CN113070482A - Preparation method of oxide dispersion-strengthened copper-based composite material - Google Patents
Preparation method of oxide dispersion-strengthened copper-based composite material Download PDFInfo
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- CN113070482A CN113070482A CN202110302112.2A CN202110302112A CN113070482A CN 113070482 A CN113070482 A CN 113070482A CN 202110302112 A CN202110302112 A CN 202110302112A CN 113070482 A CN113070482 A CN 113070482A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
- B22F3/15—Hot isostatic pressing
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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Abstract
The preparation method of the oxide dispersion strengthened copper-based composite material comprises the following steps: (1) adding soluble salt and copper salt corresponding to the dispersion-strengthened oxide into deionized water to prepare a uniformly mixed salt solution, and adjusting the pH value to prepare a precursor colloidal solution; (2) spray drying the precursor colloidal solution to prepare composite oxide powder; (3) and carrying out vacuum calcination and reduction treatment on the composite oxide powder to obtain dispersion-strengthened copper-based composite powder. In the preparation method, spray drying is used for regulating and controlling the content and the variety of the reinforcement, so that the final mechanical property of the composite material is favorably regulated and controlled. The density and the air tightness of the composite material can be improved by adopting the spray drying and hot isostatic pressing sintering processes, and the application field of the dispersion-strengthened copper-based composite material is further improved.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a preparation method of an oxide dispersion strengthened copper-based composite material.
Background
The dispersion strengthened copper is an excellent high-strength and high-conductivity material, and is one of the most promising composite materials in high-strength and high-conductivity composite materials. Because of the dispersion strengthening effect of the nano-scale particle reinforcement on the copper matrix, the copper matrix has the characteristics of high strength, high hardness, high conductivity, high softening temperature and the like. At present, dispersion strengthened copper is widely applied to the fields of electrical appliance change-over switches, contact materials, resistance welding electrodes, large-scale integrated circuit lead frames, filament leads, high-power microwave tube structure materials, rotor materials and the like.
At present, the most common commercial dispersion strengthened copper materials at home and abroad are aluminum oxide dispersion strengthened copper-based composite materials, and the processes mainly adopted at present are an internal oxygen method and a mechanical alloying method. The internal oxygen process has long production period, high cost, difficult control of alumina grain size, difficult control of oxygen amount and oxidation time, and strict production equipment and technological control requirement. The other difficulty is that the reinforcing body particles and the copper matrix have poor wettability, so that the reinforcing body particles have segregation and aggregation in the copper matrix, and the segregated reinforcing body is difficult to eliminate when existing in the copper-based composite material, so that cracks and cavities are easily caused, and the mechanical properties of the composite material are adversely affected. The mechanical alloying method has the disadvantages of insufficient grain size of the strengthening phase, wide grain size distribution, easy impurity mixing, difficult uniform mixing and the like, which influence the performance of the alloy. Therefore, in order to improve the application range of the dispersion-strengthened copper, the key point is to find a preparation process capable of improving the dispersibility and content of the reinforcement in the copper matrix so as to improve the mechanical property of the composite material.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background technology and provide a preparation method of an oxide dispersion strengthened copper-based composite material.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of an oxide dispersion strengthened copper-based composite material comprises the following steps:
(1) adding soluble salt and copper salt corresponding to the dispersion-strengthened oxide into deionized water to prepare a uniformly mixed salt solution, and adjusting the pH value to prepare a precursor colloidal solution;
(2) spray drying the precursor colloidal solution to prepare composite oxide powder;
(3) and carrying out vacuum calcination and reduction treatment on the composite oxide powder to obtain dispersion-strengthened copper-based composite powder.
In the above preparation method, preferably, in the step (1), the concentration ratio of the soluble salt to the copper salt corresponding to the dispersion strengthened oxide is (0.1-2 wt%): (99.9-98 wt%).
Preferably, in the step (1), the soluble salt and the copper salt corresponding to the dispersion-strengthened oxide are added into the deionized water to be stirred at a high speed, the stirring time is 10-60min, the temperature is 60 ℃, and the high-speed stirring speed is 1000-4000 r/min.
Preferably, in the preparation method, in the step (1), the soluble salt corresponding to the dispersion-strengthened oxide comprises one or more of aluminum nitrate, yttrium trichloride, zirconium chloride, magnesium nitrate and stannous chloride;
the copper salt comprises one or more of copper sulfate, copper acetate and copper chloride.
In the above production method, preferably, in the step (1), the pH is adjusted by adding potassium hydroxide, and the pH is controlled to 11 to 13.
In the preparation method, preferably, in the step (2), the speed of spray drying is 10000-.
In the preparation method, preferably, in the step (3), the vacuum calcination temperature is 500-800 ℃, and the vacuum calcination time is 1-3 h.
In the preparation method, preferably, in the step (3), the temperature of the reduction treatment is 400-.
According to the preparation method, preferably, the dispersion-strengthened copper-based composite powder is subjected to hot isostatic pressing sintering and hot extrusion to obtain a finished product of the columnar dispersion-strengthened copper-based composite material.
In the preparation method, preferably, the hot isostatic pressing sintering temperature is 700-950 ℃, the pressure is 50-150MPa, and the sintering time is 1-3 h; the hot extrusion temperature is 600-800 ℃.
Compared with the prior art, the invention has the advantages that:
(1) in the preparation method, spray drying is used for regulating and controlling the content and the variety of the reinforcement, so that the final mechanical property of the composite material can be regulated and controlled.
(2) The preparation method provided by the invention has the advantages that the density and the air tightness of the composite material can be improved by adopting spray drying and hot isostatic pressing sintering processes, and the application field of the dispersion-strengthened copper-based composite material is further improved.
(3) The invention can improve the dispersibility and the particle size of the dispersion reinforcement to a certain extent by a spray drying mode, and obtain the nano-grade composite powder.
(4) The preparation method has the advantages of simple preparation process, safety, reliability, simple equipment and easy realization of continuous preparation.
(5) The novel dispersion-strengthened copper-based composite material with the characteristics of uniform structure and excellent performance is prepared by combining the dispersion-strengthened copper-based composite powder prepared by the invention with a spray drying method and hot isostatic pressing sintering, and has important significance for improving the development potential and the application prospect of the novel dispersion-strengthened copper-based composite material.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the preparation method of the oxide dispersion strengthened copper-based composite material comprises the following steps:
(1) preparation of precursor colloidal solution
Aluminum nitrate and copper acetate were mixed in a ratio of 0.1 wt%: adding 99.9 wt.% of deionized water, adding potassium hydroxide to adjust the pH value to 11, and stirring at a high speed to form a precursor colloidal solution, wherein the high-speed stirring speed is 2000r/min, the stirring time is 10min, and the stirring temperature is 60 ℃;
(2) spray drying to prepare composite oxide powder
Preparing the prepared precursor colloidal solution into composite oxide powder by a spray dryer (the speed is 10000r/min, and the spray drying temperature is 200 ℃);
(3) preparation of dispersion-strengthened copper-based composite powder
Calcining the composite oxide powder prepared in the step (2) in a vacuum state at the calcining temperature of 500 ℃ for 2h, and then reducing the composite oxide powder in a hydrogen atmosphere at the reducing temperature of 400 ℃ for 1.5h to obtain dispersion-strengthened copper-based composite powder;
(4) preparation of dispersion-strengthened copper-based composite material
The prepared dispersion-strengthened copper-based composite powder is subjected to hot isostatic pressing sintering (the sintering temperature is 700 ℃, the pressure is 80MPa, and the sintering time is 1h), then sheath hot extrusion (the temperature is 600 ℃) is carried out, and the columnar dispersion-strengthened copper-based composite material is obtained, wherein the mechanical properties of the columnar dispersion-strengthened copper-based composite material are shown in Table 1.
Example 2:
the preparation method of the oxide dispersion strengthened copper-based composite material comprises the following steps:
(1) preparation of precursor colloidal solution
Adding aluminum nitrate and zirconium chloride (in a mass ratio of 1:1) into deionized water according to a concentration of 1 wt% and a concentration of 99 wt.% of copper sulfate, adding potassium hydroxide to adjust the pH value to 12, and stirring at a high speed to form a precursor colloidal solution, wherein the high-speed stirring speed is 6000r/min, the stirring time is 60min, and the stirring temperature is 60 ℃;
(2) spray drying to prepare composite oxide powder
Preparing the prepared precursor colloidal solution into composite oxide powder by a spray dryer (the speed is 20000r/min, and the temperature of spray drying is 300 ℃);
(3) preparation of dispersion-strengthened copper-based composite powder
Calcining the composite oxide powder prepared in the step (2) in a vacuum state at the calcining temperature of 600 ℃ for 2h, and then reducing the composite oxide powder in a hydrogen atmosphere at the reducing temperature of 600 ℃ for 2h to obtain dispersion-strengthened copper-based composite powder;
(4) preparation of dispersion-strengthened copper-based composite material
The prepared dispersion-strengthened copper-based composite powder is subjected to hot isostatic pressing sintering (the sintering temperature is 850 ℃, the pressure is 100MPa, and the sintering time is 2h), then sheath hot extrusion (the temperature is 700 ℃) is carried out, and the columnar dispersion-strengthened copper-based composite material is obtained, wherein the mechanical properties of the columnar dispersion-strengthened copper-based composite material are shown in Table 1.
Example 3:
the preparation method of the oxide dispersion strengthened copper-based composite material comprises the following steps:
(1) preparation of precursor colloidal solution
Adding aluminum nitrate, yttrium chloride and zirconium chloride (mass ratio is 1:1:1) into deionized water according to the concentration of 1.5 wt% and copper acetate salt according to the concentration of 98.5 wt%, adding potassium hydroxide to adjust the pH value to 13, and stirring at a high speed to form a precursor colloidal solution, wherein the high-speed stirring speed is 3000r/min, the stirring time is 40min, and the stirring temperature is 60 ℃;
(2) spray drying to prepare composite oxide powder
Preparing the prepared precursor colloidal solution into composite oxide powder by a spray dryer (the speed is 30000r/min, the temperature of spray drying is 350 ℃);
(3) preparation of dispersion-strengthened copper-based composite powder
Calcining the composite oxide powder prepared in the step (2) in a vacuum state at 800 ℃ for 2h, and then reducing the composite oxide powder in a hydrogen atmosphere at 700 ℃ for 2h to obtain dispersion-strengthened copper-based composite powder;
(4) preparation of dispersion-strengthened copper-based composite material
The prepared dispersion-strengthened copper-based composite powder is subjected to hot isostatic pressing sintering (sintering temperature is 950 ℃, pressure is 150MPa, sintering time is 3h), then sheath hot extrusion (temperature is 800 ℃) is carried out, and the columnar dispersion-strengthened copper-based composite material is obtained, wherein the mechanical properties of the columnar dispersion-strengthened copper-based composite material are shown in Table 1.
TABLE 1 mechanical Properties of the samples of the examples (GB/T228.1-2010)
Claims (10)
1. The preparation method of the oxide dispersion strengthening copper-based composite material is characterized by comprising the following steps of:
(1) adding soluble salt and copper salt corresponding to the dispersion-strengthened oxide into deionized water to prepare a uniformly mixed salt solution, and adjusting the pH value to prepare a precursor colloidal solution;
(2) spray drying the precursor colloidal solution to prepare composite oxide powder;
(3) and carrying out vacuum calcination and reduction treatment on the composite oxide powder to obtain dispersion-strengthened copper-based composite powder.
2. The method of claim 1, wherein in the step (1), the dispersion-strengthened oxide has a concentration ratio of soluble salt to copper salt of (0.1-2 wt%): 99.9-98 wt%).
3. The method according to claim 1, wherein in step (1), the soluble salt and the copper salt corresponding to the dispersion-strengthened oxide are added into the deionized water and stirred at a high speed, wherein the stirring time is 10-60min, the temperature is 60 ℃, and the speed of high-speed stirring is 1000-4000 r/min.
4. The method according to claim 1, wherein in step (1), the soluble salt corresponding to the dispersion-strengthened oxide comprises one or more of aluminum nitrate, yttrium trichloride, zirconium chloride, magnesium nitrate and stannous chloride;
the copper salt comprises one or more of copper sulfate, copper acetate and copper chloride.
5. The method according to claim 1, wherein in the step (1), the pH is adjusted by adding potassium hydroxide, and the pH is controlled to 11 to 13.
6. The method as claimed in claim 1, wherein the spray drying speed in step (2) is 10000-30000r/min, and the spray drying temperature is 150-350 ℃.
7. The method according to any one of claims 1 to 6, wherein in the step (3), the vacuum calcination temperature is 500-800 ℃, and the vacuum calcination time is 1-3 h.
8. The method according to any one of claims 1 to 6, wherein in the step (3), the temperature of the reduction treatment is 400-800 ℃, the reduction time is 1-3h, and the reduction treatment is carried out in hydrogen.
9. The production method according to any one of claims 1 to 6, wherein the dispersion-strengthened copper-based composite powder is subjected to hot isostatic pressing sintering and hot extrusion to obtain a finished product of a columnar dispersion-strengthened copper-based composite material.
10. The preparation method according to claim 9, wherein the hot isostatic pressing sintering temperature is 700-950 ℃, the pressure is 50-150MPa, and the sintering time is 1-3 h; the hot extrusion temperature is 600-800 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114574728A (en) * | 2022-03-10 | 2022-06-03 | 合肥工业大学 | Cu-Y with excellent comprehensive performance3Zr4O12Method for preparing composite material |
| CN115747553A (en) * | 2022-11-10 | 2023-03-07 | 合肥工业大学 | Method for preparing Cu-based composite material by using deionized water as process control agent and oxidant |
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2021
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114574728A (en) * | 2022-03-10 | 2022-06-03 | 合肥工业大学 | Cu-Y with excellent comprehensive performance3Zr4O12Method for preparing composite material |
| CN115747553A (en) * | 2022-11-10 | 2023-03-07 | 合肥工业大学 | Method for preparing Cu-based composite material by using deionized water as process control agent and oxidant |
| CN115747553B (en) * | 2022-11-10 | 2023-12-01 | 合肥工业大学 | Method for preparing Cu-based composite material by using deionized water as process control agent and oxidant |
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