CN113070474A - Preparation and forming method of nano tungsten-copper alloy radiating fin - Google Patents

Preparation and forming method of nano tungsten-copper alloy radiating fin Download PDF

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Publication number
CN113070474A
CN113070474A CN202110336280.3A CN202110336280A CN113070474A CN 113070474 A CN113070474 A CN 113070474A CN 202110336280 A CN202110336280 A CN 202110336280A CN 113070474 A CN113070474 A CN 113070474A
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copper alloy
radiating fin
nano tungsten
alloy radiating
tungsten
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赵利亚
姚艳斌
周永贵
张越
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Shenzhen Pim Technology Co ltd
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Shenzhen Pim Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/006Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/108Mixtures obtained by warm mixing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention relates to the technical field of powder metallurgy injection molding, and discloses a preparation and forming method of a nano tungsten-copper alloy radiating fin, which comprises the following steps: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; extruding the feed after vacuum mixing by a double-screw machine according to preset times; adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin; and (3) sintering the degreased injection molding blank of the nano tungsten-copper alloy radiating fin by passing hydrogen to obtain the nano tungsten-copper alloy radiating fin. The invention can prepare the nano tungsten-copper alloy radiating fin with uniform tissue, high density and low carbon residue.

Description

Preparation and forming method of nano tungsten-copper alloy radiating fin
Technical Field
The invention relates to the technical field of powder metallurgy injection molding, in particular to a preparation and forming method of a nano tungsten-copper alloy radiating fin.
Background
The tungsten-copper alloy has the characteristics of high melting point and low expansion of tungsten and high electric conductivity and high thermal conductivity of copper, and the thermal expansion coefficient, the thermal conductivity and the electric conductivity of the tungsten-copper alloy can be adjusted according to the percentage content of tungsten and copper components. Therefore, the method plays an important role in the fields of mobile communication equipment, medical instruments, precision mold processing, microelectronics and the like.
The traditional method for preparing tungsten-copper alloy is to carry out compression molding on tungsten-copper powder and finally produce corresponding parts by machining. However, with the development of science and technology, the application field is widened continuously, the market demand is updated continuously, and the tungsten-copper alloy not only has a more complex structure, but also has higher performance requirements. The traditional die forming process is difficult to produce tungsten-copper alloy with complex shape, and the traditional tungsten-copper alloy product is difficult to have good electric conduction and heat conduction performance while considering the performance, thereby seriously restricting the development of tungsten-copper alloy materials.
Therefore, how to provide a method for preparing and forming a nano tungsten-copper alloy heat sink to obtain a nano tungsten-copper alloy heat sink with uniform structure, high density and low carbon residue is a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for preparing and forming a nano tungsten-copper alloy radiating fin so as to obtain the nano tungsten-copper alloy radiating fin with uniform tissue, high density, low carbon residue and good heat conductivity.
Therefore, according to a first aspect, the embodiment of the invention discloses a method for preparing and forming a nano tungsten-copper alloy radiating fin, which comprises the following steps: high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; the mixed powder is precipitated and dried after being ball-milled uniformly, and is sieved and packaged in a sealing box; vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; and (3) extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times; injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin; and (3) sintering: and (3) carrying out hydrogen sintering on the degreased injection molding blank of the nano tungsten-copper alloy radiating fin to obtain the nano tungsten-copper alloy radiating fin.
Optionally, the step of adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and performing vacuum refining to prepare the feed specifically comprises the following steps:
when the oxygen content shows 0%, starting to heat the vacuum internal mixer; when the temperature of the materials in the banburying chamber is about 60 ℃, starting stirring until the temperature is raised to about 150 ℃; after mixing thoroughly for 30 minutes, the discharge was cooled and broken into granules to form the feed.
Optionally, the graphene powder accounts for 1% -5% of the mixed powder by mass, and the weight ratio of the absolute ethyl alcohol to the mixed powder is (0.1-0.5): 1, the weight ratio of the grinding tungsten balls of the high-energy ball mill to the mixed powder is (1-5): 1.
optionally, the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time of the high-energy ball mill is 30-100 h.
Optionally, the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax and 1-10% of stearic acid.
Optionally, the binder accounts for 1-10% of the feed weight, the nano tungsten powder accounts for 50-95% of the feed weight, the nano tungsten powder accounts for 5-40% of the feed weight, and the graphene powder accounts for 1-10% of the feed weight.
Optionally, the mixing temperature of the vacuum mixer is 120 ℃ to 180 ℃.
Optionally, the solvent for solvent degreasing is trichloroethylene, n-heptane or an environment-friendly novel cleaning agent, the degreasing temperature for solvent degreasing is 30-80 ℃, and the degreasing time is 2-8 h; and after extraction, drying at the temperature of 30-80 ℃ for 1-4 h.
Optionally, the thermal degreasing is performed by using bottled hydrogen or ammonia decomposition hydrogen atmosphere, and the degreasing temperature is 500-800 ℃.
Optionally, sintering the degreased injection-molded blank of the nano tungsten-copper alloy radiating fin in a hydrogen atmosphere at 1150-1400 ℃ for 60-120 min.
The invention has the following beneficial effects: the preparation and forming method of the nano tungsten-copper alloy radiating fin is provided by adopting the steps of high-energy ball milling, vacuum mixing, extrusion granulation, injection molding, degreasing and sintering, and the nano tungsten-copper alloy radiating fin with uniform tissue, high density, low carbon residue and good heat conductivity is obtained; due to the fact that the graphene is added into the tungsten-copper alloy, the electrical conductivity and the thermal conductivity of the nanometer tungsten-copper alloy radiating fin are improved while the strength of the product is guaranteed; the special binder is adopted, so that the mixing uniformity of the nano tungsten-copper powder and the graphene powder and the strength of an injection molding blank are ensured, the phenomena of degreasing, bubbling and cracking of the conventional binder are avoided, and the carbon residue of the nano tungsten-copper alloy radiating fin is reduced; by adopting the powder injection molding technology and the hydrogen atmosphere sintering process, the nano tungsten-copper alloy radiating fin product with complex shape, high dimensional precision and uniform tissue structure can be prepared, and the production efficiency is higher.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a flowchart of a method for forming a nano tungsten-copper alloy heat sink disclosed in this embodiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; the two elements may be directly connected or indirectly connected through an intermediate medium, or may be communicated with each other inside the two elements, or may be wirelessly connected or wired connected. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1:
the embodiment of the invention discloses a preparation and forming method of a nano tungsten-copper alloy radiating fin, which comprises the following steps of:
step S101, high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; after ball milling, the mixed powder is precipitated, dried and sieved and packaged in a sealing box; in the embodiment, the weight ratio of the absolute ethyl alcohol to the metal mixed powder is (0.1-0.5): 1, and the weight ratio of the grinding tungsten balls of the high-energy ball mill to the mixed powder is (1-5): 1; the particle size of the nano tungsten powder is 10-100 nm, the particle size of the nano copper powder is 100-500 nm, the diameter of a grinding ball is 3-8 mm, the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time is 30-100 h.
Step S102, vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; in this embodiment, the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax, and stearic acid: 1 to 10 percent.
In the specific implementation process, the nano tungsten powder accounts for 50-95% of the feeding weight, the nano copper powder accounts for 5-40% of the feeding weight, and the graphene powder accounts for 1-10% of the feeding weight. The binder accounts for 1 to 10 percent of the weight of the feed.
The mixing temperature of the mixed powder and the binder is 120-180 ℃. Adding the mixed powder into a mixing barrel of a mixer for preheating, adding a binder when the temperature of the mixed powder reaches 80 ℃, heating and adjusting the rotating speed of the mixer to 200 r/min; when the temperature of the mixed powder and the binder reaches 120 ℃, heating and adjusting the rotating speed of the mixer to 400 r/min; when the temperature of the mixed powder and the binder reaches 150 ℃ and the metal powder and the binder are sufficiently mixed, the mixer stops rotating and heating to prepare a mixed material.
Step S103, extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times;
step S104, injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; in this embodiment, the injection temperature is 130-190 ℃, the injection pressure is 25-95 MPa, the injection speed is 30-90%, and the mold temperature is 40-80 ℃.
Step S105, degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin; in the embodiment, solvent degreasing is performed by adopting a water-bath heating mode, trichloroethylene, n-heptane or an environment-friendly novel cleaning agent is selected as a degreasing solvent, the degreasing temperature is 30-80 ℃, and the degreasing time is 2-8 hours. And drying after degreasing, wherein the drying temperature is 30-80 ℃, and the drying time is 1-4 hours. Wherein the degreasing atmosphere of the hot degreasing is hydrogen, and the degreasing temperature range is 400-750 ℃.
Step S106, sintering: and (3) sintering the degreased injection molding blank of the nano tungsten-copper alloy radiating fin by passing hydrogen to obtain the nano tungsten-copper alloy radiating fin. In this embodiment, the sintering temperature is 1150-1400 ℃ and the sintering time is 60-120 minutes.
Example 2:
the embodiment of the invention discloses a preparation and forming method of a nano tungsten-copper alloy radiating fin, which comprises the following steps of:
step S101, high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; after ball milling, the mixed powder is precipitated, dried and sieved and packaged in a sealing box; in the embodiment, the graphene powder accounts for 1% by mass of the metal mixed powder, and the weight ratio of the absolute ethyl alcohol to the metal mixed powder is (0.1-0.5): 1, the weight ratio of the grinding tungsten balls to the mixed powder of the high-energy ball mill is (1-5): 1. the particle size of the nano tungsten powder is 10-100 nm, the particle size of the nano copper powder is 100-500 nm, the diameter of a grinding ball is 3-8 mm, the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time is 30-100 h.
Step S102, vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; in this embodiment, the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax, and stearic acid: 1 to 10 percent.
In the specific implementation process, the nano tungsten powder accounts for 50-95% of the feeding weight, and the nano copper powder accounts for 5-40% of the feeding weight. The binder accounts for 1 to 10 percent of the weight of the feed.
The mixing temperature of the mixed powder and the binder is 120-180 ℃. Adding the mixed powder into a mixing barrel of a mixer for preheating, adding a binder when the temperature of the mixed powder reaches 80 ℃, heating and adjusting the rotating speed of the mixer to 200 r/min; when the temperature of the mixed powder and the binder reaches 120 ℃, heating and adjusting the rotating speed of the mixer to 400 r/min; when the temperature of the mixed powder and the binder reaches 150 ℃ and the metal powder and the binder are sufficiently mixed, the mixer stops rotating and heating to prepare a mixed material.
Step S103, extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times;
step S104, injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; in this embodiment, the injection temperature is 130-190 ℃, the injection pressure is 25-95 MPa, the injection speed is 30-90%, and the mold temperature is 40-80 ℃.
Step S105, degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin; in the embodiment, solvent degreasing is performed by adopting a water-bath heating mode, trichloroethylene, n-heptane or an environment-friendly novel cleaning agent is selected as a degreasing solvent, the degreasing temperature is 30-80 ℃, and the degreasing time is 2-8 hours. And drying after degreasing, wherein the drying temperature is 30-80 ℃, and the drying time is 1-4 hours. Wherein the degreasing atmosphere of the hot degreasing is hydrogen, and the degreasing temperature range is 400-750 ℃.
Step S106, sintering: and (3) sintering the degreased injection molding blank of the nano tungsten-copper alloy radiating fin by passing hydrogen to obtain the nano tungsten-copper alloy radiating fin. In this embodiment, the sintering temperature is 1150-1400 ℃ and the sintering time is 60-120 minutes.
Example 3:
the embodiment of the invention discloses a preparation and forming method of a nano tungsten-copper alloy radiating fin, which comprises the following steps of:
step S101, high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; after ball milling, the mixed powder is precipitated, dried and sieved and packaged in a sealing box; in this embodiment, the mass ratio of graphene to the metal mixed powder is 3%. The weight ratio of the absolute ethyl alcohol to the metal mixed powder is (0.1-0.5): 1, and the weight ratio of the grinding balls of the high-energy ball milling to the metal powder is (1-5): 1. The particle size of the nano tungsten powder is 10-100 nm, the particle size of the nano copper powder is 100-500 nm, the diameter of a grinding ball is 3-8 mm, the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time is 30-100 h.
Step S102, vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; in this embodiment, the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax, stearic acid: 1 to 10 percent. The binder accounts for 1 to 10 percent of the weight of the feed.
In the specific implementation process, the nano tungsten powder accounts for 50-95% of the feeding weight, and the nano copper powder accounts for 5-40% of the feeding weight.
The mixing temperature of the mixed powder and the binder is 120-180 ℃. Adding the mixed powder into a mixing barrel of a mixer for preheating, adding a binder when the temperature of the mixed powder reaches 80 ℃, heating and adjusting the rotating speed of the mixer to 200 r/min; when the temperature of the mixed powder and the binder reaches 120 ℃, heating and adjusting the rotating speed of the mixer to 400 r/min; when the temperature of the mixed powder and the binder reaches 150 ℃ and the metal powder and the binder are sufficiently mixed, the mixer stops rotating and heating to prepare a mixed material.
Step S103, extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times;
step S104, injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; in this embodiment, the injection temperature is 130-190 ℃, the injection pressure is 25-95 MPa, the injection speed is 30-90%, and the mold temperature is 40-80 ℃.
Step S105, degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin; in the embodiment, solvent degreasing is performed by adopting a water-bath heating mode, trichloroethylene, n-heptane or an environment-friendly novel cleaning agent is selected as a degreasing solvent, the degreasing temperature is 30-80 ℃, and the degreasing time is 2-8 hours. And drying after degreasing, wherein the drying temperature is 30-80 ℃, and the drying time is 1-4 hours. Wherein the degreasing atmosphere of the hot degreasing is hydrogen, and the degreasing temperature range is 400-750 ℃.
Step S106, sintering: and (3) sintering the degreased injection molding blank of the nano tungsten-copper alloy radiating fin by passing hydrogen to obtain the nano tungsten-copper alloy radiating fin. In this embodiment, the sintering temperature is 1150-1400 ℃ and the sintering time is 60-120 minutes.
Example 4:
the embodiment of the invention discloses a preparation and forming method of a nano tungsten-copper alloy radiating fin, which comprises the following steps of:
step S101, high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; after ball milling, the mixed powder is precipitated, dried and sieved and packaged in a sealing box; in the embodiment, the graphene powder accounts for 5% of the metal mixed powder by mass, the weight ratio of the absolute ethyl alcohol to the metal mixed powder is (0.1-0.5): 1, and the weight ratio of the grinding tungsten balls of the high-energy ball mill to the metal powder is (1-5): 1. the particle size of the nano tungsten powder is 10-100 nm, the particle size of the nano copper powder is 100-500 nm, the diameter of a tungsten ball is 3-8 mm, the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time is 30-100 h.
Step S102, vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed; in this embodiment, the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax, and stearic acid: 1 to 10 percent.
In the specific implementation process, the nano tungsten powder accounts for 50-95% of the feeding weight, and the nano copper powder accounts for 5-40% of the feeding weight. The binder accounts for 1 to 10 percent of the weight of the feed.
The mixing temperature of the mixed powder and the binder is 120-180 ℃. Adding the mixed powder into a mixing barrel of a mixer for preheating, adding a binder when the temperature of the mixed powder reaches 80 ℃, heating and adjusting the rotating speed of the mixer to 200 r/min; when the temperature of the mixed powder and the binder reaches 120 ℃, heating and adjusting the rotating speed of the mixer to 400 r/min; when the temperature of the mixed powder and the binder reaches 150 ℃ and the metal powder and the binder are sufficiently mixed, the mixer stops rotating and heating to prepare a mixed material.
Step S103, extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times;
step S104, injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process; in this embodiment, the injection temperature is 130-190 ℃, the injection pressure is 25-95 MPa, the injection speed is 30-90%, and the mold temperature is 40-80 ℃.
Step S105, degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin; in the embodiment, solvent degreasing is performed by adopting a water-bath heating mode, trichloroethylene, n-heptane or an environment-friendly novel cleaning agent is selected as a degreasing solvent, the degreasing temperature is 30-80 ℃, and the degreasing time is 2-8 hours. And drying after degreasing, wherein the drying temperature is 30-80 ℃, and the drying time is 1-4 hours. Wherein the degreasing atmosphere of the hot degreasing is hydrogen, and the degreasing temperature range is 400-750 ℃.
Step S106, sintering: and (3) sintering the degreased injection molding blank of the nano tungsten-copper alloy radiating fin by passing hydrogen to obtain the nano tungsten-copper alloy radiating fin. In this embodiment, the sintering temperature is 1150-1400 ℃ and the sintering time is 60-120 minutes.
The performance parameters of the nano tungsten-copper alloy samples prepared in examples 1 to 4 were tested, and the test standards and results are as follows:
and (3) conductivity test: preparing a nano tungsten-copper alloy sample according to a standard, wherein the sample size is as follows: 50X 4mm, the upper and lower surfaces of the sample are flat, and three points are tested according to the standard. Each set of examples tested 5 samples.
And (3) testing thermal conductivity: preparing a nano tungsten-copper alloy sample according to a standard, wherein the sample size is as follows: 10X 12.7 mm. Each set of examples tested 5 samples.
And (3) testing the density: the sintered product was tested directly, and 5 samples were tested per set of examples. The test results are shown in table 1 below.
TABLE 1 indices of Performance of materials corresponding to examples 1, 2, 3, 4
Figure BDA0002997815640000101
As can be seen from table 1 above, in the embodiment of the present invention, the density of the nano tungsten-copper alloy sample gradually decreases with the increase of the addition amount of graphene, and both the electrical conductivity and the thermal conductivity increase with the increase of the content of graphene. The reasonable addition of the graphene can improve the electrical conductivity and the thermal conductivity of the nano tungsten-copper alloy sample to a certain extent under the condition that the density meets the standard of the sample.
According to the invention, nano tungsten copper is used as a base material, and graphene with different contents is added, so that the electrical conductivity and the thermal conductivity of the product can be controlled, and the product has good electrical conductivity and thermal conductivity under certain strength. On the other hand, the special binder is adopted, so that the mixing uniformity of the nano tungsten-copper powder and the graphene powder and the strength of an injection molding blank are ensured, and the phenomena of degreasing, bubbling and cracking of the conventional binder are avoided. The operation method is simple and easy to implement, the nano tungsten-copper alloy radiating fin with a complex shape and a uniform tissue structure can be directly produced by adopting a powder injection molding technology, the machining cost and the material cost are saved, and the production efficiency of the product is improved.
The preparation and forming method of the nano tungsten-copper alloy radiating fin is provided by adopting the steps of high-energy ball milling, vacuum mixing, extrusion granulation, injection molding, degreasing and sintering, and the nano tungsten-copper alloy radiating fin with uniform tissue, high density, low carbon residue and good heat conductivity is obtained; due to the fact that the graphene is added into the tungsten-copper alloy, the electrical conductivity and the thermal conductivity of the nanometer tungsten-copper alloy radiating fin are improved while the strength of the product is guaranteed; the special binder is adopted, so that the mixing uniformity of the nano tungsten-copper powder and the graphene powder and the strength of an injection molding blank are ensured, the phenomena of degreasing, bubbling and cracking of the conventional binder are avoided, and the carbon residue of the nano tungsten-copper alloy radiating fin is reduced; by adopting the powder injection molding technology and the hydrogen atmosphere sintering process, the nano tungsten-copper alloy radiating fin product with complex shape, high dimensional precision and uniform tissue structure can be prepared, and the production efficiency is high.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A preparation forming method of a nanometer tungsten-copper alloy radiating fin is characterized by comprising the following steps:
high-energy ball milling: adding mixed powder consisting of nano tungsten powder, nano copper powder and graphene powder into a tank body of a high-energy ball mill, and then adding a preset amount of absolute ethyl alcohol and tungsten balls for wet milling; the mixed powder is precipitated and dried after being ball-milled uniformly, and is sieved and packaged in a sealing box;
vacuum mixing: adding the uniformly mixed powder and a special wax-based binder into a vacuum internal mixer, and vacuumizing and refining to prepare a feed;
and (3) extrusion granulation: extruding the feed after vacuum mixing by a double-screw machine according to preset times, wherein the preset times are 3 or 4 times;
injection molding: adding the granulated feed into an injection machine, and injecting into a nano tungsten-copper alloy radiating fin injection blank under a specific process;
degreasing: sequentially carrying out solvent degreasing and thermal degreasing on the injection molded blank of the nano tungsten-copper alloy radiating fin so as to remove the binder in the injection molded blank of the nano tungsten-copper alloy radiating fin;
and (3) sintering: and (3) carrying out hydrogen sintering on the degreased injection molding blank of the nano tungsten-copper alloy radiating fin to obtain the nano tungsten-copper alloy radiating fin.
2. The method for preparing and forming a nano tungsten-copper alloy radiating fin according to claim 1, wherein the step of adding the uniformly mixed powder and the special wax-based binder into a vacuum internal mixer, and the step of vacuum refining to prepare the feed material specifically comprises the following steps:
when the oxygen content shows 0%, starting to heat the vacuum internal mixer; when the temperature of the materials in the banburying chamber is about 60 ℃, starting stirring until the temperature is raised to about 150 ℃; after mixing thoroughly for 30 minutes, the discharge was cooled and broken into granules to form the feed.
3. The method for preparing and forming the nano tungsten-copper alloy radiating fin according to claim 1, wherein the graphene powder accounts for 1-5% by mass of the mixed powder, and the weight ratio of the absolute ethyl alcohol to the mixed powder is (0.1-0.5): 1, the weight ratio of the grinding tungsten balls of the high-energy ball mill to the mixed powder is (1-5): 1.
4. the preparation and forming method of the nano tungsten-copper alloy radiating fin according to claim 1, wherein the rotating speed of the high-energy ball mill is 100-500 r/min, and the ball milling time of the high-energy ball mill is 30-100 h.
5. The method for preparing and forming the nano tungsten-copper alloy radiating fin according to claim 1, wherein the binder comprises the following components in percentage by mass: 30-80% of paraffin, 5-20% of microcrystalline wax, 10-40% of high-density polyethylene, 5-20% of ethylene-vinyl acetate copolymer, 1-20% of PE wax and 1-10% of stearic acid.
6. The method for preparing and forming a nano tungsten-copper alloy radiating fin as claimed in claim 1, wherein the binder accounts for 1-10% of the weight of the feed material, the nano tungsten powder accounts for 50-95% of the weight of the feed material, the nano tungsten powder accounts for 5-40% of the weight of the feed material, and the graphene powder accounts for 1-10% of the weight of the feed material.
7. The method for preparing and forming a nano tungsten-copper alloy radiating fin according to claim 1, wherein the mixing temperature of the vacuum mixer is 120 ℃ to 180 ℃.
8. The preparation and forming method of the nano tungsten-copper alloy radiating fin according to claim 1, wherein a solvent for solvent degreasing is trichloroethylene, n-heptane or an environment-friendly novel cleaning agent, the degreasing temperature of the solvent degreasing is 30-80 ℃, and the degreasing time is 2-8 h; and after extraction, drying at the temperature of 30-80 ℃ for 1-4 h.
9. The method for preparing and forming a nano tungsten-copper alloy heat sink according to claim 1, wherein the thermal degreasing is performed in an atmosphere of bottled hydrogen or ammonia decomposition hydrogen at a degreasing temperature of 500 ℃ to 800 ℃.
10. The method for preparing and forming the nano tungsten-copper alloy radiating fin according to claim 1, wherein the degreased nano tungsten-copper alloy radiating fin injection blank is sintered in a hydrogen atmosphere, the sintering temperature is 1150-1400 ℃, and the heat preservation time is 60-120 min.
CN202110336280.3A 2021-03-29 2021-03-29 Preparation and forming method of nano tungsten-copper alloy radiating fin Pending CN113070474A (en)

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