CN117161391B - Preparation device and preparation method of high-laser-absorptivity metal powder - Google Patents
Preparation device and preparation method of high-laser-absorptivity metal powder Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a preparation device and a preparation method of high laser absorptivity metal powder, belongs to the field of powder material preparation, combines a sorting and powder feeding technology, a remelting spheroidization technology and an anti-adhesion device of raw material powder to prepare spherical powder, and can be used for producing graphene composite metal spherical powder raw materials with controllable particle size distribution according to specific requirements in one step, can be used for powder forming modes such as compression forming and injection forming and as 3D printing powder materials, solves the technical problem of difficult preparation of 3D printing powder, and provides a simple and convenient low-cost raw material preparation mode for preparation and application of high-quality graphene composite metal materials.
Description
Technical Field
The invention relates to the field of powder material preparation, in particular to a preparation device and a preparation method of high-laser-absorptivity metal powder.
Background
Metal powder, particularly spherical metal powder, is widely used in new manufacturing fields such as 3D printing, injection molding, and the like. 3D printing is one of the most invested specific gravity and the fastest development technologies in the advanced manufacturing industry field due to the characteristics of complex structure forming, rapid preparation, high strength and light weight and high material utilization rate. The requirements of 3D printing on metal powder are mainly high purity, good sphericity, narrow particle size distribution, low oxygen content and good fluidity. With the development of various powder forming technologies, the demand for high-quality and low-cost spherical powder is growing.
However, the existing 3D printing metal powder preparation still has the following defects:
(1) The prior art is suitable for 3D printing, and the metal powder yield is lower, and the grain size distribution range is not adjustable.
In metal 3D printing, powder particle size distribution is a very important parameter. First of all, it relates to powder flowability and compactibility during printing. The reasonable powder particle size distribution has smaller gaps among particles, and is favorable for realizing higher compactness and uniform material deposition, thereby improving the printing quality. Secondly, uneven powder particle size distribution can also lead to increased roughness of the printed surface, as larger particle size particles can form raised or roughened spots on the surface, reducing the surface quality of the printed part. In addition, the compactness of the powder can also affect the mechanical properties of the printing material. In the prior art, the yield of the metal powder suitable for 3D printing is less than 50%, and the distribution range of the powder is regulated and controlled in a mode of sieving and mixing the prepared spherical powder for secondary compounding, so that the risk of increasing the oxygen content of the powder is certainly increased.
(2) The 3D printing old powder is difficult to recycle with low cost
In the process of repeatedly 3D printing, the metal powder is subjected to high-temperature sintering for many times to gradually increase the particle size and the oxygen content, and the metal powder presents the states of slender particles, satellite powder, irregularly-shaped particles and the like, is limited by the raw material requirement and high cost of the existing powder manufacturing technology, and old powder is often sold at low price and is not used for 3D printing.
(3) The laser absorptivity of part of metal powder is low, and the 3D printing forming efficiency is low
The lower laser absorptivity of the metal powder directly leads to laser energy dissipation in the 3D printing process, the temperature of a molten pool is too low, and formed products can have defects of unfused, holes, low density and the like, so that the mechanical, heat conduction and electric conduction properties of formed parts are further affected. The absorptivity of pure copper powder such as 15-53um range to 1064nm wavelength laser is 22%, so that pure copper still has some challenges in the application field of additive manufacturing.
In addition, the existing spherical metal powder preparation method mainly comprises an air atomization method, a plasma rotating electrode atomization method, a plasma fuse wire atomization method and the like, the powder preparation methods have advantages and disadvantages, the powder prepared by the air atomization method is wide in particle size distribution, multi-satellite powder and has air holes, the plasma rotating electrode atomization method is high in cost, alloy elements are easy to volatilize, the plasma fuse wire atomization raw material is a specific wire, and the powder types are limited.
Therefore, how to solve the conventional difficulties and defects of the preparation of the 3D printing metal powder and improve the laser absorptivity of the metal powder, and to obtain a printing product with excellent performance is an important direction of technical development in the field.
Graphene is one of the thinnest and most rigid materials in the world at present, and the specific surface area of the graphene can reach 2630m 2 /g, carrier mobility up to 2X 10 5 cm 2 ·V -1 ·S -1 The thermal conductivity reaches 5000 W.m -1 K -1 . The excellent properties of graphene can be utilized to endow the new material with more excellent properties, such as mechanical properties, conductive heat dissipation properties and the like, through compounding with a metal material. The absorptivity of pure copper powder such as 15-53um range to 1064nm wavelength laser is 22%, so that pure copper still has some challenges in the application field of additive manufacturing. The carbon material modification is a mode for better improving the laser absorptivity, and in consideration of the defect of the existing 3D printing metal powder, the graphene carbon material can be used for coating the metal powder to obtain graphene metal powder, so that the laser absorptivity can be improved, and the carbon material modification is a mode for better improving the laser absorptivity not only corresponding to copper.
However, most of the current methods for preparing graphene composite metal materials on a large scale are physical blending, and the problems of two-phase dispersibility and compatibility cannot be solved in the method, and are limited by the quality of graphene powder raw materials, so that the prepared composite material cannot exert the excellent performance of graphene.
In addition, the spherical graphene metal powder is difficult to continuously produce. The remelting spheroidizing furnace adopts an external heating mode, molten micro-nano metal particles are easy to adhere to the inner wall with higher temperature, so that the particles are accumulated and fall, spherical powder of independent particles cannot be obtained, and the growth of graphene on the surfaces of the particles can be influenced.
Disclosure of Invention
In view of the above technical problems, the present invention provides a device for preparing metal powder with high laser absorptivity, comprising: the powder feeding device is arranged at the top of the furnace body, and the collecting tank is arranged at the bottom of the furnace body;
the powder feeding device comprises a powder feeding funnel, a powder feeding cavity, a vibration powder feeder and a powder feeding valve, wherein the powder feeding funnel is used for feeding raw powder, the lower part of the powder feeding funnel is communicated with the powder feeding cavity, the powder feeding valve is arranged at the tail end of the powder feeding cavity and connected with the inlet of the furnace body and used for controlling the raw powder to fall into the furnace body, and the vibration powder feeder is arranged at the inlet of the powder feeding valve and used for controlling the speed of feeding the raw powder into the powder feeding valve;
the inside of the furnace body comprises a reaction chamber and a powder rapid cooling chamber, the reaction chamber is arranged above the powder rapid cooling chamber, the bottom of the reaction chamber is communicated with a second gas inlet, the second gas inlet is used for introducing carbon-containing source gas, the top of the second gas inlet is communicated with a gas outlet, and a heating rod is arranged on the furnace body wall corresponding to the reaction chamber;
the furnace body wall that the reaction chamber corresponds is the intermediate layer furnace chamber, the intermediate layer furnace chamber includes ventilative interior boiler tube and furnace body heat preservation shell, the furnace body heat preservation shell is located the outer of ventilative interior boiler tube, leave the space between the two, the space intercommunication has a first gas inlet, first gas inlet is used for letting in inert gas, intermediate layer furnace chamber internal pressure is greater than all the time the pressure in the reaction chamber.
Preferably, the inside of advancing the powder cavity is equipped with sorting unit, sorting unit locates advance the below of powder funnel, will follow advance the metal powder that powder funnel carried and carry out target particle diameter screening, carry again to send powder valve department, sorting unit top-down includes one-level powder separation screen cloth, powder guide plate and second grade powder separation screen cloth in proper order, the mesh size of one-level powder separation screen cloth is greater than the mesh size of second grade powder separation screen cloth, the powder guide plate is located the end of one-level powder separation screen cloth with one-level powder separation screen cloth is anticlockwise contained angle, will follow the metal powder water conservancy diversion of one-level powder separation screen cloth sieve fall to on the second grade powder separation screen cloth. The powder feeding valve comprises a primary powder feeding valve, a secondary powder feeding valve and a tertiary powder feeding valve, the vibration powder feeder comprises a primary powder feeding vibrator, a secondary powder feeding vibrator and a tertiary powder feeding vibrator, the tail end of the primary powder sorting screen is connected with the primary powder feeding vibrator and is communicated with the primary powder feeding valve, the tail end of the secondary powder sorting screen is connected with the secondary powder feeding vibrator and is communicated with the secondary powder feeding valve, and the bottom wall of the powder feeding cavity is connected with the tertiary powder feeding vibrator and is communicated with the tertiary powder feeding valve.
Preferably, a rotary dispersion disc is arranged at the top of the reaction chamber, and the height of the rotary dispersion disc is lower than that of the three-level powder feeding valve.
Preferably, the porosity of the breathable inner furnace tube is 5% -50%, and the pore size is 100 nanometers to 50 microns.
The preparation method for preparing the metal powder with high laser absorptivity by using the preparation device for the metal powder with high laser absorptivity comprises the following steps:
s1, vacuumizing a device, opening the first gas inlet and the gas outlet, introducing inert gas into the interlayer furnace chamber from the first gas inlet, uniformly diffusing the inert gas into the reaction chamber through the ventilation inner furnace tube, maintaining positive pressure in the interlayer furnace chamber, and heating the reaction chamber to a standard atmospheric pressure by a heating rod at the same time until the temperature reaches a first temperature, wherein the first temperature is 0-2800 ℃, and a heating zone is formed in the reaction chamber;
s2, adding raw material powder from a powder feeding funnel, screening the raw material powder into a plurality of different particle size intervals by using a sorting device, opening a second gas inlet to introduce carbon source-containing gas, determining and opening a powder feeding valve of a corresponding level according to the particle size interval to which the raw material powder belongs, so that the powder falls on the rotary dispersion disc below the three-level powder feeding valve, and uniformly dispersing the powder by using the rotary dispersion disc;
s3, after powder enters the reaction chamber from the rotary dispersion disc, the powder falls into a heating zone to form molten metal particles, carbon source-containing gas enters the heating zone from bottom to top to contact with the molten metal particles, a graphene film is generated on the surface of the powder while remelting and spheroidizing the particles, and the molten metal particles with the surface of which is formed with the graphene film continuously fall into the powder rapid cooling chamber and finally enter the collection tank to be collected;
and S4, after the reaction is completed, stopping powder feeding by the powder feeding device, closing the second gas inlet, continuously introducing inert gas from the first gas inlet, and sealing and sub-packaging the graphene metal powder in the collecting tank after the reaction chamber is cooled to room temperature.
In S2, the method also comprises grading, wherein the grading is used in occasions needing a certain particle size distribution ratio, and the sorted raw material powder is mixed according to a preset ratio by opening different powder feeding valves.
Preferably, the raw material powder is recycled 3D printing old powder.
Preferably, the gas introduced into the first gas inlet is a mixed gas comprising inert gas and hydrogen.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention has low cost, can realize continuous high-quality preparation of metal powder, avoids formation of satellite powder and air hole powder, and can ensure that the grain size of the obtained 3D printing powder material is controllable by 100 percent through screening the grain size of the raw materials.
2. The device can effectively recycle the 3D printing old powder, takes the old powder as raw material powder of the device, can be re-sphericized, reduces the oxygen content by utilizing hydrogen generated by methane decomposition, and further recycles the waste powder into the 3D printing powder material with high added value.
3. The invention designs the interlayer furnace chamber, and the inert atmosphere is introduced to form positive pressure, so that the inert gas is uniformly diffused into the reaction chamber through the inner furnace tube, and the metal powder can be effectively prevented from being adhered to the inner wall of the furnace tube and the carbon-containing gas can be effectively prevented from being decomposed and deposited on the inner furnace tube with higher temperature.
4. The graphene layer is coated on the metal surface of the 3D printing powder material prepared by the method, so that the reflectivity of laser is reduced, and the forming efficiency and the product performance of a 3D printing product are improved.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic view showing the overall structure of a device for preparing a metal powder with high laser absorptivity according to the present invention;
FIG. 2 is an SEM image of copper powder used in the examples of the invention;
fig. 3 is an SEM image of graphene spherical copper powder prepared in an embodiment of the present invention;
fig. 4 is a Raman diagram of graphene spherical copper powder prepared in an embodiment of the present invention.
The figures represent the numbers:
1. the powder feeding hopper, 2, a primary powder sorting screen, 3, a powder guide plate, 4, a secondary powder sorting screen, 5, a vibration powder feeder, 6, a primary powder feeding valve, 7, a secondary powder feeding valve, 8, a tertiary powder feeding valve, 9, a rotary dispersion disc, 10, an air outlet, 11, a reaction chamber, 12, an air-permeable inner furnace tube, 13, a heating rod, 14, a furnace body heat-insulating shell, 15, a powder quick cooling chamber, 16, a collecting tank, 17, a first gas inlet, 18 and a second gas inlet.
Detailed Description
Various aspects of the invention are described in further detail below.
As shown in fig. 1, the present invention provides an apparatus for preparing metal powder with high laser absorptivity, comprising: furnace body, locate the powder device that send at furnace body top and locate collection tank 16 of furnace body bottom: the powder feeding device comprises a powder feeding funnel 1, a powder feeding cavity, a vibrating powder feeder 5 and a powder feeding valve, wherein the powder feeding funnel 1 is used for feeding raw powder, the lower part of the powder feeding funnel 1 is communicated with the powder feeding cavity, the powder feeding valve is arranged at the tail end of the powder feeding cavity and connected with the inlet of the furnace body and used for controlling metal powder to fall into the furnace body, and the vibrating powder feeder 5 is arranged at the inlet of the powder feeding valve and used for controlling the flow and the speed of the raw powder fed into the powder feeding valve; the furnace body inside includes reaction chamber 11 and quick cold room 15 of powder, and the top of quick cold room 15 of powder is located to reaction chamber 11, and the furnace body wall that reaction chamber 11 corresponds is a intermediate layer furnace chamber, can be equipped with heating rod 13 in the intermediate layer furnace chamber as the heating device of furnace body, the position of heating rod 13 not only is limited to in the intermediate layer furnace chamber, only need can realize the position that the furnace body heated.
When the furnace body adopts a conventional vertical smelting furnace to process spherical metal powder, the spherical metal powder enters the powder feeding cavity from the powder feeding hopper 1, the powder is required to be fed on the inclined plane in a vibrating way due to the working characteristic of the vibrating powder feeder 5, and the raw material powder is uniformly and controllably conveyed to the powder feeding valve from the inclined plane through continuous vibration.
As a preferred embodiment, the powder inlet cavity is not directly arranged right above the vertical smelting furnace, but is arranged on the top side wall of the vertical smelting furnace in a deflection mode.
As a preferred embodiment, a sorting device is arranged in the powder feeding cavity, the sorting device is arranged below the powder feeding funnel 1, metal powder conveyed from the powder feeding funnel 1 is subjected to target particle size screening and then conveyed to a powder conveying valve, the sorting device sequentially comprises a primary powder sorting screen 2, a powder guide plate 3 and a secondary powder sorting screen 4 from top to bottom, the mesh size of the primary powder sorting screen 2 is larger than that of the secondary powder sorting screen 4, the powder guide plate 3 is arranged at the tail end of the primary powder sorting screen 2, an included angle is formed between the powder guide plate and the primary powder sorting screen 2 in a anticlockwise direction, and the metal powder sieved from the primary powder sorting screen 2 is guided onto the secondary powder sorting screen 4.
The sorting device is used for selecting the grain size of raw material powder according to processing requirements, two screens with different apertures are arranged up and down, the mesh size of the primary powder sorting screen 2 is larger than that of the secondary powder sorting screen 4, and raw material powder with the grain size smaller than that of the primary powder sorting screen 2 falls onto the secondary powder sorting screen 4 from the meshes. Because the screen cloth has a certain length, advances to divide the cavity to be the inclined plane again, and the small-size raw materials powder that sieves is piled up at the afterbody of secondary powder separation screen cloth 4 under the action of gravity easily, can't thoroughly sieve on secondary powder separation screen cloth 4, consequently be equipped with powder guide plate 3 at the afterbody of primary powder separation screen cloth 2 in this embodiment, the length of powder guide plate 3 should not be too short, need guarantee to accept the most blanking of primary powder separation screen cloth 2 and leave a section distance at its front end to make things convenient for the raw materials powder that powder guide plate 3 accepted to fall to the anterior part of secondary powder separation screen cloth 4 of below.
As a preferred embodiment, the powder feeding valve comprises a primary powder feeding valve 6, a secondary powder feeding valve 7 and a tertiary powder feeding valve 8, the vibration powder feeder 5 comprises a primary powder feeding vibrator, a secondary powder feeding vibrator and a tertiary powder feeding vibrator, the tail end of the primary powder sorting screen 2 is connected with the primary powder feeding vibrator and leads to the primary powder feeding valve 6, the tail end of the secondary powder sorting screen 4 is connected with the secondary powder feeding vibrator and leads to the secondary powder feeding valve 7, and the bottom wall of the powder feeding cavity is connected with the tertiary powder feeding vibrator and leads to the tertiary powder feeding valve 8.
Different powder feeding valves correspond to the selected raw material powder with different particle sizes for later use, when the raw material powder with a certain particle size is needed, the corresponding powder feeding valve is opened to feed the raw material powder into the reaction chamber 11, and when the raw material powder with different particle sizes is needed to be subjected to grading, the different powder feeding valves can be opened to carry out targeted mixing after screening by the screen.
As a preferred embodiment, a rotary dispersion disc 9 is arranged at the top of the reaction chamber 11, and the height of the rotary dispersion disc 9 is lower than that of the three-stage powder feeding valve 8.
The rotary dispersing disc 9 is arranged below the three-level powder feeding valve 8, namely, all the powder feeding valves are higher than the rotary dispersing disc 9, so that the raw material powder discharged at the powder feeding valves can be dispersed and discharged through the rotary dispersing disc 9, and the raw material powder is uniformly dispersed in the reaction chamber 11.
As a preferred embodiment, the interlayer furnace chamber comprises a ventilation inner furnace tube 12 and a furnace body heat-insulating shell 14, the furnace body heat-insulating shell 14 is arranged on the outer layer of the ventilation inner furnace tube 12 and is composed of a heat-insulating material and a metal shell, and a space is reserved between the ventilation inner furnace tube 12 and the furnace body heat-insulating shell 14 and is used for introducing inert gas. The space is communicated with a first gas inlet 17, the first gas inlet 17 is used for introducing inert gas, the bottom of the reaction chamber 11 is communicated with a second gas inlet 18, the second gas inlet 18 is used for introducing carbon source-containing gas, the top is communicated with a gas outlet 10, and the pressure in the interlayer furnace chamber is always greater than the pressure in the reaction chamber 11.
The material of the ventilation inner furnace tube 12 can be graphite, carbon-carbon composite material, metal, ceramic and the like, inert gas is introduced into the interlayer furnace chamber, and uniformly diffuses to the reaction chamber 11 through the ventilation inner furnace tube 12, so that the pressure in the interlayer furnace chamber is always greater than the pressure in the reaction chamber 11, and as the heating rod 13 is arranged in the interlayer furnace chamber, molten metal powder is easy to adhere to the inner wall of the furnace tube, pressure difference is created by the inert gas, the adhesion of the metal powder to the inner wall of the furnace tube can be effectively prevented, and meanwhile, the decomposition and deposition of carbon source-containing gas on the inner furnace tube with higher temperature can be avoided.
The invention also provides a preparation method for preparing the high-laser-absorptivity metal powder by using the preparation device for the high-laser-absorptivity metal powder, which comprises the following steps:
s1, vacuumizing the device, opening a first gas inlet 17 and a gas outlet 10, introducing inert gas into an interlayer furnace chamber from the first gas inlet 17 at a rate of 20-40L/min, wherein the inert gas is one or mixed gas of argon and nitrogen, uniformly diffusing the inert gas into the reaction chamber 11 through a ventilation inner furnace tube 12, maintaining positive pressure in the interlayer furnace chamber, keeping standard atmospheric pressure in the reaction chamber 11, heating by a heating rod 13 to a first temperature, forming a heating zone in the reaction chamber 11, and keeping the temperature of the heating zone at 1000-2600 ℃;
s2, adding raw material powder from a powder inlet funnel 1, wherein the raw material powder can be selected from simple substance metal powder, alloy powder or recovered 3D printing old powder produced by mechanical crushing, electrolysis, atomization and other modes; the raw material powder is screened into a plurality of different particle size intervals by a sorting device, a second gas inlet 18 is opened to be filled with carbon source gas, the carbon source gas filling rate is 0.4-1L/min, the carbon source gas is hydrocarbon, methane, ethane, propane, butane, ethylene, propylene, acetylene and the like are selected, meanwhile, when the carbon source gas is filled, inert gas can be filled into the second gas inlet 18 at the same time, the inert gas partial pressure is balanced, the inert gas can be one of argon and nitrogen or mixed gas, the filling rate is 0-10L/min, the volume ratio between the inert gas and the carbon source gas is 10-20 to 1, a corresponding-level powder feeding valve is opened, the powder falls on a rotary dispersion disc 9 below, the rotary dispersion disc 9 is used for uniformly dispersing, the rotating speed of the rotary dispersion disc 9 can be adjusted according to the different particle size of the raw material powder, and the falling rate of the raw material powder is 0-2kg/h;
s3, after raw material powder enters a reaction chamber 11 from a rotary dispersion disc 9, the raw material powder falls into a heating zone to form molten metal particles, carbon source-containing gas enters the heating zone from bottom to top to contact with the molten metal particles, a graphene film is generated on the surface while remelting and spheroidizing the particles, the molten metal particles with the surface of which the graphene film is generated continuously fall into a powder rapid cooling chamber 15, and finally enter a collection tank 16 to be collected;
and S4, stopping powder feeding by the powder feeding device after the reaction is completed, closing the second gas inlet 18, continuously introducing inert gas from the first gas inlet 17, and sealing and sub-packaging the graphene metal powder in the collecting tank 16 after the reaction chamber 11 is cooled to room temperature.
As a preferred embodiment, the sorting more specifically comprises:
the raw material powder falls to a first-stage powder sorting screen 2, and powder with the particle size larger than the mesh size of the first-stage powder sorting screen 2 cannot pass through the first-stage powder sorting screen to be first-stage powder, and is conveyed to a first-stage powder feeding valve 6 for standby under the action of a first-stage powder feeding vibrator;
the passable powder falls to the powder guide plate 3 from the first-stage powder separation screen 2, slides to the second-stage powder separation screen 4 from the inclined plane of the powder guide plate 3, and the powder with the particle size larger than the mesh size of the second-stage powder separation screen 4 cannot pass through to be the second-stage powder, and is conveyed to the second-stage powder feeding valve 7 for standby under the action of the second-stage powder feeding vibrator;
the powder which can pass through falls to the bottom of the powder feeding cavity from the secondary powder sorting screen 4 to be tertiary powder, and is conveyed to a tertiary powder feeding valve 8 for standby under the action of a tertiary powder feeding vibrator;
in other examples, a plurality of sorting screens may be provided to perform sorting for a plurality of times, and the sorted powder may be prepared separately or mixed according to a certain ratio, and then prepared after mixing, and in S2, the corresponding step further includes grading, and the grading is used in a case where a certain particle size distribution ratio is required, and the raw material powder is mixed according to a preset ratio by opening different powder feeding valves. If the prepared 3D printing powder material has layering requirements of different particle sizes, corresponding valves can be opened for feeding in different periods of reaction.
As a preferred embodiment, the porosity of the ventilation inner furnace tube 12 is 5% -50%, and the pore size is 100 nm-50 μm; the pressure of the interlayer furnace chamber after the inert gas is introduced is 0.1-5 MPa; the heating temperature of the heating rod 13 is 0-2800 ℃.
The invention also provides a preparation method for preparing the metal powder with high laser absorptivity by recycling the old powder of the 3D printing powder material, the old powder (namely the old 3D printing powder material which is deformed and cannot be used after being used) is taken as raw material powder to be put into the powder inlet funnel 1, the old powder falls into a heating zone, carbon source gas is decomposed at high temperature to generate hydrogen, hydrogen is used for reducing oxidized metal in the old powder, the reduced metal powder is in molten metal particles in the heating zone, graphene films are generated on the surface of the metal powder while the metal particles are remelted and spheroidized, and the graphene films continuously fall into the powder rapid cooling chamber 15 and then enter the collecting tank 16 for collection.
The spherical copper powder coated by graphene is prepared by using the device disclosed by the invention and can be used as an embodiment of the invention, and the specific steps are as follows:
s1, adjusting the initial pressure of the device, vacuumizing the device, opening a first gas inlet 17 and a gas outlet 10, introducing 30L/min nitrogen into a sandwich furnace chamber from the first gas inlet 17, ventilating the sandwich furnace chamber and a reaction chamber 11 to a complete nitrogen state, heating a heating rod 13, heating the reaction chamber 11 to 1300 ℃, introducing mixed gas of 8L/min nitrogen and 0.6L/min methane into a second gas inlet 18, maintaining positive pressure in the sandwich furnace chamber, and keeping standard atmospheric pressure in the reaction chamber 11;
s2, blanking and sorting raw material copper powder, namely, blanking the raw material copper powder from a powder inlet funnel 1, wherein the raw material copper powder is formed by an atomization method, a primary powder sorting screen 2 adopts a 60-micron pore diameter, raw material copper powder with the particle size smaller than 60 microns is selected, a secondary powder feeding valve 7 and a tertiary powder feeding valve 8 are opened, the raw material copper powder with the particle size smaller than 60 microns falls on a rotary dispersion disc 9 below, and then the rotary dispersion disc 9 uniformly scatters a reaction chamber 11 below, so that the raw material copper powder uniformly falls at a speed of 1 kg/h;
s3, carrying out reaction and collection, namely enabling raw copper powder to enter a reaction chamber 11, wherein the temperature of a heating area is 1300 ℃, enabling the raw copper powder to fall into the heating area to form molten copper powder particles, forming balls under the action of surface tension, enabling carbon source-containing gas to enter the heating area from bottom to top to contact with the molten copper powder particles, enabling the copper powder particles to form graphene films on the surfaces while remelting and spheroidizing, enabling the molten metal particles with the graphene films formed on the surfaces to continuously fall into a powder rapid cooling chamber 15 to be rapidly cooled, and then enabling the molten metal particles to enter a collection tank 16 to be collected;
and S4, finishing preparation, stopping powder feeding by the powder feeding device according to target production requirements after the reaction is finished, closing the second gas inlet 18, continuously introducing inert gas from the first gas inlet 17, cooling to room temperature in the reaction chamber 11, and sealing and sub-packaging the graphene spherical copper powder in the collection tank 16.
As a preferred embodiment, the gas introduced into the first gas inlet 17 is a mixed gas including an inert gas and hydrogen. The mixed gas comprising inert gas and hydrogen is introduced into the first gas inlet 17, so that the concentration of the hydrogen in the methane pyrolysis product can be increased, and the preparation effect of the graphene spherical copper powder is further improved.
The graphene-coated spherical copper powder prepared by the steps has good conductivity and is a high-quality raw material for compression molding, for example, the graphene-coated spherical copper powder is prepared byPutting the composite powder into a cold isostatic pressing die with the diameter of phi 25mm, and performing compression molding under the pressure of 280MPa to obtain a copper/graphene composite material block blank. And putting the obtained blank into a sintering furnace, sintering and forming under the protection of argon atmosphere, wherein the heating rate is 10 ℃/min, the thermal sintering temperature is 900 ℃, and the heat preservation time is 1.5 h. Carrying out hot extrusion on the sintered bar, and then testing to obtain the copper-alkene alloy with the conductivity of 97.4% IACS and the density of 8.71g/cm 3 It can be seen that it has good electrical conductivity.
As shown in fig. 2, the raw copper powders in the embodiment have different particle sizes and different shapes, and cannot be used as 3D printing powder, but the graphene spherical copper powder prepared by the device of the invention has smooth and regular spherical shape as shown in SEM (scanning electron microscope) fig. 3, good sphericity and narrow particle size distribution, and the raman spectrum of the graphene spherical copper powder prepared by the invention as shown in fig. 4 completely accords with the characteristic of graphene coating instead of graphite coating. In conclusion, the graphene spherical copper powder prepared by the method meets the requirement of high-quality graphene copper powder, and can be used for 3D printing.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation device of high laser absorptivity metal powder is characterized in that: comprises a furnace body, a powder feeding device arranged at the top of the furnace body and a collecting tank arranged at the bottom of the furnace body;
the powder feeding device comprises a powder feeding funnel, a powder feeding cavity, a vibration powder feeder and a powder feeding valve, wherein the powder feeding funnel is used for feeding raw powder, the lower part of the powder feeding funnel is communicated with the powder feeding cavity, the powder feeding valve is arranged at the tail end of the powder feeding cavity and connected with the inlet of the furnace body and used for controlling the raw powder to fall into the furnace body, and the vibration powder feeder is arranged at the inlet of the powder feeding valve and used for controlling the speed of feeding the raw powder into the powder feeding valve;
the furnace body comprises a reaction chamber and a powder rapid cooling chamber, the reaction chamber is arranged above the powder rapid cooling chamber, the bottom of the reaction chamber is communicated with a second gas inlet, the second gas inlet is used for introducing carbon-containing source gas, the top of the reaction chamber is communicated with a gas outlet, a heating rod is arranged on the furnace body wall corresponding to the reaction chamber, and after raw material powder enters the reaction chamber, the raw material powder falls into a heating zone to form molten metal particles;
the furnace body wall that the reaction chamber corresponds is the intermediate layer furnace chamber, the intermediate layer furnace chamber includes ventilative interior boiler tube and furnace body heat preservation shell, the furnace body heat preservation shell is located the outer of ventilative interior boiler tube, leave the space between the two, the space intercommunication has a first gas inlet, first gas inlet is used for letting in inert gas, intermediate layer furnace chamber internal pressure is greater than all the time the pressure in the reaction chamber.
2. The apparatus for producing a high laser absorptivity metal powder according to claim 1, wherein: the inside of advancing the powder cavity is equipped with sorting unit, sorting unit locates advance the below of powder funnel, will follow advance the metal powder that the powder funnel carried carries and carry out the particle diameter screening, carry again to send powder valve department, sorting unit top-down includes one-level powder sorting screen cloth, powder guide plate and second grade powder sorting screen cloth in proper order, the mesh size of one-level powder sorting screen cloth is greater than the mesh size of second grade powder sorting screen cloth, the powder guide plate is located the end of one-level powder sorting screen cloth, will follow the metal powder that one-level powder sorting screen cloth falls is guided to on the second grade powder sorting screen cloth, send the powder valve to include one-level powder and send powder valve, second grade powder and send powder valve and tertiary powder to send powder vibrator, the tail end of one-level powder sorting screen cloth is connected one-level powder vibrator, is led to one-level powder valve, the tail end of second grade powder sorting screen cloth is connected second grade powder valve, second grade powder valve is led to powder valve, second grade powder valve is sent to the powder valve, third grade powder valve is sent to the powder valve.
3. The apparatus for producing a high laser absorptivity metal powder according to claim 2, wherein: the top of the reaction chamber is provided with a rotary dispersion disc, and the height of the rotary dispersion disc is lower than that of the three-level powder feeding valve.
4. The apparatus for producing a high laser absorptivity metal powder according to claim 1, wherein: the porosity of the breathable inner furnace tube is 5% -50%, and the pore size is 100 nanometers to 50 microns.
5. The apparatus for producing a high laser absorptivity metal powder according to claim 1, wherein: the heating rod is arranged in the interlayer furnace chamber.
6. A method for producing a metal powder with high laser absorptivity by using the production apparatus according to any one of claims 1, 4, and 5, characterized by comprising the steps of:
s1, vacuumizing a device, opening the first gas inlet and the gas outlet, introducing inert gas into the interlayer furnace chamber from the first gas inlet, uniformly diffusing the inert gas into the reaction chamber through the ventilation inner furnace tube, maintaining positive pressure in the interlayer furnace chamber, and heating the reaction chamber to a standard atmospheric pressure by a heating rod to a first temperature which is 0-2800 ℃, wherein a heating zone is formed in the reaction chamber;
s2, adding raw material powder from a powder inlet funnel, screening the raw material powder into a plurality of different particle size intervals by a sorting device, opening a second gas inlet to introduce carbon source gas, determining and opening a powder feeding valve of a corresponding level according to the particle size interval of the raw material powder, so that the powder falls on a rotary dispersion disc below a three-level powder feeding valve, and uniformly dispersing by the rotary dispersion disc;
s3, after raw material powder enters the reaction chamber from the rotary dispersion disc, the raw material powder falls into the heating zone to form molten metal particles, carbon-containing source gas enters the heating zone from bottom to top to contact with the molten metal particles, a graphene film is generated on the surface while the particles are remelted and spheroidized, the molten metal particles with the surface of which the graphene film is generated continuously fall into the powder rapid cooling chamber, and finally the molten metal particles enter the collection tank to be collected, wherein the carbon-containing source gas is hydrocarbon;
and S4, after the reaction is completed, stopping powder feeding by the powder feeding device, closing the second gas inlet, continuously introducing inert gas from the first gas inlet, and sealing and sub-packaging the graphene metal powder in the collecting tank after the reaction chamber is cooled to room temperature.
7. The method for preparing the metal powder with high laser absorptivity according to claim 6, wherein: in S2, the method also comprises grading, wherein the grading is used in occasions needing a certain particle size distribution ratio, and the sorted raw material powder is mixed according to a preset ratio by opening different powder feeding valves.
8. The method for preparing the metal powder with high laser absorptivity according to claim 6, wherein: the pressure of the sandwich furnace chamber after the inert gas is introduced is 0.1-5 MPa.
9. The method for preparing the metal powder with high laser absorptivity according to claim 6, wherein: the raw material powder is recycled 3D printing old powder.
10. The method for preparing the metal powder with high laser absorptivity according to claim 6, wherein: the gas introduced into the first gas inlet is mixed gas comprising inert gas and hydrogen.
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| CN116037944A (en) * | 2022-12-08 | 2023-05-02 | 江西咏泰粉末冶金有限公司 | Method for preparing micron-scale/nano-scale graded spherical copper powder by using plasma |
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Effective date of registration: 20240331 Address after: Building 1, 1st Floor, No. 218 Qingdao East Road, Taicang City, Suzhou City, Jiangsu Province, 215400 Patentee after: Hydrogen Field (Taicang) New Materials Technology Co.,Ltd. Country or region after: China Address before: 200444 room 243, building 2, No. 1919, Fengxiang Road, Baoshan District, Shanghai Patentee before: Shanghai Hetian New Material Technology Co.,Ltd. Country or region before: China |