CN114535589A - 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
CN114535589A
CN114535589A CN202210015222.5A CN202210015222A CN114535589A CN 114535589 A CN114535589 A CN 114535589A CN 202210015222 A CN202210015222 A CN 202210015222A CN 114535589 A CN114535589 A CN 114535589A
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tungsten
heat sink
optical module
copper
sink component
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CN114535589B (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 used for preparing spherical composite powder based on wet grinding and spray drying granulation, wherein a copper phase and an activated sintering element are distributed in gaps of tungsten particles with nanometer sizes, and the sintering process not only has copper phase filling and tungsten particle rearrangement caused by a copper liquid phase, but also has solid-phase sintering of the 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 raw material utilization rate is high, the size precision of parts is good, the thermal performance of the heat sink component is excellent, 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, the demand for high-power optical modules is increasing, and the power of a single optical module is also increasing, which puts higher requirements on the heat-conducting performance of a heat sink component of the optical module. The heat-conducting property of the existing Kovar alloy is difficult to meet the requirement, and the tungsten-copper (W-Cu) composite material with excellent heat-conducting property and low thermal expansion coefficient can meet the heat-conducting requirement. However, the heat sink member of the optical module is generally small in size, and the parts are thin and complicated in shape. The W-Cu composite material is prepared by adopting liquid phase sintering and infiltration methods. As W and Cu are not completely dissolved in a solid solution, the W-Cu composite material with high density is difficult to obtain by liquid phase sintering, and the heat conductivity of the W-Cu composite material prepared by liquid phase sintering is lower. In addition, although the infiltration method can prepare a high-density and high-performance W-Cu composite material, the infiltration method can only prepare a block body with a simple shape, and a large amount of processing is needed to prepare a heat sink component for an optical module, so that the material waste is large and the efficiency is low. Therefore, it is urgent to find a method for manufacturing a member which can be rapidly manufactured at low cost and with high material utilization and excellent thermal conductivity.
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 invention adopts the technical scheme 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, and is specifically implemented according to the following steps:
step 1, taking 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 wet grinding to prepare slurry, preparing the slurry into spherical composite powder by utilizing 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 the spherical W/Cu/activated sintering element composite powder and a binder at the temperature of 150-170 ℃ for 2-4 hours, wherein the volume ratio of the powder to the binder is 45: 55-65: 35, and preparing an injection molding feed;
step 3, preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed;
and 4, degreasing the injection molding blank, and sintering at high temperature to obtain the tungsten-copper heat sink component for the optical module.
The invention is also characterized in that:
in the step 1, the activated sintering element is at least one of soluble Ni, Fe, Co and Pd metal salts.
The particle size of the tungsten powder is 0.2-1 μm.
In the step 1, the copper source is one or a mixture of copper nitrate, copper sulfate and copper chloride.
In the step 1, the particle size of the spherical composite powder is 15-50 mu m, and the sphericity rate is more than 95%.
The calcining process of calcining the spherical composite powder in hydrogen in the step 1 is heating to 400 ℃, the heating rate is 1-5 ℃/min, keeping the temperature for 2h, then heating to 800 ℃ at the speed of 5 ℃/min, and keeping the temperature for 2 h.
The binder in the step 2 is a wax-based binder.
Step 4, the high-temperature sintering process comprises the following steps: sintering for 1-4 h in 1100-1250 ℃ hydrogen atmosphere.
The heat conductivity of the tungsten-copper heat sink component for the optical module is more than or equal to 200 W.m-1·K-1Coefficient of thermal expansion less than or equal to 8.0 x 10-6and/K, the relative density is more than or equal to 98 percent.
The invention has the beneficial effects that:
1) the invention prepares the spherical composite powder based on wet grinding and spray drying granulation, the copper phase and the activated sintering element are distributed in the gaps of the tungsten particles with nanometer size, 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 the nanometer tungsten powder particles, thereby greatly reducing the sintering temperature and the production cost.
2) The tungsten-copper heat sink component for the optical module is prepared by adopting an injection molding process, the raw material utilization rate is high, the size precision of parts 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 diagram of a tungsten-copper heat sink component for an optical module prepared by the method of the present invention
FIG. 2 is a typical microstructure morphology of a micron W/Cu composite powder sintered at 1350 ℃ in the prior art.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
The invention relates to a preparation method of a tungsten-copper heat sink component for an optical module, which is implemented by the following steps:
tungsten powder with the particle size of 0.5 mu m, copper sulfate and nickel nitrate are used as raw materials, and the raw materials are subjected to wet grinding according to the weight ratio of W to Cu: uniformly mixing Ni (79.8: 20: 0.2) in a 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 sintering element composite powder, wherein the calcining temperature is 400 ℃, the heating rate is 1 ℃/min, after the temperature is kept for 2h, the temperature is raised to 800 ℃ at the speed of 5 ℃/min, the temperature is kept for 2h, and the spherical composite powder with the particle size of 25 mu m is obtained, and the sphericity rate is 95.5%; mixing the spherical W/Cu/activated sintering element composite powder and a wax-based binder at 150 ℃ for 2h, wherein the volume ratio of the powder to the wax-based binder is 58:42, and preparing an injection molding feed; preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed; degreasing the injection molding blank, and sintering at 1150 ℃ in a hydrogen atmosphere at high temperature to obtain the tungsten-copper heat sink component for the optical module.
Prepared tungsten-copper heat sink component for optical module has heat conductivity of 220 W.m-1·K-1Coefficient of thermal expansion of 7.8X 10-6The 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 by the following steps:
tungsten powder with the particle size of 0.4 mu m, copper sulfate and ferric sulfate are used as raw materials, the raw materials are uniformly mixed according to the mass ratio of W to Cu to Fe of 79.65 to 20 to 0.35 by wet grinding to prepare slurry, and then spray drying equipment is used for preparing the slurry into spherical composite powder; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining temperature is 400 ℃, the heating rate is 2 ℃/min, after the temperature is kept for 2h, the temperature is raised to 800 ℃ at 5 ℃/min, the temperature is kept for 2h, the spherical composite powder with the particle size of 18 mu m is obtained, and the sphericity rate is 96.5%; mixing the spherical W/Cu/activated sintering element composite powder and a wax-based binder at 150 ℃ for 2h, wherein the volume ratio of the powder to the wax-based binder is 50:50, and preparing an injection molding feed; preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed; and degreasing the injection molding blank, and sintering the degreased injection molding blank for 2h at a high temperature in a hydrogen atmosphere at 1100 ℃ to obtain the tungsten-copper heat sink component for the optical module.
The prepared tungsten-copper heat sink component for the optical module has the thermal conductivity of 215 W.m-1·K-1Coefficient of thermal expansion of 7.5X 10-6The 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 by the following steps:
tungsten powder with the particle size of 0.8 mu m, copper nitrate and nickel sulfate are used as raw materials, the raw materials are uniformly mixed according to the mass ratio of W to Cu to Ni of 84.5 to 15 to 0.5 by wet grinding to prepare slurry, and the slurry is prepared into spherical composite powder by utilizing spray drying equipment, wherein the sphericity ratio is 95.0%; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process comprises the steps of heating the spherical composite powder to 400 ℃ at room temperature at the heating rate of 3 ℃/min, keeping the temperature for 2h, heating the spherical composite powder to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 2h to obtain the spherical composite powder with the particle size of 30 mu m; mixing the spherical W/Cu/activated sintering element composite powder and a binder at 150 ℃ for 2h, wherein the volume ratio of the powder to the wax-based binder is 58:42, and preparing an injection molding feed; preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed; and degreasing the injection molding blank, and sintering the degreased injection molding blank at 1180 ℃ for 2.5 hours in a hydrogen atmosphere at a high temperature to obtain the tungsten-copper heat sink component for the optical module.
Prepared tungsten-copper heat sink component for optical module has heat conductivity of 205 W.m-1·K-1Coefficient of thermal expansion of 7.0X 10-6The 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 by the following steps:
tungsten powder with the particle size of 0.25 mu m, copper nitrate and cobalt nitrate are used as raw materials, the raw materials are uniformly mixed according to the mass ratio of W to Cu to Co of 89.8 to 10 to 0.2 by wet grinding to prepare slurry, and then spray drying equipment is utilized to prepare the slurry into spherical composite powder; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process comprises the steps of heating the spherical composite powder to 400 ℃ at room temperature at the heating rate of 4 ℃/min, keeping the temperature for 2h, heating the spherical composite powder to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 2h to obtain the spherical composite powder with the particle size of 20 mu m, wherein the sphericity is 97.5%; mixing the spherical W/Cu/activated sintering element composite powder and a binder at 160 ℃ for 2h, wherein the volume ratio of the powder to the binder is 48:52, and preparing an injection molding feed; preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed; and degreasing the injection molding blank, and sintering the degreased injection molding blank for 3h in a hydrogen atmosphere at a high temperature of 1200 ℃ to obtain the tungsten-copper heat sink component for the optical module.
Thermal conductivity of prepared tungsten-copper heat sink component for optical module is 201 W.m-1·K-1Coefficient of thermal expansion of 5.2X 10-6The 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 by the following steps:
tungsten powder with the particle size of 0.25 mu m, copper nitrate and cobalt nitrate are used as raw materials, the raw materials are uniformly mixed according to the mass ratio of W to Cu to Co of 79.75 to 20 to 0.25 by wet grinding to prepare slurry, and the slurry is prepared into spherical composite powder by utilizing spray drying equipment, wherein the spherical rate is 98.0%; then calcining and reducing the spherical composite powder in hydrogen to obtain spherical W/Cu/activated sintering element composite powder, wherein the calcining process comprises the steps of heating the spherical composite powder to 400 ℃ at room temperature at the heating rate of 5 ℃/min, keeping the temperature for 2h, heating the spherical composite powder to 800 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for 2h to obtain spherical composite powder with the particle size of 20 mu m; mixing the 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 an injection molding feed; preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed; degreasing the injection molding blank, and sintering the degreased injection molding blank for 3h at 1125 ℃ in a hydrogen atmosphere at a high temperature to obtain the tungsten-copper heat sink component for the optical module.
The thermal conductivity of the prepared tungsten-copper heat sink component for the optical module is 225 W.m-1·K-1Coefficient of thermal expansion of 7.5X 10-6The 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 achieve full densification only after being sintered at 1150 ℃; in contrast, as shown in fig. 2, the microstructure of the mixed powder of micrometer W (5 μm)/Cu (5 μm) in the prior art after liquid phase sintering at 1350 ℃ shows that a large number of pores still exist in the sintered W-Cu composite material, which greatly reduces the thermal conductivity of the W-Cu composite material.
Through the mode, the preparation method of the tungsten-copper heat sink component for the optical module is used for preparing the spherical composite powder based on wet grinding and spray drying granulation, the copper phase and the activated sintering element are distributed in gaps of tungsten particles with nanometer sizes, and the sintering process not only has copper phase filling and tungsten particle rearrangement caused by a copper liquid phase, but also has solid-phase sintering of the 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 raw material utilization rate is high, the size precision of parts is good, the thermal performance of the heat sink component is excellent, and the surface state is excellent.

Claims (9)

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, and is specifically implemented according to the following steps:
step 1, taking 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 wet grinding to prepare slurry, preparing the slurry into spherical composite powder by utilizing 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 the spherical W/Cu/activated sintering element composite powder and a binder at the temperature of 150-170 ℃ for 2-4 hours, wherein the volume ratio of the powder to the binder is 45: 55-65: 35, and preparing an injection molding feed;
step 3, preparing a blank body in the shape of the tungsten-copper heat sink component for the required optical module on injection molding equipment by using the feed;
and 4, degreasing the injection molding blank, and sintering at high temperature to obtain the tungsten-copper heat sink component for the optical module.
2. The method for manufacturing a tungsten-copper heat sink component for an optical module according to claim 1, wherein the activated sintering element in step 1 is at least one of soluble Ni, Fe, Co, Pd metal salts.
3. The method for manufacturing a tungsten-copper heat sink member for an optical module according to claim 1, wherein the tungsten powder has a particle size of 0.2 to 1 μm.
4. The method for preparing a tungsten-copper heat sink component for an optical module as claimed in claim 1, wherein the copper source in step 1 is one or more of copper nitrate, copper sulfate and copper chloride.
5. The method for manufacturing a tungsten-copper heat sink component for an optical module according to claim 1, wherein the spherical composite powder in step 1 has a particle size of 15 to 50 μm and a sphericity of > 95%.
6. The method for preparing the tungsten-copper heat sink component for the optical module according to claim 1, wherein the calcining process for calcining the spherical composite powder in hydrogen in the step 1 is heating to 400 ℃, the heating rate is 1-5 ℃/min, and after 2 hours of heat preservation, heating to 800 ℃ at 5 ℃/min and preserving heat for 2 hours.
7. The method for manufacturing a tungsten-copper heat sink member for an optical module as claimed in claim 1, wherein the adhesive in step 2 is a wax-based adhesive.
8. The method for preparing the tungsten-copper heat sink component for the optical module according to claim 1, wherein the high-temperature sintering process in step 4 is as follows: sintering for 1-4 h in 1100-1250 ℃ hydrogen atmosphere.
9. The method for manufacturing a W-Cu heat sink member for an optical module as claimed in claim 1, wherein the W-Cu heat sink member for an optical module has a thermal conductivity of 200W-m or more-1·K-1Coefficient of thermal expansion less than or equal to 8.0 x 10-6and/K, the relative density is more than or equal to 98 percent.
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