An apparatus for coating a metal coating on the surface of powder by the carbonyl method and its use method

By designing a device including a closed bin and a gas circulation system, the problems of powder heating and raw material recycling during the carbonyl coating powder are solved, and high purity and low-cost mass production of the plating are achieved.

CN116121736BActive Publication Date: 2025-07-25佛山市金磁科技有限公司
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Patent Information

Application Number
CN202310198445.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-03
Publication Date
2025-07-25
Estimated Expiration
2043-03-03

AI Technical Summary

Technical Problem

During the existing carbonyl method, the problems of effective heating of powder and recycling of raw materials have not been effectively solved, resulting in low purity of the plating layer and high cost.

Method used

A device including a closed bin, a carbonyl metal gas inlet, a carrier gas tank, a carbonyl metal gas tank, a recycling device and a cooling liquid tank was designed. By controlling the gas ratio and heating method, effective heating of powder and raw material recycling can be achieved, ensuring the purity of the plating layer and reducing costs.

Benefits of technology

The high purity and high raw material utilization rate of the powder surface plating are achieved, which significantly reduces the cost of the plating treatment process and has batch processing capabilities.

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Abstract

The present invention discloses a device for coating a metal coating on the surface of powder by the carbonyl process, belonging to the technical field of devices for preparing coating layers by vapor deposition. The device for coating a metal coating on the surface of powder by the carbonyl process of the present invention includes a closed chamber, a carbonyl metal gas inlet chamber located at its center, a carrier gas tank, a carbonyl metal gas tank, a carrier gas and carbonyl metal gas recovery device respectively connected to the two tanks, and a cooling liquid tank. The device and method of the present invention solve the problems of effective heating of powder and recycling of raw materials in the process of coating nickel and iron coatings on the surface of powder by the carbonyl process. It not only ensures the high purity of the coating, but also has energy-saving process, high raw material utilization rate, significantly reduces the cost of the coating treatment process, and has batch processing capacity.
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Description

Technical Field

[0001] The present invention belongs to the technical field of devices for preparing coating layers by vapor deposition, and particularly relates to a device for coating a metal coating on the surface of powder by a carbonyl method and a using method thereof. Background Art

[0002] The principle of powder coating modification is to uniformly introduce one or more other component substances on the surface of powder particles, and form an adsorption layer or a monolayer film with a certain thickness through chemical reaction or physical adsorption, so as to change the surface characteristics of the powder or endow the powder with new properties.

[0003] Coating powder by the carbonyl method utilizes the principle of chemical migration reaction. Volatile metal carbonyl gases are formed by the reaction of metals with carbon monoxide, and then the gases are transferred and the temperature is controlled to decompose the gases into metals and carbon monoxide on the surface of the powder. The advantages of the carbonyl method for coating powder are: low energy consumption, less material consumption, high purity and variety of coating layers, high degree of automation, and actually no waste is generated and no pollution to the environment. However, some metal carbonyl gases are highly toxic, and only by achieving complete recycling (no emission) can the advantages of pollution-free and further cost reduction be realized. Moreover, if the decomposition of metal carbonyl gases cannot be controlled to occur at a lower temperature, a carbon pollution problem will occur. CO is one of the decomposition products of metal carbonyls. Existing research results show that when the temperature is higher than 704 °C, a disproportionation reaction will occur to generate CO2 and C, that is, a carbon pollution problem is caused. Generally speaking, in order to reduce and eliminate the carbon pollution degree of products, it is necessary to avoid the generation of local high-temperature regions in the decomposition chamber.

[0004] The most common metal carbonyls at present are nickel and iron. Both of them have good affinity with many metals and non-metals, and are the main alloy elements widely used. Moreover, metallic nickel also has high antioxidant and corrosion resistance capabilities. It is known that under normal pressure and conditions of 40 - 200 °C (40 - 100 °C for nickel; 150 - 200 °C for iron), carbon monoxide can react with metallic nickel and iron to generate colorless liquids of nickel carbonyl and iron carbonyl. The liquid is vaporized when heated to 50 - 105 °C (the vaporization temperature of nickel carbonyl is 42.5 °C; iron carbonyl is 103.6 °C), and further heated to 150 - 300 °C, it can be decomposed into metallic nickel or iron and carbon monoxide again. The reactions are as follows:

[0005] Ni +4CO=Ni (CO)4(liquid); Ni (CO)4=Ni (solid)+4CO↑

[0006] Fe +5CO=Fe (CO)5(liquid); Fe (CO)5=Fe (solid)+5CO↑

[0007] In order to give full play to the advantages of high purity of nickel and iron on the surface layer of nickel and iron coated powders produced by the carbonyl method, such as energy conservation, material conservation, high quality, high raw material utilization rate, strong process controllability, and being conducive to mass production, the equipment adopted first needs to solve two main problems: effective heating of powders and recycling of raw materials. Summary of the Invention

[0008] The present invention provides a device for coating a metal coating on the surface of powders by the carbonyl method, which includes a sealed chamber and a carbonyl metal gas inlet chamber located at its center, a carrier gas tank, a carbonyl metal gas tank, and carrier gas and carbonyl metal gas recovery devices respectively connected to the two tanks, and a cooling liquid tank. The device of the present invention solves the problems of effective heating of powders and recycling of raw materials in the process of coating nickel and iron coatings on the surface of powders by the carbonyl method. It not only ensures the high purity of the coatings, but also is energy-saving in the process, has a high raw material utilization rate, and significantly reduces the cost of the coating treatment process.

[0009] The technical solution adopted by the present invention is as follows:

[0010] A device for coating a metal coating on the surface of powders by the carbonyl method, which includes a sealed chamber and a carbonyl metal gas inlet chamber located at its center, a carrier gas tank, a carbonyl metal gas tank, and carrier gas and carbonyl metal gas recovery devices respectively connected to the two tanks, and a cooling liquid tank.

[0011] Further, the sealed chamber is composed of a heating chamber and a metal gas inlet chamber. The metal gas inlet chamber is connected to the carbonyl metal gas inlet chamber through pores on the wall surface of the carbonyl metal gas inlet chamber.

[0012] The central axes of the heating chamber, the metal gas inlet chamber, and the carbonyl metal gas inlet chamber coincide with the central axis of the sealed chamber.

[0013] An outlet for unreacted gas is provided at the top of the metal gas inlet chamber and is connected to the carrier gas and carbonyl metal gas recovery device through a control valve.

[0014] The carrier gas in the carrier gas tank is introduced into the heating chamber through a control valve.

[0015] The carbonyl metal gas in the carbonyl metal gas tank is connected to a pipeline branch of the carrier gas tank through a control valve, and the mixed gas adjusted to a suitable ratio is introduced into the carbonyl metal gas inlet chamber.

[0016] Further, the heating chamber is located below the metal gas inlet chamber and is separated by inclined channels respectively fixed on the inner wall of the sealed chamber and the outer wall of the carbonyl metal gas inlet chamber. The volume ratio of the two is 1:1 - 1:2 (that is, the heating part accounts for 1 / 3 - 1 / 2 of the entire sealed chamber part); the angle between the inclined channels and the direction perpendicular to the walls of the sealed chamber and the carbonyl metal gas inlet chamber is 5° - 35°.

[0017] Among them, the inclined channel is fixed at a lower position at the end of the wall of the sealed chamber and opens towards the opening of the chamber for introducing metal gas. The fixed point of the inclined channel and the wall of the chamber for introducing metal carbonyl gas is slightly higher and opens towards the heating chamber (to avoid powder backflow and enable effective circulating flow in the processing chamber).

[0018] Furthermore, a coolant loop pipe is uniformly arranged on the inner wall of the chamber for introducing metal carbonyl gas. Both ends of the coolant loop pipe are connected to a coolant tank through valves; on the wall of the part of the chamber for introducing metal carbonyl gas inside, fine holes with pore diameters smaller than the pore diameters of the powder to be processed are uniformly distributed, and the fine holes are distributed at 1 / 25 - 2 / 3 of the height of the part of the chamber for introducing metal carbonyl gas inside the chamber for introducing metal gas.

[0019] Furthermore, an outlet for unreacted gas is arranged near the wall at the top of the chamber for introducing metal gas and is connected to a carrier gas and metal carbonyl gas recovery device through a control valve; the four walls of the front pipeline of the carrier gas and metal carbonyl gas recovery device are wrapped with a heat conduction coil pipe, and the temperature is controlled at 0 - 100 °C by the heat conduction liquid or gas flowing inside. The pipeline is inclined downward to collect the obtained liquefied metal carbonyl liquid and introduce it into the corresponding metal carbonyl liquid storage device (after treatment, introduce it into the metal carbonyl gas tank); a carrier gas outlet is arranged near the tail end and is connected to a processing device through a control valve for recovering the carrier gas and subsequent treatment and introducing it into the carrier gas tank.

[0020] Furthermore, 2 - 4 rows of a total of n heating wires are uniformly distributed in the heating chamber, where n is an even number from 8 - 24;

[0021] On the side wall of the chamber for introducing metal gas, 2 - 8 even - numbered powder inlets are arranged at 1 / 5 - 1 / 4 near the top, and the opening and closing are adjusted through a sealing flange and a control valve. 2 - 8 even - numbered powder outlets are arranged at 1 / 5 - 1 / 10 near the bottom on the side wall, and the opening and closing are adjusted through a sealing flange and a control valve;

[0022] The carrier gas from the carrier gas tank passes through a primary heating device through a control valve and then enters the heating chamber;

[0023] The metal carbonyl gas from the metal carbonyl gas tank is connected to a pipeline branch of the carrier gas tank controlled by a valve through a control valve, and a mixed gas of the two gases adjusted to a suitable ratio is introduced into the chamber for introducing metal carbonyl gas.

[0024] Furthermore, the sealed chamber is a geometric body with an axisymmetric shape including a cylinder, a cuboid, a cube, etc.; the chamber for introducing metal carbonyl gas located at its center is a cylinder.

[0025] The metal carbonyl gas is nickel carbonyl and iron carbonyl gas.

[0026] The usage method of the device for coating a metal coating on the surface of powder by the carbonyl method includes the following steps:

[0027] (1) Loading: Close the powder outlet, open the powder inlet, transport the powder to be processed to the metal gas inlet chamber, and then close the powder inlet;

[0028] (2) Starting the heating device: Turn on the primary heating device; Turn on the power supply of the heating wire and gradually increase the heating current to the set value;

[0029] (3) Introducing the carrier gas for heating: Pre-adjust the temperature of the gas output from the carrier gas tank to the predetermined decomposition temperature of the carbonyl metal gas, and open the carrier gas control valve to allow the carrier gas to enter the heating chamber;

[0030] (4) Introducing the carbonyl metal gas for decomposition: Open the valves at both ends of the coolant loop connected to the coolant tank and control the appropriate flow rate; Control the carrier gas branch valve and the valve connected to the carbonyl metal gas tank, and mix the carbonyl metal gas and the carrier gas in an appropriate ratio and then introduce them into the carbonyl metal gas inlet chamber;

[0031] (5) Starting the recovery device: Open the outlet for unreacted gas, control the valve and start the recovery device for the carrier gas and the carbonyl metal gas; Adjust the heat-conducting coil to an appropriate temperature to quickly separate the liquefied carbonyl metal liquid from the carrier gas;

[0032] (6) Sequentially close the recovery device for the carrier gas and the carbonyl metal gas, the outlet for unreacted gas, the carrier gas branch valve and the valve connected to the carbonyl metal gas tank, the valves at both ends of the coolant loop connected to the coolant tank, the carrier gas control valve and the primary heating device in reverse order, and open the powder outlet and take out the processed powder.

[0033] After adopting the above scheme, the beneficial effects of the present invention are as follows:

[0034] The device and method of the present invention solve the problems of effective heating of powder and recycling of raw materials in the process of coating nickel and iron coatings on the surface of powder by the carbonyl method. It not only ensures the high purity of the coating, but also has energy-saving in the process, high raw material utilization rate, significantly reduces the cost of the coating treatment process, and has the ability of batch processing. Description of the Drawings

[0035] Figure 1 It is a device for coating a metal coating on the surface of powder by the carbonyl method of the present invention.

[0036] Specific reference numerals:

[0037] 0. Preheater; 1. Inlet for the carrier gas for heating the heating chamber; 2. Inlet for the gas in the carbonyl metal gas inlet chamber; 3. Heating wire; 4. Inclined channel separating the heating chamber and the metal gas inlet chamber (see the attached Figure 1Top left figure); 5. Powder outlet; 6. Powder inlet; 7. Carbonyl metal gas is introduced into the fine pores of the chamber wall; 8. Outlet for unreacted gas; 9. Heat-conducting coil. Detailed implementation mode

[0038] The present invention will be further described below in conjunction with embodiments and the drawings.

[0039] A device for coating nickel and iron coatings on the surface of powder by the carbonyl method, comprising a sealed chamber (with a heating chamber, a metal gas introduction chamber, and an anti-backflow circulation channel connecting the bottom of the metal gas introduction chamber to the top of the heating chamber) and a carbonyl metal gas introduction chamber located at its center, a carrier gas tank, a carbonyl metal gas tank, and a carrier gas and carbonyl metal gas recovery device and a cooling liquid tank respectively connected to the two tanks; the central axes of the heating chamber, the metal gas introduction chamber, and the carbonyl metal gas introduction chamber coincide with the central axis of the sealed chamber; an outlet for unreacted gas is provided at the top of the metal gas introduction chamber and is connected to the carrier gas and carbonyl metal gas recovery device; the front pipeline walls of the carrier gas and carbonyl metal gas recovery device are surrounded by a heat-conducting coil (flowing with a heat-conducting liquid or gas) with controllable temperature; powder inlets (high-end) and outlets (low-end) are arranged at both ends of the metal gas introduction chamber; the carrier gas from the carrier gas tank passes through a primary heating device and is introduced into the heating chamber through a control valve; the carbonyl metal gas from the carbonyl metal gas tank is connected to the carrier gas tank branch line through a control valve, and a mixed gas with a suitable ratio is regulated and introduced into the carbonyl metal gas introduction chamber.

[0040] Specifically:

[0041] A device for coating a metal coating on the surface of powder by the carbonyl method according to the present invention comprises a sealed chamber and a carbonyl metal gas introduction chamber located at its center, a carrier gas tank, a carbonyl metal gas tank, and a carrier gas and carbonyl metal gas recovery device and a cooling liquid tank respectively connected to the two tanks.

[0042] Specifically:

[0043] The sealed chamber is composed of a heating chamber and a metal gas introduction chamber, and the metal gas introduction chamber is connected to the carbonyl metal gas introduction chamber through pores on the wall surface of the carbonyl metal gas introduction chamber.

[0044] Moreover, the sealed chamber is a geometric body with an axisymmetric shape including a cylinder, a cuboid, a cube, etc.; the carbonyl metal gas introduction chamber located at its center is a cylinder.

[0045] The heating chamber is located below the metal gas inlet chamber and is separated by inclined channels respectively fixed to the inner wall of the sealed chamber and the outer wall of the metal carbonyl gas inlet chamber. The volume ratio of the two is 1:1 - 1:2 (i.e., the heating part accounts for 1 / 3 - 1 / 2 of the entire sealed chamber part); the angle between the inclined channel and the direction perpendicular to the walls of the sealed chamber and the metal carbonyl gas inlet chamber is 5° - 35°.

[0046] Among them, the inclined channel is fixed at a lower position at the end of the wall of the sealed chamber and opens to the metal gas inlet chamber. The fixed point of the inclined channel and the wall of the metal carbonyl gas inlet chamber is slightly higher and opens to the heating chamber (to avoid powder backflow and effectively circulate in the processing chamber).

[0047] The inner wall of the metal carbonyl gas inlet chamber is evenly arranged with coolant annular pipes. The two ends of the coolant annular pipes are connected to the coolant tank through valves; on the wall of the part of the metal carbonyl gas inlet chamber, fine holes with apertures smaller than the apertures of the powder to be processed are evenly distributed. The fine holes are distributed at 1 / 25 - 2 / 3 of the height of the part of the metal carbonyl gas inlet chamber inside the metal gas inlet chamber.

[0048] The central axes of the heating chamber, the metal gas inlet chamber, and the metal carbonyl gas inlet chamber coincide with the central axis of the sealed chamber; 2 - 4 rows of a total of n heating wires are evenly distributed in the heating chamber, and n is an even number from 8 to 24.

[0049] An outlet for unreacted gas is provided at the top of the metal gas inlet chamber and is connected to the carrier gas and metal carbonyl gas recovery device through a control valve; 2 - 8 even - numbered powder inlets are arranged at 1 / 5 - 1 / 4 of the side wall near the top of the metal gas inlet chamber, and 2 - 8 even - numbered powder outlets are arranged at 1 / 5 - 1 / 10 of the side wall near the bottom, and the opening and closing are adjusted through sealed flanges and control valves.

[0050] An outlet for unreacted gas is provided near the wall at the top of the metal gas inlet chamber and is connected to the carrier gas and metal carbonyl gas recovery device through a control valve; the front - end pipeline of the carrier gas and metal carbonyl gas recovery device is surrounded by heat - conducting coiled pipes on four walls, and the temperature is controlled at 0 - 100 °C by the heat - conducting liquid or gas flowing inside. The pipeline slopes downward to collect the obtained liquefied metal carbonyl liquid and introduce it into the corresponding metal carbonyl liquid storage device (after treatment, introduce it into the metal carbonyl gas tank); a carrier gas outlet is provided near the tail end and is connected to the treatment device through a control valve for recovering the carrier gas and subsequent treatment and introducing it into the carrier gas tank.

[0051] The carrier gas in the carrier gas tank is introduced into the heating chamber through a control valve; the metal carbonyl gas in the metal carbonyl gas tank is connected to the pipeline branch of the carrier gas tank through a control valve, and the mixed gas adjusted to an appropriate ratio is introduced into the metal carbonyl gas inlet chamber.

[0052] More specifically, the carrier gas in the carrier gas tank passes through a primary heating device via a control valve and then enters the heating chamber; the metal carbonyl gas in the metal carbonyl gas tank is connected to a pipeline branch of the carrier gas tank controlled by a valve through a control valve, and the two gases are regulated to a mixed gas with a suitable ratio and then introduced into the metal carbonyl gas inlet chamber.

[0053] The usage method of the device for coating a metal coating on the surface of powder by the above-mentioned carbonyl method includes the following steps:

[0054] (1) Loading: Close the powder outlet, open the powder inlet, transport the powder to be processed to the metal gas inlet chamber, and then close the powder inlet;

[0055] (2) Starting the heating device: Turn on the primary heating device; Turn on the power supply for controlling the heating wire and gradually increase the heating current to the set value;

[0056] (3) Introducing the carrier gas for heating: Adjust the temperature of the gas output from the carrier gas tank to the predetermined decomposition temperature of the metal carbonyl gas in advance, and open the carrier gas control valve to allow the carrier gas to enter the heating chamber;

[0057] (4) Introducing the metal carbonyl gas for decomposition: Open the valves connecting the two ends of the coolant loop pipe to the coolant tank and control the appropriate flow rate; Control the carrier gas branch valve and the valve connected to the metal carbonyl gas tank, and mix the metal carbonyl gas and the carrier gas in a suitable ratio and then introduce them into the metal carbonyl gas inlet chamber;

[0058] (5) Starting the recovery device: Open the outlet for unreacted gas, control the valve and start the recovery device for the carrier gas and the metal carbonyl gas; Adjust the heat-conducting coil to a suitable temperature to quickly separate the liquefied metal carbonyl liquid from the carrier gas;

[0059] (6) Sequentially close the recovery device for the carrier gas and the metal carbonyl gas, the outlet for unreacted gas, the carrier gas branch valve and the valve connected to the metal carbonyl gas tank, the valves connecting the two ends of the coolant loop pipe to the coolant tank, the carrier gas control valve and the primary heating device in reverse order, and open the powder outlet and take out the processed powder.

[0060] The above is the preferred embodiment of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements are also regarded as the protection scope of the present invention.

Claims

1. An apparatus for coating a metal coating on the surface of a powder by the carbonyl method, characterized in that: It includes an airtight chamber, a metal carbonyl gas inlet chamber located at its center, a carrier gas tank, a metal carbonyl gas tank, a carrier gas and metal carbonyl gas recovery device respectively connected to the two tanks, and a cooling liquid tank; The airtight chamber consists of a heating chamber and a metal gas inlet chamber. The metal gas inlet chamber is connected to the metal carbonyl gas inlet chamber through pores on the wall surface of the metal carbonyl gas inlet chamber; An unreacted gas outlet is provided at the top of the metal gas inlet chamber and is connected to the carrier gas and metal carbonyl gas recovery device through a control valve; The carrier gas in the carrier gas tank is introduced into the heating chamber through a control valve; The metal carbonyl gas in the metal carbonyl gas tank is connected to a pipeline branch of the carrier gas tank through a control valve, and the mixed gas adjusted to an appropriate ratio is introduced into the metal carbonyl gas inlet chamber; The heating chamber is located below the metal gas inlet chamber and is separated by an inclined channel respectively fixed on the inner wall of the airtight chamber and the outer wall of the metal carbonyl gas inlet chamber. The volume ratio of the two is 1:1 - 1:2; the included angle between the inclined channel and the direction perpendicular to the inner walls of the airtight chamber and the metal carbonyl gas inlet chamber is 5° - 35°; Among them, the lower end of the inclined channel is fixed on the inner wall of the airtight chamber and opens towards the metal gas inlet chamber. The fixed point of the inclined channel and the inner wall of the metal carbonyl gas inlet chamber is slightly higher and opens towards the heating chamber, avoiding powder backflow and enabling effective circulation in the metal gas inlet chamber; Cooling liquid loop pipes are evenly arranged on the inner wall of the metal carbonyl gas inlet chamber. Both ends of the cooling liquid loop pipes are connected to the cooling liquid tank through valves; on the inner wall of the part of the metal carbonyl gas inlet chamber, fine holes with pore diameters smaller than the pore diameters of the powder to be processed are evenly distributed. The fine holes are distributed at 1 / 25 - 2 / 3 of the height of the part of the metal carbonyl gas inlet chamber in the metal gas inlet chamber; An unreacted gas outlet is provided near the wall at the top of the metal gas inlet chamber and is connected to the carrier gas and metal carbonyl gas recovery device through a control valve; the front pipeline walls of the carrier gas and metal carbonyl gas recovery device are surrounded by heat-conducting coil pipes, and the temperature is controlled at 0 - 100 °C by the heat-conducting liquid or gas flowing inside. The pipeline slopes downward to collect the obtained liquefied metal carbonyl liquid and introduce it into the corresponding metal carbonyl liquid storage device, and after treatment, it is introduced into the metal carbonyl gas tank; a carrier gas outlet is provided near the end of the pipeline and is connected to a treatment device through a control valve for recovering the carrier gas and subsequent treatment and introducing it into the carrier gas tank.

2. The device for coating a metal coating on the surface of powder by the carbonyl method according to claim 1, characterized in that: The central axes of the heating chamber, the metal gas inlet chamber, and the metal carbonyl gas inlet chamber coincide with the central axis of the airtight chamber.

3. The apparatus for coating a metal coating on the surface of a powder by the carbonyl method according to claim 1, characterized in that: 2 - 4 rows of a total of n heating wires are evenly distributed in the heating chamber, and n is an even number from 8 - 24; 2 - 8 even-numbered powder inlets are arranged at 1 / 5 - 1 / 4 of the side wall near the top of the metal gas inlet chamber, and the opening and closing are adjusted through a sealing flange and a control valve. 2 - 8 even-numbered powder outlets are arranged at 1 / 5 - 1 / 10 of the side wall near the bottom, and the opening and closing are adjusted through a sealing flange and a control valve; The carrier gas in the carrier gas tank is introduced into the heating chamber through a control valve after passing through a primary heating device; The metal carbonyl gas in the metal carbonyl gas tank is connected to the carrier gas tank pipeline branch controlled by the control valve through the control valve. The mixed gas of the two gases regulated to an appropriate ratio is heated and then introduced into the metal carbonyl gas inlet chamber.

4. The apparatus for coating a metal coating on the surface of a powder by the carbonyl method according to claim 3, characterized in that: The closed chamber is a geometric body with an axisymmetric shape including a cylinder, a cuboid, and a cube; the metal carbonyl gas inlet chamber located at its center is a cylinder.

5. The method of using the device for coating a metal coating on the surface of powder by the carbonyl method according to claim 3, characterized in that: It includes the following steps: (1) Loading: Close the powder outlet, open the powder inlet, transport the powder to be processed to the metal gas inlet chamber, and then close the powder inlet; (2) Starting the heating device: Open the primary heating device; turn on the power supply of the heating wire and gradually increase the heating current to the set value; (3) Introducing the carrier gas for heating: Pre-adjust the temperature of the gas output from the carrier gas tank to the predetermined metal carbonyl gas decomposition temperature, and open the carrier gas control valve to allow the carrier gas to enter the heating chamber; (4) Introducing the metal carbonyl gas for decomposition: Open the valves connecting the two ends of the coolant loop pipe to the coolant tank and control the appropriate flow rate; control the carrier gas branch valve and the valve connected to the metal carbonyl gas tank, and mix the metal carbonyl gas and the carrier gas in an appropriate ratio and then introduce them into the metal carbonyl gas inlet chamber; (5) Starting the recovery device: Open the outlet for unreacted gas, control the valve and start the recovery device for the carrier gas and the metal carbonyl gas; adjust the heat conduction coil to an appropriate temperature to quickly separate the liquefied metal carbonyl liquid from the carrier gas; (6) Sequentially close the recovery device for the carrier gas and the metal carbonyl gas, the outlet for unreacted gas, the carrier gas branch valve and the valve connected to the metal carbonyl gas tank, the valves connecting the two ends of the coolant loop pipe to the coolant tank, the carrier gas control valve and the primary heating device in reverse order, and open the powder outlet and take out the processed powder.

Citation Information

Patent Citations

  • System and method for preparing metal carbonyl-clad micro-nano nuclear shell powder

    CN110172670A