cooling medium sprayed by the gas cooling pipe 21 in a mixing manner to perform heat exchange, so that metal particles in the powder forming chamber 22 are rapidly cooled, a water cooling layer II 23 on the outer wall of the powder forming chamber 22 and the gas cooling pipe 21 are combined inside and outside, the temperature of each position in the powder forming chamber 22 can be rapidly controlled, the continuous growth or agglomeration of the metal particles is avoided, the particle size range of the metal particles is controlled within a certain range, the powder forming speed is faster, and the particle size is uniform; compared with the traditional single temperature control mode, the metal vapor can be quickly nucleated and quickly cooled to a certain temperature.
The gas flow formed by the inert gaseous cooling medium sprayed by the gas cooling pipe 21 can further disperse the nucleated metal vapor entering the powder forming chamber 22, so that the temperature of the nucleated metal vapor is more easily reduced, and the continuous growth or agglomeration of metal particles is further avoided, and the particle size of the powder is more uniform.
The temperature of the water cooling layer II 23, the temperature of the gaseous cooling medium in the gas cooling pipe 21 and the flow of the gaseous cooling medium are specifically changed to adjust the temperature and the cooling speed in the powder forming chamber 22, or the temperature and the cooling speed in the powder forming chamber are controlled by changing the size proportion of the components, and various temperature control modes are adopted, so that the range of the temperature control mode and the cooling speed are larger than those of the traditional mode, the speed is faster, the metal vapor can be effectively nucleated and grown into superfine metal powder with a certain particle size range, the generation of large particles and the particle agglomeration phenomenon are effectively reduced, the loss of products in the equipment is reduced, and the method is suitable for batch continuous production.
The heat preservation layer 12 is arranged on the outer wall of the first water cooling layer 13, so that the cold energy loss is avoided, the temperature control effect is further ensured, the metal gas nucleation tube 1 comprises an inner pipeline 11, the heat preservation layer 12 and the first water cooling layer 13, and the purpose of controlling the nucleation speed can be achieved by controlling the thickness of the inner pipeline 11, the heat preservation layer 12 and the first water cooling layer 13. The heat preservation layer 12 is a ceramic felt heat preservation layer, a carbon felt heat preservation layer or other high temperature resistant heat preservation materials.
The first inner pipeline 11 of the nucleation pipe 1 is a horn-shaped pipeline with a large feed inlet 4 and a small discharge outlet 5, accords with the fluid principle, accelerates the material flowing speed in the channel along the flowing direction, ensures that the atom nucleation is more uniform to a certain extent, is relatively straight-barrel type, can reduce the atom nucleation time and reduces the probability of generating large metal particles.
The first inner pipeline, the heat-insulating layer and the first water-cooling layer of the nucleation pipe 1 are coaxial pipelines, the ratio of the outer diameter A of the first inner pipeline to the outer diameter B of the heat-insulating layer on the same section is 1:1-4, and the ratio of the outer diameter A of the first inner pipeline 11 to the outer diameter C of the first water-cooling layer on the same section is 1:1-15. The ratio of the inner diameter of the feed inlet to the inner diameter of the discharge outlet at the two ends of the nucleation tube is 1:1-2. The ratio of the length D of the nucleation tube to the length E of the powder forming chamber of the condenser powder is 1:0.5-50, the ratio of the average diameter of the nucleation tube to the length D of the nucleation tube is 1:1-50, and the ratio of the minimum inner diameter Amin of the nucleation tube to the maximum inner diameter G of the powder forming chamber of the condenser powder 2 is 1: 1-30, the size ratio of the components can be adjusted to control the temperature and the cooling speed in the powder chamber, and the flow speed of the air flow in the whole device can be adjusted. If the nucleation tube 1 is too long, the metal is excessively nucleated to generate large-particle powder, and if the inner diameter of the powder forming chamber 22 is too large, the metal vapor cannot be uniformly diffused into the component chamber, so that the particle size distribution of the powder is wide.
The number of the gas cooling pipes which are arranged in parallel in the powder forming chamber is more than 3.
The gas cooling pipe is of a double-layer pipe structure and comprises an inner pipe and an outer pipe, a water cooling layer IV is arranged inside the inner pipe, a gas flowing layer is arranged between the outer pipe and the inner pipe, gas nozzles are arranged on the surface of the outer pipe, the arc of the gas nozzles on the outer pipe corresponds to the outer circle center angle of the gas flowing layer to be 15-45 degrees, the ratio of the inner diameter K of the water cooling layer of the gas cooling pipe to the outer diameter H of the gas flowing layer is 1:1-4, 2-4 gas nozzles are arranged at the same cross section position of the outer pipe 8 of the gas flowing layer along the circumferential direction, the total number of the gas nozzles is 30-200, and the temperature in the powder chamber can be controlled by adjusting the size proportion of the components. Too large an outer diameter of the gas flow layer 211 tends to cause insufficient cooling of the gas, and the gas temperature is not low enough to quench the metal.
The powder forming chamber 22 is in a bullet shell shape, one end, which is close to the metal gas nucleation tube 1, is in a cylindrical structure, and one end, which is close to the discharge tube 3, is in an arc funnel structure. The method accords with the principle of fluidics, reduces the residual loss of the superfine metal powder in the powder forming chamber 22 and on the pipeline, and improves the yield of the metal powder. The gas cooling pipe 21 is of a double-layer pipe structure and comprises an inner pipe 7 and an outer pipe 8, a water cooling layer IV 212 and a gas flow layer 211 between the outer pipe 8 and the inner pipe 7 are arranged inside the inner pipe 7, and a gas nozzle 213 is arranged on the outer pipe 8, so that the temperature of the water cooling layer IV 212 can be further controlled, and the temperature of an inert gaseous cooling medium of the gas flow layer 211 can be further controlled.
The connection part of the nucleation tube 1 and the powder forming chamber 22 is in a horn mouth shape, which is beneficial to the rapid diffusion of nucleated metal vapor into the powder forming chamber 22 after entering the powder forming chamber 22, and the metal vapor is fully mixed and contacted with the ejected low-temperature inert gas for heat exchange.
The method comprises the steps of introducing circulating water cooled by an external heat exchanger into pipelines of a first water cooling layer, a second water cooling layer 23, a third water cooling layer 31 and a fourth water cooling layer 212, regulating the temperature of the circulating water through the heat exchanger, introducing gas into a gas cooling pipe 21, opening an external blower, enabling metal gas evaporated by a front-end high-temperature evaporator to enter a nucleation pipe 1 under the carrying of carrier gas, enabling metal atoms to accumulate and nucleate in the nucleation pipe 1, then enter a shock condenser, enabling the nucleated metal particles to further grow up in a powder forming chamber 22, fully contacting and mixing cooling gas sprayed out of a gas nozzle 213 on a gas flowing layer 211 of the gas cooling pipe 21 with the temperature of the second water cooling layer 21, rapidly reducing the temperature to 50-200 ℃ under the synergistic effect of the second water cooling layer and the fourth water cooling layer, enabling the metal powder to stop growing up at the rear end of the powder forming chamber by a temperature sensor or an infrared thermometer, enabling the metal powder to continuously nucleate into large particles or agglomerate into large powder clusters, and forming the required metal powder into superfine metal powder with a certain particle size range through experiment, and enabling the required particle size to be in the gas cooling pipe 21 to correspond to the particle size of the cooling medium or the gas phase size of the metal powder to the required cooling medium.
In example 2, based on example 1, the ratio of the inner diameter K of the water cooling layer of the gas cooling tube 21 to the outer diameter H of the gas flow layer 211 was 1:3, and the outer tube 8 of the gas flow layer 211 was provided with 3 gas spouts 213 in the circumferential direction at the same cross-sectional position, and 270 gas spouts 213 were provided in total. The first inner pipe 11, the heat insulating layer 12 and the first water cooling layer 13 of the nucleation pipe 1 are coaxial pipes, the ratio of the outer diameter A of the first inner pipe 11 to the outer diameter B of the heat insulating layer 12 on the same section is 1:1.1, and the ratio of the outer diameter A of the first inner pipe 11 to the outer diameter C of the water cooling layer on the same section is 1:3. The ratio of the inner diameter of the feed inlet 4 to the inner diameter of the discharge outlet 5 at the two ends of the nucleation tube 1 is 1:1.5. The ratio of the length D of the nucleation tube 1 to the length E of the powdering chamber 22 of the condenser 2 is 1:20, the ratio of the average diameter of the nucleation tube 1 to the length D of the nucleation tube 1 is 1:5, and the ratio of the minimum inner diameter Amin of the nucleation tube 1 to the maximum inner diameter G of the powdering chamber 22 of the condenser 2 is 1:10. The first water cooling layer 13, the second water cooling layer 23, the third water cooling layer 31 and the fourth water cooling layer 212 are respectively connected with circulating cooling water cooled by an external heat exchanger, the temperature of the cooling water in the second water cooling layer 23 is controlled to be lower than 40 ℃, the temperature of the cooling water in the fourth water cooling layer 212 is controlled to be 30 ℃, the gas cooling pipe 21 is connected with an inert gas cooling medium, the input temperature of the gas cooling medium is controlled to be 30 ℃, and the flow rate of the gas cooling medium is controlled to be 100
And (h), turning on an external blower, enabling metal vapor to enter the device from a feed pipe of a first pipeline 11 in the nucleation pipe 1 under the action of air flow, cooling and nucleating the metal vapor through the nucleation pipe 1, then entering a powder forming chamber 22, fully contacting and mixing the powder forming chamber with an inert gaseous cooling medium sprayed out of the gas nozzle 213, and rapidly cooling the temperature detected by a temperature sensor or an infrared thermometer arranged at the discharge pipe 3 to below 160 ℃ to ensure that the metal particles cannot be continuously nucleated into large particles or agglomerated into large powder clusters, thereby preparing the metal powder with the diameter smaller than 100nm.
Example 3 in practiceBased on example 1, the ratio of the water cooling layer inner diameter K of the gas cooling tube 21 to the outer diameter H of the gas flow layer 211 was 1:3, and the outer tube 8 of the gas flow layer 211 was provided with 3 gas spouts 213 in the circumferential direction at the same cross-sectional position, and 270 gas spouts 213 in total. The first inner pipe 11, the heat insulating layer 12 and the first water cooling layer 13 of the nucleation pipe 1 are coaxial pipes, the ratio of the outer diameter A of the first inner pipe 11 to the outer diameter B of the heat insulating layer 12 on the same section is 1:1.1, and the ratio of the outer diameter A of the first inner pipe 11 to the outer diameter C of the water cooling layer on the same section is 1:3. The ratio of the inner diameter of the feed inlet 4 to the inner diameter of the discharge outlet 5 at the two ends of the nucleation tube 1 is 1:1.5. The ratio of the length D of the nucleation tube 1 to the length E of the powdering chamber 22 of the condenser 2 is 1:20, the ratio of the average diameter of the nucleation tube 1 to the length D of the nucleation tube 1 is 1:5, and the ratio of the minimum inner diameter Amin of the nucleation tube 1 to the maximum inner diameter G of the powdering chamber 22 of the condenser 2 is 1:10. The first water cooling layer 13, the second water cooling layer 23, the third water cooling layer 31 and the fourth water cooling layer 212 are respectively connected with circulating cooling water cooled by an external heat exchanger, the temperature of the cooling water in the second water cooling layer 23 is controlled to be below 50 ℃, the temperature of the cooling water in the fourth water cooling layer 212 is controlled to be 40-50 ℃, an inert gaseous cooling medium is led into the gas cooling pipe 21, the input temperature of the gaseous cooling medium is controlled to be 40 ℃, and the flow rate of the gaseous cooling medium is controlled to be 70
And (h), turning on an external blower, enabling metal vapor to enter the device from a feed pipe of a first pipeline 11 in the nucleation pipe 1 under the action of air flow, cooling and nucleating the metal vapor through the nucleation pipe 1, then entering a powder forming chamber 22, fully contacting and mixing the metal vapor with an inert gaseous cooling medium sprayed out of the gas nozzle 213, rapidly cooling the temperature detected by a temperature sensor or an infrared thermometer arranged at the discharge pipe 3 to below 200 ℃, and enabling the metal particles not to be nucleated into large particles or agglomerated into large powder clusters continuously, thus preparing the metal powder with the diameter smaller than 200nm.
In example 4, based on example 1, the ratio of the inner diameter K of the water cooling layer of the gas cooling tube 21 to the outer diameter H of the gas flow layer 211 was 1:2.5, and the outer tube 8 of the gas flow layer 211 was provided with 3 gas spouts 213 in the circumferential direction at the same cross-sectional position, and a total of 80 gas spouts 213. The inner pipeline I11, the heat preservation layer 12 and the water cooling layer I13 of the nucleation pipe 1 are coaxialThe ratio of the outer diameter A of the first inner pipeline 11 to the outer diameter B of the heat preservation layer 12 on the same section is 1:1.05, and the ratio of the outer diameter A of the first inner pipeline 11 to the outer diameter C of the water cooling layer on the same section is 1:2. The ratio of the inner diameter of the feed inlet 4 to the inner diameter of the discharge outlet 5 at the two ends of the nucleation tube 1 is 1:1.4. The ratio of the length D of the nucleation tube 1 to the length E of the powdering chamber 22 of the condenser 2 is 1:15, the ratio of the average diameter of the nucleation tube 1 to the length D of the nucleation tube 1 is 1:4, and the ratio of the minimum inner diameter Amin of the nucleation tube 1 to the maximum inner diameter G of the powdering chamber 22 of the condenser 2 is 1:10. The first water cooling layer 13, the second water cooling layer 23, the third water cooling layer 31 and the fourth water cooling layer 212 are respectively connected with circulating cooling water cooled by an external heat exchanger, the temperature of the cooling water in the second water cooling layer 23 is controlled to be below 50 ℃, the temperature of the cooling water in the fourth water cooling layer 212 is controlled to be 40-50 ℃, an inert gaseous cooling medium is led into the gas cooling pipe 21, the input temperature of the gaseous cooling medium is controlled to be 40 ℃, and the flow rate of the gaseous cooling medium is controlled to be 70
And (h), turning on an external blower, enabling metal vapor to enter the device from a feed pipe of a first pipeline 11 in the nucleation pipe 1 under the action of air flow, cooling and nucleating the metal vapor through the nucleation pipe 1, then entering a powder forming chamber 22, fully contacting and mixing the metal vapor with an inert gaseous cooling medium sprayed out of the gas nozzle 213, rapidly cooling the temperature detected by a temperature sensor or an infrared thermometer arranged at the discharge pipe 3 to below 200 ℃, and enabling the metal particles not to be nucleated into large particles or agglomerated into large powder clusters continuously, thus preparing the metal powder with the diameter smaller than 400nm.
In summary, the solution can control the temperature inside the powder forming chamber or the cooling speed by changing the temperature inside the powder forming chamber and the cooling speed, specifically, cooling water with different temperatures is introduced into the water cooling layer, gaseous cooling media with different temperatures are introduced into the gas cooling pipe, and gaseous cooling media with different flow rates are introduced into the gas cooling pipe to control the temperature inside the powder forming chamber, or the temperature inside the powder forming chamber or the cooling speed is controlled by changing the size proportion of the components, and the temperature control range and the cooling speed are larger than those of the traditional mode, so that the speed is faster, the metal vapor can be quickly nucleated and grow into superfine metal powder with a certain particle size range, the generation of large particles and the particle agglomeration phenomenon are effectively reduced, the loss of products inside the equipment is reduced, and the solution is suitable for batch continuous production.
The foregoing is only illustrative of the preferred embodiments of the present utility model.
Claims (8)
1. The metal vapor quenching nucleation and powdering device is characterized by comprising a nucleation tube (1), wherein two ends of the nucleation tube (1) are respectively provided with a feed inlet (4) and a discharge outlet (5), the nucleation tube (1) comprises an inner pipeline I (11) and a water cooling layer I (13) positioned on the outer wall of the inner pipeline I (11), an outlet of the nucleation tube (1) is connected with a quenching powder container (2), the quenching powder container (2) comprises a powdering chamber (22), a gas cooling tube (21) positioned inside the powdering chamber (22) and a water cooling layer II (23) positioned on the outer wall of the powdering chamber (22), the nucleation tube (1) is communicated with the inside of the powdering chamber (22), the powdering chamber (22) is connected with a discharge tube (3), the discharge tube (3) comprises an inner pipeline II (32) and a water cooling layer III (31) positioned on the outer wall of the inner pipeline II (32), the gas cooling tube (21) is provided with a gas inlet (6), the gas inlet (6) extends to the outside the powdering chamber (22), and gas nozzles (213) are uniformly distributed on the gas cooling tube (21); the powder forming chamber (22) is in a bullet shell shape, one end, which is close to the nucleation tube (1), is in a cylindrical structure, and the end, which is close to the discharge tube (3), is in an arc funnel structure; the gas cooling pipes (21) are arranged in parallel in the powder forming chamber (22) along the material flowing direction in a reciprocating and uniform way, and the cooling pipes in parallel in the powder forming chamber (22) are sequentially communicated through arc-shaped pipelines.
2. The metal vapor quenching nucleation and powdering device according to claim 1, wherein an insulation layer (12) is arranged on the outer wall of the water cooling layer I (13), and the insulation layer (12) is a ceramic felt insulation layer (12) or a carbon felt insulation layer (12).
3. The metal vapor quenching nucleation and powdering device according to claim 2, wherein the first inner pipe (11) of the nucleation pipe (1) is a horn-shaped pipe with a large feed inlet (4) and a small discharge outlet (5), the first inner pipe (11), the heat insulating layer (12) and the first water cooling layer (13) of the nucleation pipe (1) are coaxial pipes, the ratio of the outer diameter A of the first inner pipe (11) to the outer diameter B of the heat insulating layer (12) on the same section is 1:1-4, the ratio of the outer diameter A of the first inner pipe (11) to the outer diameter C of the first water cooling layer (13) on the same section is 1:1-15, the ratio of the inner diameter of the feed inlet (4) to the inner diameter of the discharge outlet (5) at both ends of the nucleation pipe (1) is 1:1-2, the ratio of the length D of the nucleation pipe (1) to the length E of the powdering chamber (22) of the shock condenser (2) is 1:0.5-50, the ratio of the average diameter D of the nucleation pipe (1) to the length D of the nucleation pipe (1) is 1:1-50, and the inner diameter C of the minimum shock pipe (1) to the inner diameter C of the shock condenser (22) is the maximum powder (2). 1-30.
4. A metal vapor quenching nucleation and powdering device as claimed in claim 2, wherein the number of the gas cooling pipes (21) arranged in parallel in the powdering device (22) is more than 3.
5. The metal vapor quenching nucleation and powdering device according to claim 3, wherein the gas cooling tube (21) is of a double-layer tube structure and comprises an inner tube and an outer tube (8), the inner tube is internally provided with a water cooling layer IV (212) and a gas flow layer between the outer tube (8) and the inner tube, the gas nozzles (213) are positioned on the surface of the outer tube (8), the radian of the gas nozzles (213) on the outer tube (8) corresponds to the excircle center angle of the gas flow layer (211) to be 15-45 degrees, the ratio of the water cooling layer inner diameter K of the gas cooling tube (21) to the gas flow layer outer diameter H is 1:1-4, 2-4 gas nozzles (213) are arranged at the same section position of the outer tube (8) of the gas flow layer (211) along the circumferential direction, and the total number of the gas nozzles (213) is 30-200.
6. A metal vapor quenching nucleation and powdering device according to claim 5, wherein the junction of the nucleation tube (1) and the powdering chamber (22) is flared.
7. The metal vapor quenching nucleation powder particle diameter control method is characterized in that metal vapor is connected into a feed port (4) of a nucleation pipe (1) in the metal vapor quenching nucleation powder device according to claim 6, the temperature and the cooling speed inside a powder chamber (22) are changed to be controlled to be the powder particle diameter, specifically, the temperature and the cooling speed inside the powder chamber (22) are changed to be two modes, firstly, cooling water with different temperatures is introduced into a water cooling layer II (23), gaseous cooling media with different temperatures are introduced into a gas cooling pipe (21), and the gaseous cooling media with different flow rates are introduced into the gas cooling pipe (21) to be controlled to be the temperature inside the powder chamber (22); second, the ratio of the outer diameter A of the first inner pipeline (11) to the outer diameter B of the heat insulation layer (12), the ratio of the outer diameter A of the first inner pipeline (11) to the outer diameter C of the first water cooling layer (13), the ratio of the inner diameter of the feed port (4) to the inner diameter of the discharge port (5) at the two ends of the nucleation pipe (1), the ratio of the length D of the nucleation pipe (1) to the length E of the powder forming chamber (22) of the condenser powder (2), the ratio of the average diameter of the nucleation pipe (1) to the length D of the nucleation pipe (1), and the minimum inner diameter A of the nucleation pipe (1) are adjusted min The ratio of the gas jet nozzle to the maximum inner diameter G of the powder forming chamber (22) of the shock condenser (2), the number of the gas jet nozzles (213), the circle center angle of the outer circle of the gas flow layer corresponding to the radian of the gas jet nozzles (213) on the outer tube (8), and the ratio of the inner diameter K of the water cooling layer of the gas cooling tube (21) to the outer diameter H of the gas flow layer.
8. The method for controlling particle diameter of metal vapor quenching nucleation as defined in claim 7, wherein said gaseous cooling medium is nitrogen, argon, helium, hydrogen or a mixture of said 2 gases.
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