Method for preparing powder by adopting amorphous powder-carbonyl powder composite granulation

Through the amorphous powder-carbonyl powder composite granulation method, multiple processes are used to process in stages, which solves the problem of easy cracking on the outer surface of the carbonyl powder granulation, and achieves high-efficiency and high-quality granulation effect.

CN119425515APending Publication Date: 2025-02-14YANGZHOU JINGTE ELECTRONIC TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411409263.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-10
Publication Date
2025-02-14
Patent Text Reader

Abstract

A method for preparing powder by adopting amorphous powder-carbonyl powder composite granulation comprises the steps that raw materials are prepared, amorphous powder and carbonyl powder serve as granulation raw materials to be prepared in advance, when the raw materials are prepared, the amorphous powder and the carbonyl powder are sieved through a sieving device, and when sieving is conducted, the amorphous powder and the carbonyl powder are sieved; the magnetic attraction stone can be used for adsorbing particles in the amorphous powder and the carbonyl powder, particularly, the magnetic attraction stone can be used for adsorbing scrap iron on the amorphous powder and the carbonyl powder when the amorphous powder and the carbonyl powder encounter scrap iron, then the amorphous powder and the carbonyl powder are subjected to secondary screening, and follow-up treatment of raw materials can be conducted after secondary screening.
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Description

Technical Field

[0001] The invention relates to a powder granulation method, in particular to a powder making method using amorphous powder-carbonyl powder composite granulation. Background Art

[0002] As electronic products develop towards smaller, thinner and lighter, inductors as basic circuits will also develop in the direction of smaller and thinner. With the advent of 5G and the Internet of Things, the processing power of chips is getting stronger and stronger, and at the same time, chips require more powerful resources, which requires large current, high frequency and low loss of chip peripheral products. The smaller space also puts higher requirements on the anti-interference of components. While not interfering with the surroundings, they must also resist external interference. When inductors are needed, carbonyl powder is needed when preparing the inductors. Carbonyl powder can cover the outer surface of the inductor well, and the anti-interference ability of the inductor can be improved.

[0003] In the prior art: CN201811653368.2 A method for preparing a carbonyl powder. The present invention discloses a method for preparing a carbonyl iron powder, comprising the following steps: adding anhydrous ethanol, phosphoric acid, and a coupling agent to a ball mill to form a mixed solution; adjusting the pH value of the mixed solution to 8-9, and adding the carbonyl iron powder to the ball mill for the first ball milling; after the first ball milling, adding tetraethyl orthosilicate and a coupling agent to the ball mill, adjusting the pH value of the solution to 8-9, and performing a second ball milling; after the second ball milling, taking out the slurry, washing and drying it to obtain a flaky carbonyl iron powder having a phosphate and siloxane coating structure. The flaky carbonyl iron powder in the present invention not only has excellent absorption efficiency and good impedance matching performance in the low-frequency band, but also has the characteristics of low density, high temperature resistance, and corrosion resistance.

[0004] Although it can meet the complex environment of high temperature, high humidity, high salt fog marine climate environment and multiple vibrations induced by equipment, the granulation process of carbonyl powder is not very convenient during preparation, and cracks are prone to appear on the outer surface of the granulation. Summary of the invention

[0005] In order to overcome the deficiencies of the prior art, the present invention provides.

[0006] The present invention is implemented by the following technical solutions:

[0007] A method for preparing powder by composite granulation of amorphous powder and carbonyl powder, comprising the following steps:

[0008] Preparation of raw materials: prepare amorphous powder and carbonyl powder as raw materials for granulation in advance. When preparing the raw materials, use a screening device to screen the amorphous powder and carbonyl powder. When screening, use a magnetic stone to adsorb the particles inside the amorphous powder and carbonyl powder. In particular, when encountering iron filings, the magnetic stone can be used to adsorb the iron filings for the amorphous powder and carbonyl powder. Then, the amorphous powder and carbonyl powder are screened for a second time. After the second screening, the raw materials can be subsequently processed;

[0009] The first treatment of the raw materials is to perform the first treatment on the amorphous powder and the carbonyl powder processed by the screening device. During the first treatment, the amorphous powder and the carbonyl powder are mixed with each other. When mixing is required, ceramic powder can be added to the amorphous powder and the carbonyl powder. The ceramic powder can be aluminum oxide, silicon carbide and chromium dioxide. After the ceramic powder is added to the amorphous powder and the carbonyl powder, metal oxides are added. The metal oxides can be titanium dioxide and magnesium oxide. Finally, they are mixed with each other to form a granulated blank. Silicates with bonding effect are added to the granulated blank, and then the blank is sent to a heating device for heating treatment. The heating device can be a heating kiln or a heating tank.

[0010] A granulation blank is formed by mixing amorphous powder and carbonyl powder, and the granulation blank is heated to form a problem of 100-120 degrees Celsius during the heating treatment. Then, the heated granulation blank is placed in a spraying device, and a cooling component is arranged beside the spraying device. The cooling component is a metal cooling roller, and a cooling pipeline is arranged inside the metal cooling roller, so that the outer surface temperature of the metal cooling roller can be maintained at minus 10-15 degrees Celsius. Then, the spraying device is used to spray the granulation blank onto the metal cooling roller by using a nozzle, so that a temperature difference can be formed by using the high-temperature granulation blank and the low-temperature metal cooling roller, so that the granulation blank can be quickly cooled, and the granulation blank can be well formed into a metal powder blank;

[0011] The second treatment of the raw materials, when the granulation blank is sprayed onto the outer surface of the metal cooling roller, the metal cooling roller can be used to cool the granulation blank. During the cooling treatment, the granulation blank can be easily formed into granulated metal powder blanks. These metal powder blanks require further second treatment. During the second treatment, the granulation blank is carbonylated. The granulation blank is placed in a high-temperature device for secondary high-temperature calcination. Carbon monoxide is introduced into the high-temperature device. Carbon monoxide and the granulation blank are reacted at high temperature to form carbonyl compounds in the granulation blank. This completes the carbonyl treatment of the granulation blank.

[0012] The granulated blanks after carbonyl treatment subsequently start the first granulation treatment, the granulated blanks are compressed, and during the compression, the granulated blanks are placed in a die-casting mold for die-casting. Before die-casting, a demoulding liquid can be sprayed on the die-casting mold. The demoulding liquid is composed of a lubricating liquid, and the lubricating liquid is composed of water, glycerol, propylene glycol and sodium hyaluronate. These lubricating liquids are sprayed on the die-casting mold before die-casting, and then allowed to stand for 10 minutes after spraying. The granulated blanks are placed in the die-casting mold, and the die-casting mold is used for die-casting. After die-casting, the granulated blanks are demoulded by external force. After demoulding, the granulated blanks are placed in a recycling frame to wait for the second granulation treatment.

[0013] The granulated blanks are then subjected to secondary granulation treatment. During the secondary granulation treatment, the granulated blanks are transported to the sintering equipment for sintering treatment. During the sintering treatment, the granulated blanks are placed on the sintering car using a transfer sintering car, and the granulated blanks are pushed into the sintering equipment using the sintering car. Then, the high temperature in the sintering equipment is used for high-temperature sintering of the granulated blanks. During high-temperature sintering, the temperature needs to be increased to 200-300 degrees Celsius for high temperature sintering, and then the temperature is reduced to 120-150 degrees Celsius, and then the temperature is increased again. The increased temperature is maintained at 200-300 degrees Celsius for 50 minutes, which has a better sintering effect on the granulated blanks.

[0014] The granulated blanks after sintering need to be processed for burrs. When processing the burrs, the granulated blanks need to be placed in a drum for rolling processing. The inner wall of the drum is provided with spikes. The spikes are small spikes with a height of 1-5mm. In this way, the drum with spikes on the inner wall can process the burrs on the outer surface of the granulated blanks. When processing the burrs, it is necessary to spray water on the outside of the drum. When spraying water, the nozzle can be manually lifted to spray water on the drum. The spraying time is 10 minutes, which is based on wetting the granulated blanks. It does not need to be sprayed for too long.

[0015] The granulated blank needs to be pretreated on the surface when deburring. During the surface pretreatment, the granulated blank can be subjected to surface plasma spraying. During the plasma spraying, the granulated blank is placed inside the spraying equipment, and then a plasma spraying gun is arranged inside the spraying equipment. The coating material is sprayed by the plasma spraying gun. The coating material is a mixed material composed of aluminum oxide, silicon nitride and titanium oxide. The coating material is sprayed onto the outer surface of the granulated blank by a spray gun to strengthen the surface of the granulated blank.

[0016] The surface-strengthened granulated blanks are subjected to terminal treatment. During the terminal treatment, the sprayed granulated blanks are placed on a drying device for drying. The drying device adopts a drying box. The granulated blanks are placed on the drying box for drying. Inert gas is injected during drying. The inert gas can be nitrogen. The granulated blanks are continuously dried in the drying box.

[0017] Compared with the prior art, the present invention adopts multiple processes to carry out staged treatment of carbonyl powder granulation when it is necessary to prepare carbonyl powder granulation. When processing in different stages, the needs of die-casting and granulation of carbonyl powder are met. During granulation, the blank can be prepared by relying on a metal cooling roller, especially when the granulated blank is sprayed on the metal cooling roller, the granulated blank can be rapidly cooled, which can effectively affect the granulated blank powder, making the preparation of the granulated blank more convenient.

[0018] When the carbonyl powder is granulated, a plasma spray gun is used to spray a coating material. The coating material is a mixed material composed of aluminum oxide, silicon nitride and titanium oxide. The coating material is sprayed onto the outer surface of the granulated blank by a spray gun to further strengthen the surface of the granulated blank. The mixed material forms a relatively strong outer surface coating on the outer surface of the granulated blank formed by the carbonyl powder die-casting, so that the outer surface strength of the carbonyl powder is further improved. DETAILED DESCRIPTION

[0019] The present invention is further described below.

[0020] A method for preparing powder by composite granulation of amorphous powder and carbonyl powder, comprising the following steps:

[0021] Preparation of raw materials: prepare amorphous powder and carbonyl powder as raw materials for granulation in advance. When preparing the raw materials, use a screening device to screen the amorphous powder and carbonyl powder. When screening, use a magnetic stone to adsorb the particles inside the amorphous powder and carbonyl powder. In particular, when encountering iron filings, the magnetic stone can be used to adsorb the iron filings for the amorphous powder and carbonyl powder. Then, the amorphous powder and carbonyl powder are screened for a second time. After the second screening, the raw materials can be subsequently processed;

[0022] The first treatment of the raw materials is to perform the first treatment on the amorphous powder and the carbonyl powder processed by the screening device. During the first treatment, the amorphous powder and the carbonyl powder are mixed with each other. When mixing is required, ceramic powder can be added to the amorphous powder and the carbonyl powder. The ceramic powder can be aluminum oxide, silicon carbide and chromium dioxide. After the ceramic powder is added to the amorphous powder and the carbonyl powder, metal oxides are added. The metal oxides can be titanium dioxide and magnesium oxide. Finally, they are mixed with each other to form a granulated blank. Silicates with bonding effect are added to the granulated blank, and then the blank is sent to a heating device for heating treatment. The heating device can be a heating kiln or a heating tank.

[0023] When the amorphous powder and the carbonyl powder are mixed to form a granulated blank and sent into the heating kiln and the heating tank, a dispersion treatment can be performed. A dispersant is added to the granulated blank formed by mixing the amorphous powder and the carbonyl powder. The dispersant can effectively prevent the amorphous powder and the carbonyl powder from forming a granulated blank from forming large lumps of particles during heating, which is inconvenient for subsequent further heating treatment.

[0024] A granulation blank is formed by mixing amorphous powder and carbonyl powder, and the granulation blank is heated to form a problem of 100-120 degrees Celsius during the heating treatment. Then, the heated granulation blank is placed in a spraying device, and a cooling component is arranged beside the spraying device. The cooling component is a metal cooling roller, and a cooling pipeline is arranged inside the metal cooling roller, so that the outer surface temperature of the metal cooling roller can be maintained at minus 10-15 degrees Celsius. Then, the spraying device is used to spray the granulation blank onto the metal cooling roller by using a nozzle, so that a temperature difference can be formed by using the high-temperature granulation blank and the low-temperature metal cooling roller, so that the granulation blank can be quickly cooled, and the granulation blank can be well formed into a metal powder blank;

[0025] The second treatment of the raw materials, when the granulation blank is sprayed onto the outer surface of the metal cooling roller, the metal cooling roller can be used to cool the granulation blank. During the cooling treatment, the granulation blank can be easily formed into granulated metal powder blanks. These metal powder blanks require further second treatment. During the second treatment, the granulation blank is carbonylated. The granulation blank is placed in a high-temperature device for secondary high-temperature calcination. Carbon monoxide is introduced into the high-temperature device. Carbon monoxide and the granulation blank are reacted at high temperature to form carbonyl compounds in the granulation blank. This completes the carbonyl treatment of the granulation blank.

[0026] The granulated blanks after carbonyl treatment subsequently start the first granulation treatment, the granulated blanks are compressed, and during the compression, the granulated blanks are placed in a die-casting mold for die-casting. Before die-casting, a demoulding liquid can be sprayed on the die-casting mold. The demoulding liquid is composed of a lubricating liquid, and the lubricating liquid is composed of water, glycerol, propylene glycol and sodium hyaluronate. These lubricating liquids are sprayed on the die-casting mold before die-casting, and then allowed to stand for 10 minutes after spraying. The granulated blanks are placed in the die-casting mold, and the die-casting mold is used for die-casting. After die-casting, the granulated blanks are demoulded by external force. After demoulding, the granulated blanks are placed in a recycling frame to wait for the second granulation treatment.

[0027] The granulated blanks are then subjected to secondary granulation treatment. During the secondary granulation treatment, the granulated blanks are transported to the sintering equipment for sintering treatment. During the sintering treatment, the granulated blanks are placed on the sintering car using a transfer sintering car, and the granulated blanks are pushed into the sintering equipment using the sintering car. Then, the high temperature in the sintering equipment is used for high-temperature sintering of the granulated blanks. During high-temperature sintering, the temperature needs to be increased to 200-300 degrees Celsius for high temperature sintering, and then the temperature is reduced to 120-150 degrees Celsius, and then the temperature is increased again. The increased temperature is maintained at 200-300 degrees Celsius for 50 minutes, which has a better sintering effect on the granulated blanks.

[0028] The granulated blanks after sintering need to be processed for burrs. When processing the burrs, the granulated blanks need to be placed in a drum for rolling processing. The inner wall of the drum is provided with spikes. The spikes are small spikes with a height of 1-5mm. In this way, the drum with spikes on the inner wall can process the burrs on the outer surface of the granulated blanks. When processing the burrs, it is necessary to spray water on the outside of the drum. When spraying water, the nozzle can be manually lifted to spray water on the drum. The spraying time is 10 minutes, which is based on wetting the granulated blanks. It does not need to be sprayed for too long.

[0029] The granulated blank needs to be pretreated on the surface when deburring. During the surface pretreatment, the granulated blank can be subjected to surface plasma spraying. During the plasma spraying, the granulated blank is placed inside the spraying equipment, and then a plasma spraying gun is arranged inside the spraying equipment. The coating material is sprayed by the plasma spraying gun. The coating material is a mixed material composed of aluminum oxide, silicon nitride and titanium oxide. The coating material is sprayed onto the outer surface of the granulated blank by a spray gun to strengthen the surface of the granulated blank.

[0030] After surface strengthening, laboratory testing is carried out. The testing standard is based on GB / T 24532-2009. The tap density of the granulated blank is 3.8-4.1 g / cm3. The strength of the outer surface of the granulated blank is further guaranteed.

[0031] The surface-strengthened granulated blanks are subjected to terminal treatment. During the terminal treatment, the sprayed granulated blanks are placed on a drying device for drying. The drying device adopts a drying box. The granulated blanks are placed on the drying box for drying. Inert gas is injected during drying. The inert gas can be nitrogen. The granulated blanks are continuously dried in the drying box.

[0032] The dried granulated blanks can be subsequently stabilized. During the stabilization treatment, it is only necessary to spray metal oxides on the outer surface of the granulated blanks. Such metal oxides can be zinc oxide or iron oxide. The stabilization layer formed by zinc oxide or iron oxide on the outer surface of the granulated blanks can better enhance the electromagnetic wave reflection and absorption capabilities of the granulated blanks, and can also further protect the carbonyl powder granulated blanks from internal oxidation treatment.

[0033] Finally, the granulated blanks that have been stabilized are formed into granular carbonyl powder granules, which can be easily processed later and then used in the inductance devices of many electronic products. In order to better protect the carbonyl powder granules from the influence of moisture, the carbonyl powder granules need to be moisture-proofed, and a drying device or drying component needs to be provided inside the equipment where the carbonyl powder granules are placed. Hygroscopic silica gel particles are placed between the carbonyl powder granules. The silica gel particles can absorb moisture very well, which can better keep the carbonyl powder granules dry.

Claims

1. A method for preparing powder by composite granulation of amorphous powder and carbonyl powder, characterized in that: The steps include: Preparation of raw materials: prepare amorphous powder and carbonyl powder as raw materials for granulation in advance. When preparing the raw materials, use a screening device to screen the amorphous powder and carbonyl powder. When screening, use a magnetic stone to adsorb the particles inside the amorphous powder and carbonyl powder. In particular, when encountering iron filings, the magnetic stone can be used to adsorb the iron filings for the amorphous powder and carbonyl powder. Then, the amorphous powder and carbonyl powder are screened for a second time. After the second screening, the raw materials can be subsequently processed; The first treatment of the raw materials is to perform the first treatment on the amorphous powder and the carbonyl powder processed by the screening device. During the first treatment, the amorphous powder and the carbonyl powder are mixed with each other. When mixing is required, ceramic powder can be added to the amorphous powder and the carbonyl powder. The ceramic powder can be aluminum oxide, silicon carbide and chromium dioxide. After the ceramic powder is added to the amorphous powder and the carbonyl powder, metal oxides are added. The metal oxides can be titanium dioxide and magnesium oxide. Finally, they are mixed with each other to form a granulated blank. Silicates with bonding effect are added to the granulated blank, and then the blank is sent to a heating device for heating treatment. The heating device can be a heating kiln or a heating tank. A granulation blank is formed by mixing amorphous powder and carbonyl powder, and the granulation blank is heated to form a problem of 100-120 degrees Celsius during the heating treatment. Then, the heated granulation blank is placed in a spraying device, and a cooling component is arranged beside the spraying device. The cooling component is a metal cooling roller, and a cooling pipeline is arranged inside the metal cooling roller, so that the outer surface temperature of the metal cooling roller can be maintained at minus 10-15 degrees Celsius. Then, the spraying device is used to spray the granulation blank onto the metal cooling roller by using a nozzle, so that a temperature difference can be formed by using the high-temperature granulation blank and the low-temperature metal cooling roller, so that the granulation blank can be quickly cooled, and the granulation blank can be well formed into a metal powder blank; The second treatment of the raw materials, when the granulation blank is sprayed onto the outer surface of the metal cooling roller, the metal cooling roller can be used to cool the granulation blank. During the cooling treatment, the granulation blank can be easily formed into granulated metal powder blanks. These metal powder blanks require further second treatment. During the second treatment, the granulation blank is carbonylated. The granulation blank is placed in a high-temperature device for secondary high-temperature calcination. Carbon monoxide is introduced into the high-temperature device. Carbon monoxide and the granulation blank are reacted at high temperature to form carbonyl compounds in the granulation blank. This completes the carbonyl treatment of the granulation blank.

2. The method for preparing powder by composite granulation of amorphous powder and carbonyl powder according to claim 1, characterized in that: The granulated blanks after carbonyl treatment subsequently start the first granulation treatment, the granulated blanks are compressed, and during the compression, the granulated blanks are placed in a die-casting mold for die-casting. Before die-casting, a demoulding liquid can be sprayed on the die-casting mold. The demoulding liquid is composed of a lubricating liquid, and the lubricating liquid is composed of water, glycerol, propylene glycol and sodium hyaluronate. These lubricating liquids are sprayed on the die-casting mold before die-casting, and then allowed to stand for 10 minutes after spraying. The granulated blanks are placed in the die-casting mold, and the die-casting mold is used for die-casting. After die-casting, the granulated blanks are demoulded by external force. After demoulding, the granulated blanks are placed in a recycling frame to wait for the second granulation treatment.

3. The method for preparing powder by composite granulation of amorphous powder and carbonyl powder according to claim 2, characterized in that: The granulated blanks are then subjected to secondary granulation treatment. During the secondary granulation treatment, the granulated blanks are transported to the sintering equipment for sintering treatment. During the sintering treatment, the granulated blanks are placed on the sintering car using a transfer sintering car, and the granulated blanks are pushed into the sintering equipment using the sintering car. Then, the high temperature in the sintering equipment is used for high-temperature sintering of the granulated blanks. During high-temperature sintering, the temperature needs to be increased to 200-300 degrees Celsius for high temperature sintering, and then the temperature is reduced to 120-150 degrees Celsius, and then the temperature is increased again. The increased temperature is maintained at 200-300 degrees Celsius for 50 minutes, which has a better sintering effect on the granulated blanks.

4. The method for preparing powder by composite granulation of amorphous powder and carbonyl powder according to claim 3, characterized in that: The granulated blanks after sintering need to be processed for burrs. When processing the burrs, the granulated blanks need to be placed in a drum for rolling processing. The inner wall of the drum is provided with spikes. The spikes are small spikes with a height of 1-5mm. In this way, the drum with spikes on the inner wall can process the burrs on the outer surface of the granulated blanks. When processing the burrs, it is necessary to spray water on the outside of the drum. When spraying water, the nozzle can be manually lifted to spray water on the drum. The spraying time is 10 minutes, which is based on wetting the granulated blanks. It does not need to be sprayed for too long.

5. The method for preparing powder by composite granulation of amorphous powder and carbonyl powder according to claim 4, characterized in that: The granulated blank needs to be pretreated on the surface when deburring. During the surface pretreatment, the granulated blank can be subjected to surface plasma spraying. During the plasma spraying, the granulated blank is placed inside the spraying equipment, and then a plasma spraying gun is arranged inside the spraying equipment. The coating material is sprayed by the plasma spraying gun. The coating material is a mixed material composed of aluminum oxide, silicon nitride and titanium oxide. The coating material is sprayed onto the outer surface of the granulated blank by a spray gun to strengthen the surface of the granulated blank.

6. The method for preparing powder by composite granulation of amorphous powder and carbonyl powder according to claim 5, characterized in that: The surface-strengthened granulated blanks are subjected to terminal treatment. During the terminal treatment, the sprayed granulated blanks are placed on a drying device for drying. The drying device adopts a drying box. The granulated blanks are placed on the drying box for drying. Inert gas is injected during drying. The inert gas can be nitrogen. The granulated blanks are continuously dried in the drying box.

Citation Information

Patent Citations

  • Preparation method of carbonyl powder

    CN111377486A