CN101984118A - Method for preparing CuAl2O3 composite material through spray co-deposition reaction - Google Patents
Method for preparing CuAl2O3 composite material through spray co-deposition reaction Download PDFInfo
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Abstract
The invention discloses a method for preparing CuAl2O3 composite material through a spray co-deposition reaction, which comprises the following steps: 1, processing of CuO powder; 2, preparation of alloy fusant; 3, preparation of CuAl/CuO alloy by the spray co-deposition; 4, preparation of CuAl2O3 composite material by carrying out in situ chemical reaction on the CuAl/CuO alloy; and 5, extrusion, rolling and drawing. The Al2O3 particle in the invention is synthesized by the in situ chemical reaction, has fresh reaction interface, is firmly matched with Cu, has nano-scale size, and obvious enhanced effect. The method of the invention has the characteristics of simple raw material preparation, excellent performance of the prepared materials, and easily controlled process; and the dispersion distribution of the wide phase of the composite material particle is completed by deformation through the process, and the problem of difficult subsequent process of the particle enhanced metal matrix composite is preferably solved.
Description
Technical field
The invention belongs to the metal-base composites technical field, be specifically related to a kind of spray co deposition prepared in reaction CuAl
2O
3The method of matrix material.
Background technology
CuAl
2O
3Matrix material not only conducts electricity, thermal conductivity is good, also has higher hardness, intensity and softening temperature etc., is widely used in fields such as automobile, electronics, electrician, electromechanics.
Just adopted the powder internal oxidation to produce CuAl in batches the seventies in eighties of last century abroad
2O
3Matrix material, the C15715, the Al of C15760 that produce as SCM Corporation of the U.S.
2O
3Dispersed and strengthened copper-based composite material, its softening temperature are 900 ℃, and specific conductivity is 90%IACS, and tensile strength reaches 540MPa, and have formed the industrial scale of daily output 20t.The company of Japan, Germany and Korea S is at CuAl
2O
3The production aspect of matrix material has had suitable scale, and has worked out corresponding product technology standard.Because this series products still is listed in patented product abroad, production technology is still maintained secrecy.
China is to CuAl
2O
3Composite study is started late, just begin formal project verification the seventies in 20th century, in the nineties at the end of the eighties, units such as University Of Tianjin, Harbin Institute of Technology, Kunming Inst. of Metallurgy, Xi'an University of Technology, Beijing Non-Ferrous Metal Research General Academy, Kunming Institute of Precious Metals are arranged, carried out the research-and-development activity of such material in succession.But, because CuAl
2O
3Reasons such as composite material preparation process complexity, homogeneity of structure is poor, density is not high, production cost height, domestic relevant unit has only set up small-scale pilot production line, always can not large-scale production; Zhi Bei CuAl simultaneously
2O
3Matrix material is also unstable at aspects such as mechanical property and softening temperatures, and the yield rate of processing is low, causes cost of manufacture higher; Therefore, every technical performance index all awaits further improving.At present, most of CuAl of domestic use
2O
3Matrix material still depends on import.
At present, the preparation method of domestic aluminium oxide particle reinforced copper base matrix material mainly contains: powder metallurgic method, composite electrodeposition method, mechanical alloying method, chemical coprecipitation, reaction synthesis method, internal oxidation etc.Though these known preparation methods have obtained CuAl
2O
3Matrix material, but all exist tangible deficiency, mainly show as: the powder metallurgic method preparation technique complexity, the cost height, production efficiency is low; The composite powder that mechanical alloying method is made the poly-partially of wild phase aluminium sesquioxide can occur and grow up in the agglomerating process, influence performance of composites; Chemical coprecipitation and composite electrodeposition method have pollution to environment, and the material property that chemical coprecipitation obtains is low, and the particle of composite electrodeposition method evenly suspends wayward in plating bath; The reaction synthesis method complicated process of preparation will be through mixing powder and multi-steps sintering for a long time; Though the CuAl of internal oxidation preparation
2O
3Composite material combination property is better, but in preparation process, and oxygen partial pressure, oxidization time and amount of oxidation all are difficult to control, causes its complex process, production cycle elongated, and unstable product quality is unfavorable for suitability for industrialized production simultaneously.In addition, the matrix material of these method preparations all can not directly prepare nearly formed parts such as ingot, plate, wheel, and material preparation process technical sophistication, quality product are difficult to control, and production cost is higher, can not form large-scale production etc.Cause CuAl
2O
3The preparation level of matrix material and over-all properties exist big gap with comparing abroad, and the situation that also depends on import is used in mass-producing.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, provides a kind of preparation process easy to control, and starting material are prepared simple, the spray co deposition prepared in reaction CuAl of the excellent material performance of preparation
2O
3The method of matrix material.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of spray co deposition prepared in reaction CuAl
2O
3The method of matrix material is characterized in that, this method may further comprise the steps:
(1) be to handle 0.5h～2h under 100 ℃～300 ℃ the condition with the CuO powder in temperature;
(2) mixture of Cu and Al is placed alloying obtains alloy melt in the spray co deposition vacuum intermediate frequency (IF) smelting stove, the mass percent of Al is 0.1%～4% in the described mixture, and surplus is Cu; Or the mixture of Cu and Al and modifying element placed together alloying obtains alloy melt in the spray co deposition vacuum intermediate frequency (IF) smelting stove, described modifying element is one or more among La, Ce and the Y, and the addition of described modifying element is 0.01%～2% of an alloy melt quality;
(3) treat that the alloy melt temperature reaches 100 ℃～200 ℃ described in the step (2) after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and started in the powder conveying device supplying step (1) CuO powder after treatment, carry out spray co deposition and obtain the CuAl/CuO alloy; The operational throughput of described CuO powder is 3/2 times of molar weight of Al, perhaps is Al and modifying element amount of substance sum 3/2 times;
(4) be in-situ chemical reaction 4h～10h under 800 ℃～1000 ℃ the vacuum condition with CuAl/CuO alloy described in the step (3), prepare CuAl in temperature
2O
3Matrix material;
(5) with CuAl described in the step (4)
2O
3The matrix material extrusion processing becomes the CuAl of bar or sheet material shape
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into sheet material, silk material, profiled material or contact shape according to application requiring
2O
3Matrix material.
The particle diameter of CuO powder described in the above-mentioned steps (1) is 10 μ m～100 μ m.
Quality purity 〉=99.9% of Cu described in the above-mentioned steps (2), the quality purity of described Al 〉=99.9%.
The temperature of alloying described in the above-mentioned steps (2) is 1040 ℃～1100 ℃.
The distance of the deposition of spray co deposition described in the above-mentioned steps (3) is 300mm～400mm, and atomization pressure is 0.8MPa～2.0MPa, and the thrust-augmenting nozzle internal diameter is 3.5mm～4.5mm, and the depositor rotating speed is 10rpm/min～40rpm/min.
The temperature of extruding is 400 ℃～600 ℃ described in the above-mentioned steps (5).
The present invention compared with prior art has the following advantages:
1, the present invention is integrated by advanced machining technologies such as spray co deposition, in-situ chemical reactions, can realize that short flow process, nearly shaping, compelling, equal-freezing prepare CuAl
2O
3Matrix material has the production efficiency height, and tooling cost is low, characteristics such as constant product quality.
2, it is simple that the present invention has the starting material preparation, the characteristics such as excellent material performance of preparation, and preparation process is easy to control, the disperse of composite material granular wild phase distributes finishes by machining deformation, has well solved the problem of particles reiforced metal-base composition following process difficulty.
3, Al of the present invention
2O
3Particle generates in position, and the interface is fresh, and is firm with combining of Cu; And the second phase particle that in-situ chemical reaction generates reaches nano level (particle diameter is less than 100nm), is uniformly distributed on the intracrystalline and crystal boundary of Cu matrix, and strengthening effect is obvious, makes the thermostability of material and heat resistance obviously improve Al
2O
3Disperse distribute and to finish by machining deformation, well solved the problem of matrix material following process difficulty.
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment
Embodiment 1
(1) be that the CuO powder of 10 μ m is to handle 2h under 100 ℃ of conditions in temperature with particle diameter;
(2) mixture with the Al of the Cu of quality purity 〉=99.9% and quality purity 〉=99.9% places in the spray co deposition vacuum intermediate frequency (IF) smelting stove, is that alloying obtains alloy melt under 1040 ℃ of conditions in temperature; The mass percent of Al is 0.1% in the described mixture, and surplus is Cu;
(3) treat that the alloy melt temperature reaches 200 ℃ after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and is started powder conveying device and carry after treatment CuO powder, carry out spray co deposition and obtain the CuAl/CuO alloy; The amount of described CuO powder is 3/2 times of molar weight of Al; The deposition distance of described spray co deposition is 300mm, and atomization pressure is 2.0MPa, and the thrust-augmenting nozzle internal diameter is 3.5mm, and the depositor rotating speed is 10rpm/min;
(4) under vacuum condition, in-situ chemical reaction 4h under 1000 ℃ the condition to the CuAl/CuO alloy in temperature, prepare CuAl
2O
3Matrix material;
(5) with CuAl
2O
3Matrix material is the CuAl that extrusion processing becomes bar or sheet material shape under 400 ℃ of conditions in temperature
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into shapes such as sheet material, silk material, profiled material or contact according to application requiring
2O
3Matrix material.
Embodiment 2
Present embodiment is identical with embodiment 1 preparation method, and wherein difference is: the particle diameter of CuO powder is 100 μ m, and the temperature of CuO powder treatment is 200 ℃, and the treatment time is 0.5h; The mass percent of Al is 2% in the mixture; The alloying temperature is 1070 ℃, treat that the alloy melt temperature reaches 100 ℃ after, open the atomization gas valve; The deposition distance of spray co deposition is 400mm, and atomization pressure is 0.8MPa, and the thrust-augmenting nozzle internal diameter is 4mm, and the depositor rotating speed is 25rpm/min; The temperature of in-situ chemical reaction is 800 ℃, and the time of in-situ chemical reaction is 10h; The temperature of extruding is 600 ℃.
Embodiment 3
Present embodiment is identical with embodiment 1 preparation method, and wherein difference is: the particle diameter of CuO powder is 55 μ m, and the temperature of CuO powder treatment is 300 ℃, and the treatment time is 1.3h; The mass percent of Al is 4% in the mixture; The alloying temperature is 1100 ℃, treat that the alloy melt temperature reaches 150 ℃ after, open the atomization gas valve; The deposition distance of spray co deposition is 350mm, and atomization pressure is 1.4MPa, and the thrust-augmenting nozzle internal diameter is 4.5mm, and the depositor rotating speed is 40rpm/min; The temperature of in-situ chemical reaction is 900 ℃, and the time of in-situ chemical reaction is 7h; The temperature of extruding is 500 ℃.
Embodiment 4
(1) be that the CuO powder of 10 μ m is to handle 2h under 100 ℃ of conditions in temperature with particle diameter;
(2) mixture and the modifying element with the Al of the Cu of quality purity 〉=99.9% and quality purity 〉=99.9% together places in the spray co deposition vacuum intermediate frequency (IF) smelting stove, is that alloying obtains alloy melt under 1100 ℃ of conditions in temperature; The mass percent of Al is 0.1% in the described mixture, and surplus is Cu; Described modifying element is La, and the addition of modifying element is 0.01% of an alloy melt quality;
(3) treat that the alloy melt temperature reaches 200 ℃ after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and is started powder conveying device and carry after treatment CuO powder, carry out spray co deposition and obtain the CuAl/CuO alloy; The operational throughput of described CuO powder is Al and La amount of substance sum 3/2 times; The deposition distance of described spray co deposition is 300mm, and atomization pressure is 2.0MPa, and the thrust-augmenting nozzle internal diameter is 3.5mm, and the depositor rotating speed is 10rpm/min;
(4) under vacuum condition, in-situ chemical reaction 4h under 1000 ℃ the condition to the CuAl/CuO alloy in temperature, prepare CuAl
2O
3Matrix material;
(5) with CuAl
2O
3Matrix material is the CuAl that extrusion processing becomes bar or sheet material shape under 400 ℃ of conditions in temperature
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into shapes such as sheet material, silk material, profiled material or contact according to application requiring
2O
3Matrix material.
Embodiment 5
Present embodiment is identical with embodiment 4 preparation methods, and wherein difference is: described modifying element is Ce or Y, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 2% of an alloy melt quality.
Embodiment 6
Present embodiment is identical with embodiment 4 preparation methods, and wherein difference is: described modifying element is Ce or Y, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 1% of an alloy melt quality.
Embodiment 7
(1) be that the CuO powder of 100 μ m is to handle 0.5h under 300 ℃ of conditions in temperature with particle diameter;
(2) mixture and the modifying element with the Al of the Cu of quality purity 〉=99.9% and quality purity 〉=99.9% together places in the spray co deposition vacuum intermediate frequency (IF) smelting stove, is that alloying obtains alloy melt under 1070 ℃ of conditions in temperature; The mass percent of Al is 2% in the described mixture, and surplus is Cu; Described modifying element is Ce, and the addition of modifying element is 2% of an alloy melt quality;
(3) treat that the alloy melt temperature reaches 100 ℃ after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and is started powder conveying device and carry after treatment CuO powder, carrying out spray co deposition, to obtain CuAl/CuO be alloy; The operational throughput of described CuO powder is Al and Ce amount of substance sum 3/2 times; The deposition distance of described spray co deposition is 400mm, and atomization pressure is 0.8MPa, and the thrust-augmenting nozzle internal diameter is 4mm, and the depositor rotating speed is 25rpm/min;
(4) under vacuum condition, in-situ chemical reaction 10h under 800 ℃ the condition to the CuAl/CuO alloy in temperature, prepare CuAl
2O
3Matrix material;
(5) with CuAl
2O
3Matrix material is the CuAl that extrusion processing becomes bar or sheet material shape under 500 ℃ of conditions in temperature
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into shapes such as sheet material, silk material, profiled material or contact according to application requiring
2O
3Matrix material.
Embodiment 8
Present embodiment is identical with embodiment 7 preparation methods, and wherein difference is: described modifying element is La or Y, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 0.01% of an alloy melt quality.
Embodiment 9
Present embodiment is identical with embodiment 7 preparation methods, and wherein difference is: described modifying element is La or Y, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 1% of an alloy melt quality.
Embodiment 10
(1) be that the CuO powder of 55 μ m is to handle 1.2h under 200 ℃ of conditions in temperature with particle diameter;
(2) mixture and the modifying element with the Al of the Cu of quality purity 〉=99.9% and quality purity 〉=99.9% together places in the spray co deposition vacuum intermediate frequency (IF) smelting stove, is that alloying obtains alloy melt under 1040 ℃ of conditions in temperature; The mass percent of Al is 4% in the described mixture, and surplus is Cu; Described modifying element is Y, and the addition of modifying element is 1% of an alloy melt quality;
(3) treat that the alloy melt temperature reaches 150 ℃ after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and is started powder conveying device and carry after treatment CuO powder, carrying out spray co deposition, to obtain CuAl/CuO be alloy; The operational throughput of described CuO powder is Al and Y amount of substance sum 3/2 times; The deposition distance of described spray co deposition is 350mm, and atomization pressure is 1.4MPa, and the thrust-augmenting nozzle internal diameter is 4.5mm, and the depositor rotating speed is 40rpm/min;
(4) under vacuum condition, in-situ chemical reaction 7h under 900 ℃ the condition to the CuAl/CuO alloy in temperature, prepare CuAl
2O
3Matrix material;
(5) with CuAl
2O
3Matrix material is the CuAl that extrusion processing becomes bar or sheet material shape under 600 ℃ of conditions in temperature
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into shapes such as sheet material, silk material, profiled material or contact according to application requiring
2O
3Matrix material.
Embodiment 11
Present embodiment is identical with embodiment 10 preparation methods, and wherein difference is: described modifying element is La or Ce, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 0.01% of an alloy melt quality.
Embodiment 12
Present embodiment is identical with embodiment 10 preparation methods, and wherein difference is: described modifying element is La or Ce, perhaps is at least two kinds among La, Ce and the Y, and the addition of modifying element is 2% of an alloy melt quality.
The CuAl of the embodiment of the invention 1 to embodiment 12 preparation
2O
3The physicals of matrix material is as shown in table 1.
The CuAl of table 1 preparation
2O
3The physicals of matrix material
Claims (6)
1. spray co deposition prepared in reaction CuAl
2O
3The method of matrix material is characterized in that, this method may further comprise the steps:
(1) be to handle 0.5h～2h under 100 ℃～300 ℃ the condition with the CuO powder in temperature;
(2) mixture of Cu and Al is placed alloying obtains alloy melt in the spray co deposition vacuum intermediate frequency (IF) smelting stove, the mass percent of Al is 0.1%～4% in the described mixture, and surplus is Cu; Or the mixture of Cu and Al and modifying element placed together alloying obtains alloy melt in the spray co deposition vacuum intermediate frequency (IF) smelting stove, described modifying element is one or more among La, Ce and the Y, and the addition of described modifying element is 0.01%～2% of an alloy melt quality;
(3) treat that the alloy melt temperature reaches 100 ℃～200 ℃ described in the step (2) after, open the atomization gas valve, simultaneously alloy melt is poured into insulation bag, and started in the powder conveying device supplying step (1) CuO powder after treatment, carry out spray co deposition and obtain the CuAl/CuO alloy; The operational throughput of described CuO powder is 3/2 times of molar weight of Al, perhaps is Al and modifying element amount of substance sum 3/2 times;
(4) be in-situ chemical reaction 4h～10h under 800 ℃～1000 ℃ the vacuum condition with CuAl/CuO alloy described in the step (3), prepare CuAl in temperature
2O
3Matrix material;
(5) with CuAl described in the step (4)
2O
3The matrix material extrusion processing becomes the CuAl of bar or sheet material shape
2O
3Matrix material, further rolling or drawing again, the final CuAl that is reprocessed into sheet material, silk material, profiled material or contact shape according to application requiring
2O
3Matrix material.
2. spray co deposition prepared in reaction CuAl according to claim 1
2O
3The method of matrix material is characterized in that, the particle diameter of CuO powder described in the step (1) is 10 μ m～100 μ m.
3. spray co deposition prepared in reaction CuAl according to claim 1
2O
3The method of matrix material is characterized in that, quality purity 〉=99.9% of Cu described in the step (2), the quality purity of described Al 〉=99.9%.
4. spray co deposition prepared in reaction CuAl according to claim 1
2O
3The method of matrix material is characterized in that, the temperature of alloying described in the step (2) is 1040 ℃～1100 ℃.
5. spray co deposition prepared in reaction CuAl according to claim 1
2O
3The method of matrix material, it is characterized in that the distance of the deposition of spray co deposition described in the step (3) is 300mm～400mm, atomization pressure is 0.8MPa～2.0MPa, the thrust-augmenting nozzle internal diameter is 3.5mm～4.5mm, and the depositor rotating speed is 10rpm/min～40rpm/min.
6. spray co deposition prepared in reaction CuAl according to claim 1
2O
3The method of matrix material is characterized in that, the temperature of extruding is 400 ℃～600 ℃ described in the step (5).
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Cited By (1)
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| CN106735223A (en) * | 2016-12-14 | 2017-05-31 | 中国科学院力学研究所 | A kind of Metal Substrate in-situ authigenic particle strengthens the increasing material manufacturing method of component |
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| CN101890498A (en) * | 2010-06-24 | 2010-11-24 | 昆明理工大学 | Preparation method of CuAlO2 target |
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2010
- 2010-12-06 CN CN 201010575412 patent/CN101984118B/en active Active
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| CN106735223A (en) * | 2016-12-14 | 2017-05-31 | 中国科学院力学研究所 | A kind of Metal Substrate in-situ authigenic particle strengthens the increasing material manufacturing method of component |
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