CN114535589B - Preparation method of tungsten copper heat sink component for optical module - Google Patents

Preparation method of tungsten copper heat sink component for optical module Download PDF

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Publication number
CN114535589B
CN114535589B CN202210015222.5A CN202210015222A CN114535589B CN 114535589 B CN114535589 B CN 114535589B CN 202210015222 A CN202210015222 A CN 202210015222A CN 114535589 B CN114535589 B CN 114535589B
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tungsten
heat sink
optical module
copper
composite powder
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CN114535589A (en
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陈铮
梁淑华
张乔
邓楠
肖鹏
邹军涛
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Xian University of Technology
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Xian University of Technology
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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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • 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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/026Spray drying of solutions or suspensions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum

Abstract

The invention discloses a preparation method of a tungsten copper heat sink component for an optical module, which is based on wet milling and spray drying granulation to prepare spherical composite powder, wherein copper phases and activated sintering elements are distributed in gaps of nano-sized tungsten particles, and the sintering process not only has copper phase filling and tungsten particle rearrangement caused by the copper liquid phase, but also has solid phase sintering of nano-tungsten powder particles, so that the sintering temperature and the production cost can be greatly reduced. The tungsten copper heat sink component for the optical module is prepared by adopting an injection molding process, the utilization rate of raw materials is high, the dimensional accuracy of parts is good, the heat sink component has excellent thermal performance and the surface state is excellent.

Description

Preparation method of tungsten copper heat sink component for optical module
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method of a tungsten copper heat sink component for an optical module.
Background
With the advent of the 5G era, there is an increasing demand for high-power optical modules, and the power of a single optical module is also increasing, which puts higher demands on the heat conducting performance of the heat sink component of the optical module. The heat conduction performance of the existing Kovar alloy is difficult to meet the requirement, and the tungsten-copper (W-Cu) composite material with excellent heat conduction performance and low thermal expansion coefficient can meet the heat conduction requirement. However, the heat sink components of the light module are generally small in size and the parts are thin in wall and complex in shape. The W-Cu composite material is prepared by adopting a liquid phase sintering and infiltration method. Because W and Cu are not dissolved at all, the W-Cu composite material with high density is difficult to obtain by liquid phase sintering, so that the W-Cu composite material prepared by liquid phase sintering has lower thermal conductivity. In addition, although the infiltration method can prepare the W-Cu composite material with high density and high performance, the infiltration method can only prepare blocks with simple shapes, and the heat sink component for the optical module can be manufactured through a large amount of processing, so that the material waste is high and the efficiency is low. Therefore, it is urgent to find a manufacturing method that can rapidly, at low cost, with high material utilization and obtain a component with excellent heat conductive properties.
Disclosure of Invention
The invention aims to provide a preparation method of a tungsten copper heat sink component for an optical module, and the prepared tungsten copper heat sink component for the optical module has the characteristics of high heat conductivity and low thermal expansion coefficient.
The technical scheme adopted by the invention is that the preparation method of the tungsten copper heat sink component for the optical module comprises the following components in percentage by mass: 8-22% of copper, 0.05-1.0% of activated sintering element, and the balance of tungsten, wherein the method is implemented according to the following steps:
step 1, using tungsten powder, a copper source and an activated sintering element source as raw materials, uniformly mixing the raw materials according to a certain proportion by using wet grinding to prepare slurry, preparing spherical composite powder from the slurry by using spray drying equipment, and calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder;
step 2, mixing spherical W/Cu/activated sintering element composite powder and a binder for 2-4 hours at 150-170 ℃, wherein the volume ratio of the powder to the binder is 45:55-65:35, and preparing injection molding feed;
step 3, preparing a blank in the shape of a tungsten copper heat sink part for the required optical module by feeding on injection molding equipment;
and step 4, degreasing the injection molding blank, and sintering at a high temperature to obtain the tungsten copper heat sink component for the optical module.
The invention is also characterized in that:
the activated sintering element in the step 1 is at least one of soluble Ni, fe, co, pd metal salts.
The particle size of the tungsten powder is 0.2-1 mu m.
In the step 1, the copper source is one or a mixture of a plurality of copper nitrate, copper sulfate and copper chloride.
The particle size of the spherical composite powder in the step 1 is 15-50 mu m, and the sphericity rate is more than 95%.
And step 1, the calcining process of calcining the spherical composite powder in hydrogen is heating to 400 ℃, the heating rate is 1-5 ℃/min, and after heat preservation for 2 hours, heating to 800 ℃ at 5 ℃/min, and heat preservation for 2 hours.
The binder in step 2 is a wax-based binder.
The high-temperature sintering process of the step 4 is as follows: sintering for 1-4 h in hydrogen atmosphere at 1100-1250 ℃.
The thermal conductivity of the tungsten copper heat sink component for the optical module is more than or equal to 200 W.m -1 ·K -1 The thermal expansion coefficient is less than or equal to 8.0X10 -6 The relative density of the composite material is not less than 98 percent.
The invention has the beneficial effects that:
1) According to the invention, the spherical composite powder is prepared based on wet grinding and spray drying granulation, copper phases and activated sintering elements are distributed in gaps of nano-sized tungsten particles, and the sintering process not only has copper phase filling and tungsten particle rearrangement caused by the copper liquid phase, but also has solid phase sintering of nano-tungsten powder particles, so that the sintering temperature and the production cost can be greatly reduced.
2) The tungsten copper heat sink component for the optical module is prepared by adopting an injection molding process, the utilization rate of raw materials is high, the dimensional accuracy of the component is good, the thermal performance of the heat sink component is excellent, and the surface state is excellent.
Drawings
FIG. 1 is a typical microstructure of a tungsten copper heat sink component for an optical module prepared by the method of the present invention
FIG. 2 is a graph of a typical microstructure morphology of a prior art micron W/Cu composite powder after 1350 ℃.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
Example 1
The invention relates to a preparation method of a tungsten copper heat sink component for an optical module, which is implemented according to the following steps:
tungsten powder, copper sulfate and nickel nitrate with the particle size of 0.5 mu m are used as raw materials, and wet grinding is used for mixing the raw materials according to the following weight ratio: uniformly mixing Ni=79.8:20:0.2 in mass ratio to prepare slurry, and preparing the slurry into spherical composite powder by using spray drying equipment; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintered element composite powder, wherein the calcining temperature is 400 ℃, the heating rate is 1 ℃/min, the temperature is kept for 2 hours, the temperature is raised to 800 ℃ at 5 ℃/min, and the temperature is kept for 2 hours, so that spherical composite powder with the particle size of 25 mu m is obtained, and the sphericity rate is 95.5%; mixing spherical W/Cu/activated sintering element composite powder and a wax-based binder for 2 hours at 150 ℃, wherein the volume ratio of the powder to the wax-based binder is 58:42, and preparing injection molding feed; preparing a blank in the shape of a tungsten copper heat sink part for a required optical module by feeding on injection molding equipment; and degreasing the injection molding blank, and sintering at a high temperature in a hydrogen atmosphere at 1150 ℃ to obtain the tungsten copper heat sink component for the optical module.
Thermal conductivity 220 W.m of tungsten copper heat sink component for optical module -1 ·K -1 Coefficient of thermal expansion 7.8X10 -6 The relative density was 98.5%.
Example 2
The invention relates to a preparation method of a tungsten copper heat sink component for an optical module, which is implemented according to the following steps:
uniformly mixing tungsten powder, copper sulfate and ferric sulfate with the particle size of 0.4 mu m by wet grinding according to the mass ratio of W to Cu to Fe=79.65:20:0.35 to prepare slurry, and preparing the slurry into spherical composite powder by spray drying equipment; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintered element composite powder, wherein the calcining temperature is 400 ℃, the heating rate is 2 ℃/min, the temperature is kept for 2 hours, the temperature is raised to 800 ℃ at 5 ℃/min, and the temperature is kept for 2 hours, so that spherical composite powder with the particle size of 18 mu m is obtained, and the sphericity rate is 96.5%; mixing spherical W/Cu/activated sintering element composite powder and a wax-based binder for 2 hours at 150 ℃, wherein the volume ratio of the powder to the wax-based binder is 50:50, and preparing injection molding feed; preparing a blank in the shape of a tungsten copper heat sink part for a required optical module by feeding on injection molding equipment; and degreasing the injection molding blank, and sintering the blank for 2 hours at a high temperature in a hydrogen atmosphere at 1100 ℃ to obtain the tungsten copper heat sink component for the optical module.
The thermal conductivity of the tungsten copper heat sink component for the optical module is 215 W.m -1 ·K -1 A thermal expansion coefficient of 7.5X10 -6 The relative density was 99.0%.
Example 3
The invention relates to a preparation method of a tungsten copper heat sink component for an optical module, which is implemented according to the following steps:
uniformly mixing tungsten powder, copper nitrate and nickel sulfate with the particle size of 0.8 mu m by wet grinding according to the mass ratio of W to Cu to Ni=84.5 to 15 to 0.5 to prepare slurry, and preparing the slurry into spherical composite powder with the spherical rate of 95.0% by spray drying equipment; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process is that the room temperature is heated to 400 ℃, the heating rate is 3 ℃/min, the temperature is kept for 2 hours, and the temperature is raised to 800 ℃ at 5 ℃/min, and the temperature is kept for 2 hours, so that the spherical composite powder with the particle size of 30 μm is obtained; mixing spherical W/Cu/activated sintering element composite powder and a binder for 2 hours at 150 ℃, wherein the volume ratio of the powder to the wax-based binder is 58:42, and preparing injection molding feed; preparing a blank in the shape of a tungsten copper heat sink part for a required optical module by feeding on injection molding equipment; and degreasing the injection molding blank, and sintering at a high temperature in a hydrogen atmosphere at 1180 ℃ for 2.5 hours to obtain the tungsten copper heat sink component for the optical module.
Thermal conductivity of tungsten copper heat sink component for optical module prepared is 205 W.m -1 ·K -1 Coefficient of thermal expansion 7.0X10 -6 The relative density was 99.0%.
Example 4
The invention relates to a preparation method of a tungsten copper heat sink component for an optical module, which is implemented according to the following steps:
uniformly mixing tungsten powder, copper nitrate and cobalt nitrate with the particle size of 0.25 mu m by wet grinding according to the mass ratio of W to Cu to Co=89.8 to 10 to 0.2 to prepare slurry, and preparing the slurry into spherical composite powder by spray drying equipment; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process is that the room temperature is heated to 400 ℃, the heating rate is 4 ℃/min, the temperature is kept for 2 hours, the temperature is raised to 800 ℃ at 5 ℃/min, and the temperature is kept for 2 hours, so that the spherical composite powder with the particle size of 20 mu m is obtained, and the sphericity rate is 97.5%; mixing spherical W/Cu/activated sintering element composite powder and a binder for 2 hours at 160 ℃, wherein the volume ratio of the powder to the binder is 48:52, and preparing injection molding feed; preparing a blank in the shape of a tungsten copper heat sink part for a required optical module by feeding on injection molding equipment; and degreasing the injection molding blank, and sintering at a high temperature in a hydrogen atmosphere of 1200 ℃ for 3 hours to obtain the tungsten copper heat sink component for the optical module.
The thermal conductivity of the tungsten copper heat sink component for the prepared optical module is 201 W.m -1 ·K -1 Coefficient of thermal expansion 5.2×10 -6 The relative density was 98.5%.
Example 5
The invention relates to a preparation method of a tungsten copper heat sink component for an optical module, which is implemented according to the following steps:
uniformly mixing tungsten powder, copper nitrate and cobalt nitrate with the particle size of 0.25 mu m by wet grinding according to the mass ratio of W to Cu to Co=79.75 to 20 to 0.25 to prepare slurry, and preparing the slurry into spherical composite powder with the spherical rate of 98.0% by spray drying equipment; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process is that the room temperature is heated to 400 ℃, the heating rate is 5 ℃/min, the temperature is kept for 2 hours, and the temperature is raised to 800 ℃ at 5 ℃/min, and the temperature is kept for 2 hours, so that the spherical composite powder with the particle size of 20 μm is obtained; mixing spherical W/Cu/activated sintering element composite powder and a binder for 2 hours at 160 ℃, wherein the volume ratio of the powder to the binder is 48:52, and preparing injection molding feed; preparing a blank in the shape of a tungsten copper heat sink part for a required optical module by feeding on injection molding equipment; and degreasing the injection molding blank, and sintering at 1125 ℃ under a hydrogen atmosphere for 3 hours to obtain the tungsten copper heat sink component for the optical module.
The thermal conductivity of the tungsten copper heat sink component for the optical module is 225 W.m -1 ·K -1 A thermal expansion coefficient of 7.5X10 -6 The relative density was 99.5%.
The microstructure of the material obtained according to example 1 is shown in FIG. 1, and it can be seen from FIG. 1 that the W-20Cu composite material can be fully densified only after sintering at 1150 ℃; in contrast, as shown in fig. 2, the microstructure of the mixed powder of micron W (5 μm)/Cu (5 μm) after liquid phase sintering at 1350 ℃ in the prior art shows that a large number of pores still exist in the sintered W-Cu composite material, which greatly reduces the heat conductivity of the W-Cu composite material.
According to the preparation method of the tungsten copper heat sink component for the optical module, disclosed by the invention, the spherical composite powder is prepared based on wet grinding and spray drying granulation, copper phases and activated sintering elements are distributed in gaps of nano-sized tungsten particles, copper phase filling and tungsten particle rearrangement caused by the copper liquid phase are carried out in the sintering process, and solid phase sintering of nano-tungsten powder particles is carried out, so that the sintering temperature and the production cost can be greatly reduced. The tungsten copper heat sink component for the optical module is prepared by adopting an injection molding process, the utilization rate of raw materials is high, the dimensional accuracy of parts is good, the heat sink component has excellent thermal performance and the surface state is excellent.

Claims (3)

1. The preparation method of the tungsten copper heat sink component for the optical module is characterized in that the tungsten copper heat sink component for the optical module comprises the following components in percentage by mass: 8-22% of copper, 0.05-1.0% of activated sintering element, and the balance of tungsten, wherein the method comprises the following steps of:
step 1, using tungsten powder, a copper source and an activated sintering element source as raw materials, uniformly mixing the raw materials according to a certain proportion by using wet grinding to prepare slurry, preparing spherical composite powder from the slurry by using spray drying equipment, and calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder;
the activated sintering element is at least one of soluble Ni, fe, co, pd metal salts;
the copper source is one or more of copper nitrate, copper sulfate and copper chloride;
the calcining process of calcining the spherical composite powder in hydrogen is that the spherical composite powder is heated to 400 ℃, the heating rate is 1-5 ℃/min, the spherical composite powder is heat-preserved for 2 hours, and then the spherical composite powder is heated to 800 ℃ at 5 ℃/min and is heat-preserved for 2 hours;
step 2, mixing spherical W/Cu/activated sintering element composite powder and a binder for 2-4 hours at 150-170 ℃, wherein the volume ratio of the powder to the binder is 45:55-65:35, and preparing injection molding feed;
the binder is a wax-based binder;
step 3, preparing a blank in the shape of a tungsten copper heat sink part for the required optical module by feeding on injection molding equipment;
step 4, degreasing the injection molding blank, and sintering at a high temperature to obtain a tungsten copper heat sink component for the optical module;
the high-temperature sintering process comprises the following steps: sintering for 1-4 hours in hydrogen atmosphere at 1100-1250 ℃;
the thermal conductivity of the tungsten copper heat sink component for the optical module is more than or equal to 200 W.m -1 ·K -1 The thermal expansion coefficient is less than or equal to 8.0X10 -6 The relative density of the composite material is not less than 98 percent.
2. The method for manufacturing a tungsten copper heat sink component for an optical module according to claim 1, wherein the tungsten powder has a particle size of 0.2-1 μm.
3. The method for manufacturing a tungsten copper heat sink component for an optical module according to claim 1, wherein the particle size of the spherical composite powder in the step 1 is 15-50 μm, and the sphericity is more than 95%.
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