CN111996408B - Preparation method of oxide ceramic particle reinforced Cu-based composite material - Google Patents

Preparation method of oxide ceramic particle reinforced Cu-based composite material Download PDF

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CN111996408B
CN111996408B CN202010873930.3A CN202010873930A CN111996408B CN 111996408 B CN111996408 B CN 111996408B CN 202010873930 A CN202010873930 A CN 202010873930A CN 111996408 B CN111996408 B CN 111996408B
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powder
composite material
temperature
copper
ceramic particle
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CN111996408A (en
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李秀青
魏世忠
杨晴霞
徐流杰
周玉成
张敏杰
张国赏
毛丰
陈冲
张程
熊美
潘昆明
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Henan University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper

Abstract

The invention relates to an oxide ceramic particle reinforced Cu-based composite material and a preparation method thereof. The present invention belongs to the field of composite material, and is characterized by that it uses aluminium nitrate (or zirconium nitrate), copper nitrate and ammonium metatungstate as raw material, and respectively prepares them into solutions with a certain concentration, and uniformly mixes them, adopts cyclone spray-drying process to prepare composite powder precursor, and makes them pass through roasting so as to obtain Al2O3‑WO3-CuO mixed powder; then adding Al2O3‑WO3Al is obtained after-CuO is reduced by high-purity hydrogen2O3Doping copper-tungsten composite powder, and preparing Al by directly carrying out vacuum hot-pressing sintering on the composite powder2O3Ceramic particle reinforced Cu-based composite material, in which ZrO may also be used2‑WO3-CuO mixed powder to obtain ZrO2Its effect is in accordance with Al2O3The effect is the same. The invention has simple process and the prepared Al2O3The ceramic particle reinforced Cu-based composite material has uniform components, fine and uniform crystal grains, extremely low impurity content and good comprehensive performance index, can be used for the harsh working conditions of electricity, high temperature, abrasion and corrosion interaction, is suitable for large-scale industrial production, and has wide industrial application prospect.

Description

Preparation method of oxide ceramic particle reinforced Cu-based composite material
Technical Field
The invention belongs to the field of metal and composite materials thereof, and particularly relates to a preparation method of an oxide ceramic particle reinforced Cu-based composite material.
Background
The metal copper (Cu) is one of the earliest metals used by human beings, has the outstanding characteristics of high thermal conductivity and electrical conductivity, good ductility, good corrosion resistance, excellent forming processability and the like, and is widely applied to the fields of cables, electric and electronic components, military armor-breaking weapons, electromagnetic gun rails and the like. However, with the development of science and technology, the application range of the metal copper is wider and wider, and the application requirement of the metal copper is higher and higher correspondingly. In the background of the difficulty of meeting the growing demands of humans with copper as a single metal, a wide variety of copper alloys or copper-based composites have come into force. In actual working conditions, various factors interact with each other, the requirement on the service performance of the material is very high, for example, the harsh working conditions of electricity receiving, abrasion, corrosion and nuclear radiation interaction, the material is required to have good comprehensive performance, such as good conductivity, high strength, high hardness, abrasion resistance, corrosion resistance and the like, the integration of the structure and the function is realized, and the existing material is difficult to meet the requirement.
The copper-tungsten alloy has the characteristics of high melting point, high density and high strength of metal tungsten, high electric conduction and heat conduction of metal copper, excellent arc ablation resistance and the like, so that the copper-tungsten alloy is widely applied to the engineering fields of military industry, electronics, aerospace, machinery and the like. However, most of the current researches and applications are high-tungsten type copper-tungsten alloys (the W content is more than 50%), and few researches are carried out on the high-copper type copper-tungsten alloys (the Cu content is more than 50%). The development of science and technology is changing day by day, and the application demand of the high-copper type copper-tungsten alloy is more and more strong. In recent years, ceramic particles, especially oxide ceramic particle reinforced copper-tungsten composite materials, have been one of the hot researches due to a series of excellent properties.
Due to the large performance difference between Cu and W elements, the phenomenon of mutual insolubility or weak solubility exists in the sintering process of two powder metallurgy methods, so that the sintering performance of the alloy is poor, such as large crystal grains, low density and the like, and the application range of the Cu-W alloy is greatly limited. At present, many researches on Cu-W alloy with high tungsten content are carried out at home and abroad, and the preparation method mainly comprises an infiltration method and a high-temperature liquid phase sintering method. However, both of these methods are difficult to implement in the production of Cu — W alloys with high copper content. The reason is that firstly, it is difficult to form a W skeleton because of a small W content, and secondly, the liquid phase sample collapses once formed because of a high Cu content. Therefore, a new preparation process needs to be explored for preparing the high-performance oxide ceramic particle reinforced copper-tungsten composite material.
Disclosure of Invention
In view of the problems in the prior art, the invention discloses an oxide ceramic particle reinforced Cu-based composite material and a preparation method thereof, and adopts the technical scheme that the preparation method comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and aluminum nitrate powder with the purity of more than 99.99% as raw materials, and mixing the raw materials according to the weight ratio of Cu: w: al (Al)2O3The weight ratio is controlled to be (77-94.95): (5-20): (0.05-3) calculating required copper nitrate powder, ammonium metatungstate powder and aluminum nitrate powder, and weighing by using a high-precision balance for later use;
step two, slowly adding the aluminum nitrate powder, the copper nitrate powder and the ammonium metatungstate powder weighed in the step one into 3 beakers added with deionized water in advance, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer at the same time, selecting a material of a stirring rod as polytetrafluoroethylene, and slowly stirring to prepare an ammonium metatungstate solution A, an aluminum nitrate solution B and a copper nitrate solution C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the aluminum nitrate solution B prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring to obtain a mixed solution;
step four, starting up the cyclone type spray dryer and electrifying, inserting a peristaltic pump tube into the mixed solution prepared in the step three, starting to perform spray drying operation, and unloading a material collector to take materials after spraying is finished to obtain a composite powder precursor;
step five, roasting the precursor powder obtained in the step four in a high-temperature muffle furnace to obtain Al2O3-WO3-CuO mixed powder;
step six, mixing Al obtained in the step five2O3-WO3The first reduction of-CuO mixed powder is carried out in a high-purity hydrogen atmosphere,
then, the control parameters are changed to carry out secondary reduction to obtain Al2O3Doping copper-tungsten composite powder;
step seven, Al obtained in the step six2O3Filling the copper-doped tungsten composite powder into a die for manufacturing heat-resistant steel, performing vacuum hot-pressing sintering, and cooling to 260 ℃ along with a furnace after sintering;
step eight, taking out the sample cooled to 260 ℃, and rapidly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.5 to 1 hour to finally obtain Al2O3The oxide ceramic particles reinforce the Cu-based composite material.
The invention discloses an oxide ceramic particle reinforced Cu-based composite material and a preparation method thereof, and adopts another technical scheme that the preparation method comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and zirconium nitrate powder with the purity of more than 99.99% as raw materials, and mixing the raw materials according to the weight ratio of Cu: w: ZrO (ZrO)2The weight ratio is controlled to be (77-94.95): (5-20): (0.05-3) calculating required copper nitrate powder, ammonium metatungstate powder and zirconium nitrate powder, and weighing by using a high-precision balance for later use;
secondly, slowly adding the zirconium nitrate powder, the copper nitrate powder and the ammonium metatungstate powder weighed in the first step into 3 beakers which are added with deionized water in advance, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer at the same time, selecting a stirring rod made of polytetrafluoroethylene, and slowly stirring to prepare an ammonium metatungstate solution A, a zirconium nitrate solution D and a copper nitrate solution C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the zirconium nitrate solution D prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring to obtain a mixed solution;
step four, starting up the cyclone type spray dryer and electrifying, inserting a peristaltic pump tube into the mixed solution prepared in the step three, starting to perform spray drying operation, and unloading a material collector to take materials after spraying is finished to obtain a composite powder precursor;
step five, roasting the precursor powder obtained in the step four in a high-temperature muffle furnace to obtain ZrO2-WO3-CuO mixed powder;
step six, ZrO obtained in the step five2-WO3Carrying out first reduction on-CuO mixed powder in a high-purity hydrogen atmosphere, and then changing control parameters to carry out second reduction to obtain ZrO2Doping copper-tungsten composite powder;
step seven, ZrO obtained in the step six2Filling the copper-doped tungsten composite powder into a die for manufacturing heat-resistant steel, performing vacuum hot-pressing sintering, and cooling to 260 ℃ along with a furnace after sintering;
step eight, taking out the sample cooled to 260 ℃, and rapidly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.5 to 1 hour to finally obtain ZrO2The oxide ceramic particles reinforce the Cu-based composite material.
As a preferable scheme of the invention, the concentration of 3 beakers in the step two is controlled to be 1-1.5 mol/L, and the stirring speed is 30-50 r/min.
As a preferable scheme of the invention, the electric stirring time in the step three is 10-20 min.
As a preferred embodiment of the present invention, the operating parameters of the cyclone spray dryer in the fourth pair of steps are as follows: the temperature is 270-280 ℃, the fan is 60-65%, the needle passing speed is 5 s/time, the creep rate is 40-50%, and the outlet temperature is controlled to be 105-110 ℃.
According to a preferable scheme of the invention, the temperature for roasting in the high-temperature muffle furnace in the step five is 500-515 ℃, and the time is 2.1-2.5 h.
As a preferable embodiment of the present invention, the reduction control parameters in the sixth first hydrogen atmosphere are: the hydrogen flow is 2-3L/h, the temperature is 350-450 ℃, and the time is 1.5-2.5 h; the reduction control parameters in the second hydrogen atmosphere were: the hydrogen flow is 2-3L/h, the temperature is 710-800 ℃, and the time is 1.5-2.5 h.
As a preferred scheme of the invention, the parameters are controlled as follows when the furnace is cooled after the sintering in the step seven is finished: the sintering temperature is 800-850 ℃, the heat preservation time is 1-1.5 h, the axial pressure is 35-45 MPa, the vacuum degree is 10 < -3 > to 10 < -6 > Pa, and the heating rate is 50-60 ℃/min.
The invention has the beneficial effects that: the invention has simple process and the prepared Al2O3(or ZrO)2) The ceramic particle reinforced Cu-based composite material has good comprehensive performance indexes (the grain size is as low as 20nm, the impurity content is as low as below 10ppm, the highest conductivity is 85.1 percent IACS, the highest density is 99.99 percent, the highest tensile strength is 560MPa, and the highest hardness is 76.1HBW), and can be used for harsh working conditions of electricity, high temperature, abrasion and corrosion interaction.
Detailed Description
Example 1
The invention relates to a preparation method of an oxide ceramic particle reinforced Cu-based composite material, which adopts the technical scheme that the preparation method specifically comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder with the purity of more than 99.99% as raw materials, wherein the weight ratio of Cu: w: the weight ratio of Al2O3 (or ZrO2) is controlled to be 77: 5: 0.05, calculating required copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder, and weighing by using a high-precision balance for later use;
step two, slowly adding the aluminum nitrate (or zirconium nitrate), copper nitrate and ammonium metatungstate powder weighed in the step one into 3 beakers which are added with deionized water in advance, controlling the concentration to be 1mol/L, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer, stirring the materials of a stirring rod which is polytetrafluoroethylene at a slow speed, and stirring at a speed of 30r/min to prepare solutions A, B (D) and C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the aluminum nitrate solution B (or the zirconium nitrate solution D) prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring for 10min to obtain a mixed solution;
step four, starting up and electrifying the cyclone type spray dryer, and setting parameters as follows: the temperature is 270 ℃, the fan is 60%, the needle passing speed is 5 s/time, the creep rate is 40%, and the outlet temperature is controlled at 105 ℃. And (4) inserting a peristaltic pump tube into the mixed solution prepared in the third step, and starting the spray drying operation. After spraying, unloading the material collector to take materials to obtain a composite powder precursor;
fifthly, roasting the precursor powder obtained in the fourth step in a high-temperature muffle furnace at 500 ℃ for 2.1h to obtain Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder;
and step six, reducing the Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder obtained in the step five in a high-purity hydrogen atmosphere: the hydrogen flow is 2L/h, the temperature is 350 ℃, and the time is 1.5 h; then, converting the control parameters to perform second reduction: hydrogen flow rate is 2L/h, temperature is 710 ℃, and time is 1.5h, so that Al2O3 (or ZrO2) doped copper-tungsten composite powder is obtained;
step seven, directly filling the Al2O3 (or ZrO2) doped copper-tungsten composite powder obtained in the step six into a die made of heat-resistant steel without cold press molding, carrying out vacuum hot-pressing sintering, cooling to 260 ℃ along with a furnace after sintering, and controlling the following parameters: the sintering temperature is 800 ℃, the heat preservation time is 1h, the axial pressure is 35MPa, the vacuum degree is 10-3Pa, and the heating rate is 50 ℃/min;
and step eight, taking out the sample cooled to 260 ℃, and quickly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.5h to finally obtain the Al2O3 (or ZrO2) oxide ceramic particle reinforced Cu-based composite material.
Example 2
The invention relates to a preparation method of an oxide ceramic particle reinforced Cu-based composite material, which adopts the technical scheme that the preparation method specifically comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder with the purity of more than 99.99% as raw materials, wherein the weight ratio of Cu: w: the weight ratio of Al2O3 (or ZrO2) is controlled to be 94.95: 20: 3 calculating required copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder, and weighing by using a high-precision balance for later use;
step two, slowly adding the aluminum nitrate (or zirconium nitrate), copper nitrate and ammonium metatungstate powder weighed in the step one into 3 beakers which are added with deionized water in advance, controlling the concentration to be 1.5mol/L, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer, stirring the materials of a stirring rod which is polytetrafluoroethylene at a slow speed, and stirring at a speed of 50r/min to prepare a solution A, B, C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the aluminum nitrate solution B (or the zirconium nitrate solution D) prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring for 20min to obtain a mixed solution;
step four, starting up and electrifying the cyclone type spray dryer, and setting parameters as follows: the temperature is 280 ℃, the fan is 65%, the needle passing speed is 5 s/time, the creep rate is 50%, and the outlet temperature is controlled at 110 ℃. And (4) inserting a peristaltic pump tube into the mixed solution prepared in the third step, and starting the spray drying operation. After spraying, unloading the material collector to take materials to obtain a composite powder precursor;
fifthly, roasting the precursor powder obtained in the fourth step in a high-temperature muffle furnace at 515 ℃ for 2.5 hours to obtain Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder;
and step six, reducing the Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder obtained in the step five in a high-purity hydrogen atmosphere: the hydrogen flow is 3L/h, the temperature is 450 ℃, and the time is 2.5 h; then, converting the control parameters to perform second reduction: hydrogen flow rate is 3L/h, temperature is 800 ℃, time is 2.5h, and Al2O3 (or ZrO2) doped copper-tungsten composite powder is obtained;
step seven, directly filling the Al2O3 (or ZrO2) doped copper-tungsten composite powder obtained in the step six into a die made of heat-resistant steel without cold press molding, carrying out vacuum hot-pressing sintering, cooling to 260 ℃ along with a furnace after sintering, and controlling the following parameters: the sintering temperature is 850 ℃, the heat preservation time is 1.5h, the axial pressure is 45MPa, the vacuum degree is 10-6Pa, and the heating rate is 60 ℃/min;
and step eight, taking out the sample cooled to 260 ℃, and rapidly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 1h to finally obtain the Al2O3 (or ZrO2) oxide ceramic particle reinforced Cu-based composite material.
Example 3
The invention relates to a preparation method of an oxide ceramic particle reinforced Cu-based composite material, which adopts the technical scheme that the preparation method specifically comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder with the purity of more than 99.99% as raw materials, wherein the weight ratio of Cu: w: the weight ratio of Al2O3 (or ZrO2) is controlled to be 85: 15: 1.5 calculating required copper nitrate powder, ammonium metatungstate powder and aluminum nitrate (or zirconium nitrate) powder, and weighing by using a high-precision balance for later use;
step two, slowly adding the aluminum nitrate (or zirconium nitrate), copper nitrate and ammonium metatungstate powder weighed in the step one into 3 beakers which are added with deionized water in advance, controlling the concentration to be 1.25mol/L, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer (the material of a stirring rod is polytetrafluoroethylene) for slow stirring at the stirring speed of 40r/min, and preparing a solution A, B, C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the aluminum nitrate solution B prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring for 15min to obtain a mixed solution;
step four, starting up and electrifying the cyclone type spray dryer, and setting parameters as follows: the temperature is 275 ℃, the fan is 62%, the needle passing speed is 5 s/time, the peristalsis rate is 45%, and the outlet temperature is controlled at 108 ℃. And (4) inserting a peristaltic pump tube into the mixed solution prepared in the third step, and starting the spray drying operation. After spraying, unloading the material collector to take materials to obtain a composite powder precursor;
fifthly, roasting the precursor powder obtained in the fourth step in a high-temperature muffle furnace at 510 ℃ for 2.3 hours to obtain Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder;
and step six, reducing the Al2O3-WO3-CuO or ZrO2-WO3-CuO mixed powder obtained in the step five in a high-purity hydrogen atmosphere: the hydrogen flow is 2.5L/h, the temperature is 400 ℃, and the time is 2 h; then, converting the control parameters to perform second reduction: hydrogen flow rate is 2.5L/h, temperature is 760 ℃, and time is 2h, so that Al2O3 (or ZrO2) doped copper-tungsten composite powder is obtained;
step seven, directly filling the Al2O3 (or ZrO2) doped copper-tungsten composite powder obtained in the step six into a die made of heat-resistant steel without cold press molding, carrying out vacuum hot-pressing sintering, cooling to 260 ℃ along with a furnace after sintering, and controlling the following parameters: the sintering temperature is 825 ℃, the heat preservation time is 1.25h, the axial pressure is 40MPa, the vacuum degree is 10-4Pa, and the heating rate is 55 ℃/min;
and step eight, taking out the sample cooled to 260 ℃, and quickly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.7h to finally obtain the Al2O3 (or ZrO2) oxide ceramic particle reinforced Cu-based composite material.
Components not described in detail herein are prior art.
Although the present invention has been described in detail with reference to the specific embodiments, the present invention is not limited to the above embodiments, and various changes and modifications without inventive changes may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.

Claims (8)

1. A preparation method of an oxide ceramic particle reinforced Cu-based composite material is characterized by comprising the following steps: the method comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and aluminum nitrate powder with the purity of more than 99.99% as raw materials, and mixing the raw materials according to the weight ratio of Cu: w: al (Al)2O3The weight ratio is controlled to be (77-94.95): (5-20): (0.05-3) calculating required copper nitrate powder, ammonium metatungstate powder and aluminum nitrate powder, and weighing by using a high-precision balance for later use;
step two, slowly adding the aluminum nitrate powder, the copper nitrate powder and the ammonium metatungstate powder weighed in the step one into 3 beakers added with deionized water in advance, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer at the same time, selecting a material of a stirring rod as polytetrafluoroethylene, and slowly stirring to prepare an ammonium metatungstate solution A, an aluminum nitrate solution B and a copper nitrate solution C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the aluminum nitrate solution B prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring to obtain a mixed solution;
step four, starting up the cyclone type spray dryer and electrifying, inserting a peristaltic pump tube into the mixed solution prepared in the step three, starting to perform spray drying operation, and unloading a material collector to take materials after spraying is finished to obtain a composite powder precursor;
step five, roasting the precursor powder obtained in the step four in a high-temperature muffle furnace to obtain Al2O3-WO3-CuO mixed powder;
step six, mixing Al obtained in the step five2O3-WO3Carrying out first reduction on-CuO mixed powder in a high-purity hydrogen atmosphere, and then changing control parameters to carry out second reduction to obtain Al2O3Doping copper-tungsten composite powder;
step seven, Al obtained in the step six2O3Filling the copper-doped tungsten composite powder into a die for manufacturing heat-resistant steel, performing vacuum hot-pressing sintering, and cooling to 260 ℃ along with a furnace after sintering;
step eight, taking out the sample cooled to 260 ℃, and rapidly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.5 to 1 hour to finally obtain Al2O3The oxide ceramic particles reinforce the Cu-based composite material.
2. The method for preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 1, wherein: the method comprises the following steps:
selecting copper nitrate powder, ammonium metatungstate powder and zirconium nitrate powder with the purity of more than 99.99% as raw materials, and mixing the raw materials according to the weight ratio of Cu: w: ZrO (ZrO)2The weight ratio is controlled to be (77-94.95): (5-20): (0.05-3) calculating required copper nitrate powder, ammonium metatungstate powder and zirconium nitrate powder, and weighing by using a high-precision balance for later use;
secondly, slowly adding the zirconium nitrate powder, the copper nitrate powder and the ammonium metatungstate powder weighed in the first step into 3 beakers which are added with deionized water in advance, then placing the beakers into an ultrasonic oscillator for ultrasonic oscillation, starting an electric stirrer at the same time, selecting a stirring rod made of polytetrafluoroethylene, and slowly stirring to prepare an ammonium metatungstate solution A, a zirconium nitrate solution D and a copper nitrate solution C for later use;
step three, slowly pouring the ammonium metatungstate solution A and the zirconium nitrate solution D prepared in the step two into the copper nitrate solution C in sequence, and simultaneously performing ultrasonic oscillation and electric stirring to obtain a mixed solution;
step four, starting up the cyclone type spray dryer and electrifying, inserting a peristaltic pump tube into the mixed solution prepared in the step three, starting to perform spray drying operation, and unloading a material collector to take materials after spraying is finished to obtain a composite powder precursor;
step five, roasting the precursor powder obtained in the step four in a high-temperature muffle furnace to obtain ZrO2-WO3-CuO mixed powder;
step six, ZrO obtained in the step five2-WO3Carrying out first reduction on-CuO mixed powder in a high-purity hydrogen atmosphere, and then changing control parameters to carry out second reduction to obtain ZrO2Doping copper-tungsten composite powder;
step seven, ZrO obtained in the step six2Filling the copper-doped tungsten composite powder into a die for manufacturing heat-resistant steel, performing vacuum hot-pressing sintering, and cooling to 260 ℃ along with a furnace after sintering;
step eight, taking out the sample cooled to 260 ℃, and rapidly placing the sample in a low-temperature environment with the temperature of-150 to-160 ℃ for 0.5 to 1 hour to finally obtain ZrO2Oxide ceramic particle reinforcementA Cu-based composite material.
3. The method for producing an oxide ceramic particle-reinforced Cu-based composite material according to claim 1 or claim 2, wherein: and controlling the concentration of 3 beakers in the step two to be 1-1.5 mol/L, and stirring at the speed of 30-50 r/min.
4. The method of preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 3, wherein: and the electric stirring time in the step three is 10-20 min.
5. The method of preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 3, wherein: step four, the operating parameters of the cyclone spray dryer are as follows: the temperature is 270-280 ℃, the fan is 60-65%, the needle passing speed is 5 s/time, the creep rate is 40-50%, and the outlet temperature is controlled to be 105-110 ℃.
6. The method of preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 3, wherein: and fifthly, roasting in a high-temperature muffle furnace at the temperature of 500-515 ℃ for 2.1-2.5 h.
7. The method of preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 3, wherein: the reduction control parameters in the sixth first hydrogen atmosphere are as follows: the hydrogen flow is 2-3L/h, the temperature is 350-450 ℃, and the time is 1.5-2.5 h; the reduction control parameters in the second hydrogen atmosphere were: the hydrogen flow is 2-3L/h, the temperature is 710-800 ℃, and the time is 1.5-2.5 h.
8. The method of preparing an oxide ceramic particle-reinforced Cu-based composite material according to claim 3, wherein: and seventhly, controlling the parameters when the temperature is reduced along with the furnace after the sintering is finished as follows: the sintering temperature is 800-850 ℃, the heat preservation time is 1-1.5 h, the axial pressure is 35-45 MPa, the vacuum degree is 10 < -3 > to 10 < -6 > Pa, and the heating rate is 50-60 ℃/min.
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