CN116213734A - Preparation method of high-ductility material coated metal powder - Google Patents

Preparation method of high-ductility material coated metal powder Download PDF

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Publication number
CN116213734A
CN116213734A CN202211699318.4A CN202211699318A CN116213734A CN 116213734 A CN116213734 A CN 116213734A CN 202211699318 A CN202211699318 A CN 202211699318A CN 116213734 A CN116213734 A CN 116213734A
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China
Prior art keywords
metal powder
powder
material coated
ductility material
coated metal
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CN202211699318.4A
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Chinese (zh)
Inventor
董世新
季相池
刘林林
郜俊震
储义青
王贵宗
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Jiangsu Zhiren Jingxing New Material Research Institute Co ltd
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Jiangsu Zhiren Jingxing New Material Research Institute Co ltd
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Priority to CN202211699318.4A priority Critical patent/CN116213734A/en
Publication of CN116213734A publication Critical patent/CN116213734A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Powder Metallurgy (AREA)

Abstract

The application relates to the technical field of metal powder modification, in particular to a preparation method of a high-ductility material coated metal powder. The preparation method comprises the following steps: comprises S1, mixing 10-50% of high molecular polymer and 50-90% of metal powder by mass percentage, wherein the average grain diameter of the high molecular polymer is 0.1-5 mu m, and the average grain diameter of the metal powder is 1-50 mu m; s2, placing the mixed powder into a closed tank body, and vacuumizing; s3, filling inert gas into the tank body, and grinding; s4, roasting the grinded composite powder in an inert gas atmosphere; s5, cooling the baked composite powder in an inert gas atmosphere, and sieving. The method can enable the high-ductility material to be fully and uniformly attached to the surface of the metal particles, forms a compact protective layer to stop foreign matters, can ensure the purity of the composite powder, and can not cause deformation of the metal powder particles due to over-high energy, thereby influencing the coating effect.

Description

Preparation method of high-ductility material coated metal powder
Technical Field
The application relates to the field of metal powder, in particular to a preparation method of high-ductility material coated metal powder
Background
Metals and metal powders are of paramount concern in our life, and metal powders, including single metal powders, alloy powders, and certain refractory compound powders having metallic properties, are the primary raw materials for powder metallurgy. Besides being used as industrial raw materials, the metal powder can also be directly applied, and the metal powder widely used at present mainly comprises iron, aluminum, copper, magnesium, manganese, tin, lead, titanium, nickel, cobalt, tungsten and the like. However, because the metal powder particles are smaller and have a larger specific surface area, many metal powders have serious oxidation phenomena during use. Oxidation not only results in performance being affected, but also adds considerable cost. Moreover, due to the limitations of the metal material, the application of the metal material is greatly limited, and the metal material is commonly made into alloy materials or composite materials with other metal or nonmetal materials.
The research progress of the preparation of polymer coated metal nano particles (functional material, period 2016 12) provides several preparation methods of the core-shell metal nano particle/polymer composite material at present, mainly emulsion polymerization method, precipitation polymerization method, in-situ polymerization method, ligand replacement method, shell crosslinking method and the like. The methods have advantages and disadvantages, but have complicated processes, and are not suitable for realizing large-scale industrial production; a preparation method of a composite material of graphene-coated metal particles (application publication number: CN 111906296A) comprises the steps of introducing a carbon source and a growth atmosphere in a high-temperature vacuum environment, adjusting the environmental pressure to perform graphene growth and recovering to obtain the composite material of the graphene-coated metal particles, wherein the defect that a protective layer on the surface of the metal particles is not uniform and complete is easily caused by incomplete graphene growth.
Disclosure of Invention
In order to solve the problems that the existing method is complex in process, uneven and complete in coating and incapable of realizing large-scale mass production, the application provides a preparation method of high-ductility material coated metal powder.
The preparation method of the high-ductility material coated metal powder adopts the following technical scheme:
a preparation method of high-ductility material coated metal powder comprises
S1, mixing 10-50% of high molecular polymer and 50-90% of metal powder in percentage by mass, wherein the average particle size of the high molecular polymer is 0.1-5 mu m, and the average particle size of the metal powder is 1-50 mu m;
s2, placing the mixed powder into a closed tank body, and vacuumizing;
s3, filling inert gas into the tank body, and grinding;
s4, roasting the grinded composite powder in an inert gas atmosphere;
s5, cooling the baked composite powder in an inert gas atmosphere, and sieving.
Preferably, the high molecular polymer comprises one or more of polyethylene, polystyrene and polytetrafluoroethylene.
Preferably, the metal powder comprises one or more of iron, aluminum, copper, magnesium, manganese, tin, lead, titanium, nickel, cobalt and tungsten.
Preferably, the grinding time of the high polymer and the metal powder in the tank body is 0.5-4h.
Preferably, the inert gas may be nitrogen or argon.
Preferably, in S4, the roasting temperature is 100-400 ℃, the heating rate is 6-10 ℃/min, and the heat preservation time is 1-4 h.
Preferably, in S2, the air pressure after the vacuuming treatment is-0.06 MPa.
Preferably, in S3, the rotating speed is regulated to 200rpm, the rotating speed is positively rotated for 15min, the rotating speed is reversely rotated for 15min, the circulation is carried out, and the mixing and grinding time is 1-3h.
In summary, the present application has the following beneficial effects: the hardness difference of the high-ductility material and the metal powder is utilized for mixed grinding, so that foreign impurities are eliminated, the purity of the composite powder can be ensured, and the deformation of metal powder particles caused by too high energy can be avoided, thereby influencing the coating effect;
by adjusting parameters such as the mixing time, the rotating speed and the like, the micro morphology of the composite powder is favorably adjusted, and the metal powder and the high-ductility material are fully compounded;
the high-ductility material can be fully and uniformly attached to the surfaces of the metal particles by high-temperature treatment, so that a compact protective layer is formed;
under the protection of inert gas, the raw materials can be fully ensured not to be oxidized in the preparation process.
Drawings
FIG. 1 is SEM photograph at 20um and 4um after the milling of example 1;
FIG. 2 is an SEM photograph at 20um and 4um after the milling of example 2;
FIG. 3 is SEM pictures at 20um and 4um after coating in example 1;
fig. 4 is SEM photographs at 20um and 4um after coating of example 2.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples.
Examples
Example 1
Two groups of polyethylene (particle size 1 μm) and aluminum powder (median diameter 10 μm) were mixed at a ratio of 30% to 70%, each group was 500g, and the mixture was thoroughly and uniformly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling nitrogen into the tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 2h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the furnace, and filling nitrogen under the air pressure of-0.06 MPa. Setting the temperature to 310 ℃, heating up at a rate of 6 ℃/min, and keeping the temperature for 2 hours. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 2
Two groups of polystyrene (particle size 0.1 μm) and copper powder (median diameter 10 μm) were mixed at a ratio of 40% to 60%, 500g each, and thoroughly and uniformly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotation speed to 200rpm, rotating for 15min positively, rotating for 15min reversely, circulating, and mixing and grinding for 1h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to 320 ℃, heating up at a rate of 8 ℃/min, and keeping the temperature for 1h. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 3
Two groups of polytetrafluoroethylene (particle size 1 μm) and iron powder (median diameter 1 μm) were mixed at a ratio of 40% to 60%, 500g each, and thoroughly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 3h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to be 100 ℃, heating up at a speed of 10 ℃/min, and keeping the temperature for 4 hours. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 4
Polyethylene (particle size 5 μm) and an equal proportion mixture (median diameter 5 μm) of copper, magnesium and manganese powders were mixed in a proportion of 50% and 50%, each group was 500g, and the mixture was thoroughly and uniformly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 3h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to 400 ℃, heating up at a rate of 8 ℃/min, and preserving the heat for 4 hours. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 5
Two groups of polystyrene (particle size 3 μm), equal proportion mixtures of tin, lead and titanium (median diameter 30 μm) were mixed in proportions of 20% and 80%, 500g of each group, and thoroughly and uniformly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 2h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to 200 ℃, heating up at a speed of 10 ℃/min, and keeping the temperature for 1h. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 6
Two groups of polytetrafluoroethylene (particle size 0.4 μm), nickel, cobalt and tungsten in equal proportion (median diameter 5 μm) were mixed in a proportion of 15% and 85%, 500g of each group was thoroughly and uniformly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 2h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to 300 ℃, heating up at a speed of 7 ℃/min, and preserving the heat for 3 hours. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
Example 7
Two groups of polytetrafluoroethylene (particle diameter 2 μm) and nickel powder (median diameter 30 μm) were mixed in a proportion of 15% and 85%, 500g each, and thoroughly mixed. Placing the two groups of mixed powder into two metal tanks, sealing the metal tanks, vacuumizing the metal tanks, and filling a small amount of nitrogen into the metal tanks under the air pressure of-0.06 MPa. Placing the materials into mechanical mixing grinding equipment, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and mixing and grinding for 3h. Cooling to room temperature after the mixed grinding is finished, taking out powder, placing the powder into a crucible, placing the crucible into a high-temperature rotary atmosphere tube furnace, vacuumizing the crucible, performing air pressure of-0.06 MPa, and filling a small amount of nitrogen. Setting the temperature to 330 ℃, heating up at a speed of 7 ℃/min, and preserving the heat for 3 hours. And cooling after the heat preservation is finished, taking out the powder after cooling to room temperature, and carrying out coarse screening.
SEM photographs of the remaining examples are similar to those of examples 1 or 2.
After SEM analysis, a layer of compact and complete shell layer is formed on the surface of the coated metal particles, and the high-ductility polymer material and the hardness difference of the metal powder are utilized for mixed grinding, so that on one hand, the foreign impurities are eliminated, the purity of the composite powder can be ensured, on the other hand, the deformation of the metal powder particles caused by the too high energy is avoided, the coating effect is not influenced, and the high-ductility material can be fully and uniformly attached to the surface of the metal particles by high-temperature treatment, so that a compact protective layer is formed.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (8)

1. A preparation method of high-ductility material coated metal powder is characterized by comprising the following steps of
S1, mixing 10-50% of high molecular polymer and 50-90% of metal powder in percentage by mass, wherein the average particle size of the high molecular polymer is 0.1-5 mu m, and the average particle size of the metal powder is 1-50 mu m;
s2, placing the mixed powder into a closed tank body, and vacuumizing;
s3, filling inert gas into the tank body, and grinding;
s4, roasting the grinded composite powder in an inert gas atmosphere;
s5, cooling the baked composite powder in an inert gas atmosphere, and sieving.
2. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: the high molecular polymer comprises one or more of polyethylene, polystyrene and polytetrafluoroethylene.
3. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: the metal powder comprises one or more of iron, aluminum, copper, magnesium, manganese, tin, lead, titanium, nickel, cobalt and tungsten.
4. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: the grinding time of the high polymer and the metal powder in the tank body is 0.5-4h.
5. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: the inert gas may be nitrogen or argon.
6. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: in S4, the roasting temperature is 100-400 ℃, the heating rate is 6-10 ℃/min, and the heat preservation time is 1-4 h.
7. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: in S2, the air pressure after the vacuumizing treatment is minus 0.06MPa.
8. The method for preparing the high-ductility material coated metal powder according to claim 1, wherein the method comprises the following steps: and S3, regulating the rotating speed to 200rpm, rotating forward for 15min, rotating backward for 15min, circulating, and carrying out mixed grinding for 1-3h.
CN202211699318.4A 2022-12-28 2022-12-28 Preparation method of high-ductility material coated metal powder Pending CN116213734A (en)

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CN116213734A true CN116213734A (en) 2023-06-06

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