CN1141406C - Process for preparing Cu-Al2O3 composition - Google Patents
Process for preparing Cu-Al2O3 composition Download PDFInfo
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- CN1141406C CN1141406C CNB021138168A CN02113816A CN1141406C CN 1141406 C CN1141406 C CN 1141406C CN B021138168 A CNB021138168 A CN B021138168A CN 02113816 A CN02113816 A CN 02113816A CN 1141406 C CN1141406 C CN 1141406C
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Abstract
The present invention relates to a method for preparing a composite copper and alumina material which is prepared by the way that aluminum powder or xalloy powder, copper powder and an oxidant as raw materials are matched with lanthanum and cerium as additional elements, and all materials are synthesized by pressed moulding and a sintering reaction; finally, the materials are extruded and drawn into the composite copper and alumina material. Because being synthesized by an in-situ reaction in the sintering process, Al2O3 particles as reinforced phases have the advantages of fresh reaction interface, firm combination with copper as a substrate and obvious strengthening effect. The technology has the characteristics of simple preparation of raw material, one-step completion of sintering and reaction, excellent material performance, etc.; besides, the steps of the preparation process can be easily controlled, and the dispersive distribution of the reinforced phase particles of the composite material is completed by processing and deformation. Thereby, the method solves the problem of the difficult subsequent processing of the composite metal-based material with reinforced particles.
Description
(1) technical field: metal-base composites scientific domain
(2) background technology: the preparation method of known Cu-Al 2 O 3 composition has following several:
1. powder metallurgic method.With copper powder and aluminum oxide powder thorough mixing, pass through powder forming, sinter prefabricated component into, through liquid phase method of impregnation infiltration copper in strengthening the body prefabricated component, finally obtain Cu-Al 2 O 3 composition then.
2. mechanical alloying method.By the method for high-energy ball milling or bump, make copper powder and wild phase aluminum oxide thorough mixing, fragmentation, compress then, moulding, sintering.Thereby acquisition Cu-Al 2 O 3 composition.
3. coprecipitation method: with cupric nitrate and Tai-Ace S 150 is that preparation of raw material becomes to contain the certain volume mark aluminium sesquioxide aqueous solution, under the certain temperature condition, add the ammonium solution of certain volume volumetric molar concentration, through behind the sedimentation and filtration, in certain temperature oven dry and ignite into oxide compound, carry out selective reduction at last and handle.
4. composite electrodeposition method: the alumina particulate in the plating bath and matrix metal copper common deposited at cathode surface, are formed the multilayer materials of composite deposite.
5. thermal reduction method of formation: select copper-aluminium alloy powder, cupric oxide powder for use, make pressed compact according to reaction ratio, then pressed compact (1150-1250 ℃) under molten copper temperature is pressed into copper alloy, the aluminium sesquioxide particle that reaction generates disperse under the effect of electromagnetic force distributes, pour into ingot casting again through cold working, obtain Cu-Al 2 O 3 composition.
6. internal oxidation: behind a certain proportion of copper-aluminium alloy powder and oxidizing medium uniform mixing, carry out interior oxidation in confined conditions; Perhaps guaranteeing to make the aluminium element oxidation under the not oxidized prerequisite of matrix by strict hierarchy of control oxygen gesture.Then Cu-Al 2 O 3 composition is made in mixed powder sintering, cold and hot distortion.
Though known preparation method has obtained Cu-Al 2 O 3 composition, 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: coprecipitation method and composite electrodeposition method have pollution to environment, and the material property that coprecipitation method obtains is lower, and composite electrodeposition method particle evenly suspends wayward in plating bath; The gas that the thermal reduction method of formation produces is difficult for discharging in copper liquid, can cause that copper liquid splashes, and potential safety hazard is arranged in the production, and it is inhomogeneous to obtain the particle dispersion of material; Though the Cu-Al 2 O 3 composition over-all properties of internal oxidation preparation is better, in preparation process, oxygen partial pressure, oxidization time and amount of oxidation are difficult to control, are unfavorable for suitability for industrialized production.
(3) summary of the invention: the objective of the invention is the deficiency that exists at known technology and a kind of novel method that proposes, this method is to finish in chemical reaction and one step of sintering, and the aluminium sesquioxide particle generates in position, and the interface is fresh, and is firm with combining of matrix copper; And particulate disperse of wild phase aluminium sesquioxide and machining deformation carry out simultaneously, have well solved the problem of particulate reinforced composite following process difficulty.
The present invention realizes by following technical scheme.
Fig. 1 is a process flow sheet of the present invention, raw material is behind batching and thorough mixing, compression moulding in punching block, synthetic by sintering reaction again, generate the aluminium sesquioxide particle and the distribution thereof that need, behind repressing and re-sintering, directly extruding or rolling bar base or the band of becoming will become required silk material or further be processed into contact material again after bar base or band cold drawing or the rolling processing.One, material composition and shared per-cent:
(1) main raw material: copper-aluminium alloy powder or aluminium powder, copper powder, granularity are 45～150 microns, and weight percent is 1.0～30.0% copper-aluminium alloy powder, or weight percent is 0.2～8.0% aluminium powder,
Oxygenant be weight percentage 0.05～10.0% cupric oxide powder or brown iron oxide, granularity is 0～45 micron,
The copper powder surplus;
(2) add element:
1. lanthanum (La): be no more than 0.05% of gross weight;
2. cerium (Ce): be no more than 0.02% of gross weight.Two, composition of raw materials:
(1) main raw material;
(2) main raw material+the interpolation element 1.;
(3) main raw material+the interpolation element 2..Three, technical qualification:
(1) mixing raw materials time: 2-35 hour;
(2) compression moulding pressure: 300-600MPa;
(3) sintering reaction synthesis temperature: 100-1000 ℃ of segmentation insulation reaction;
(4) the synthetic atmosphere of sintering reaction: vacuum (1～5 * 10
-1Pa);
(5) sintering reaction generated time: 4-25 hour;
(6) repressing and re-sintering temperature: 300～800 ℃;
(7) repressing and re-sintering pressure: 400～700MPa;
(8) squeeze pressure: 500-700MPa.
Compare advantage and the positively effect that is had with known technology:
1. sintering is once finished with reaction is synthetic, has shortened the materials processing operation, has reduced material cost;
Aluminum oxide wild phase original position generate, fresh with the formed interface of copper matrix, combine firm, and oxygen
Change the aluminum particulate size and can pass through technology controlling and process, to strengthen strengthening effect;
3. raw material is prepared simple, technological process and is controlled excellent material performance easily.
(4) description of drawings: Fig. 1 is a process flow sheet of the present invention.
(5) embodiment:
Embodiment one
According to 0.53%Al (aluminium) (weight percent), 2.34%CuO (cupric oxide), copper surplus is raw material, through behind 6 hours batch mixings, and compression moulding in punching block, pressure is 550MPa; Be 2 * 10 at vacuum condition after the moulding
-1It is synthetic that Pa, elder generation after 2 hours, are warmed up to 850 ℃ with insulation under 100 ℃ of temperature condition, sintering reaction was carried out in insulation in 5 hours; The synthetic materials ingot blank is that 500MPa, temperature are to carry out repressing and re-sintering under 500 ℃ of conditions to improve the density of material through excess pressure, and the squeeze with 500MPa is extruded into the line bar then, and last cold drawing becomes line (silk) material.Perhaps, further be processed into contact material (as rivet).
Embodiment two
According to 8.0%Cu-Al (copper-aluminium alloy powder) (weight percent), 9.36%CuO (cupric oxide), 0.04%La (lanthanum), copper surplus is raw material, through behind 2 hours batch mixings, and compression moulding in punching block, pressure 600MPa; Be 1 * 10 in vacuum tightness after the moulding
-1Under the Pa condition, it is synthetic that elder generation after 2 hours, is warmed up to 950 ℃ with insulation under 120 ℃ of temperature condition, sintering reaction was carried out in insulation in 3 hours; Synthetic ingot blank is that 550MPa, temperature are to carry out repressing and re-sintering under 600 ℃ of conditions to improve the density of material through excess pressure, and the squeeze with 650MPa is extruded into the line bar or is rolled into strip then, finally is drawn into a material or makes band.
Embodiment three
According to 8.0%Cu-Al (copper-aluminium alloy powder) (weight percent), 9.36%CuO (cupric oxide), 0.04%Ce (cerium), copper surplus is raw material, through behind 2 hours batch mixings, and compression moulding in punching block, pressure 600MPa; Be 1 * 10 in vacuum tightness after the moulding
-1Under the Pa condition, it is synthetic that elder generation after 1 hour, is warmed up to 1000 ℃ with insulation under 180 ℃ of temperature condition, sintering reaction was carried out in insulation in 4 hours; Synthetic ingot blank is that 550MPa, temperature are to carry out repressing and re-sintering under 600 ℃ of conditions to improve the density of material through excess pressure, and the squeeze with 650MPa is extruded into the line bar or is rolled into strip then, finally is drawn into a material or makes band.
Claims (4)
1. method for preparing Cu-Al 2 O 3 composition is characterized in that:
1) technical process: raw material is behind batching and thorough mixing, compression moulding in punching block, synthetic by sintering reaction again, generate the aluminium sesquioxide particle and the distribution thereof that need, behind repressing and re-sintering, directly extruding or rolling bar base or the band of becoming will become required silk material or further be processed into contact material again after bar base or band cold drawing or the rolling processing;
(1) main raw material: copper-aluminium alloy powder or aluminium powder, copper powder, granularity are 45～150 microns, and weight percent is 1.0～30.0% copper-aluminium alloy powder, or weight percent is 0.2～8.0% aluminium powder,
Oxygenant be weight percentage 0.05～10.0% cupric oxide powder or brown iron oxide, granularity is 0～45 micron,
The copper powder surplus;
(2) add element:
1. lanthanum: be no more than 0.05% of gross weight,
2. cerium: be no more than 0.02% of gross weight; 2) composition of raw materials:
(1) main raw material,
(2) main raw material+interpolation element 1.,
(3) main raw material+the interpolation element 2.; 3) technical qualification:
(1) mixing raw materials time: 2-35 hour,
(2) compression moulding pressure: 300-600Mpa,
(3) sintering reaction synthesis temperature: 100-1000 ℃ of segmentation insulation reaction,
(4) the synthetic atmosphere of sintering reaction: vacuum tightness is 1～5 * 10
-1Pa,
(5) sintering reaction generated time: 4-25 hour,
(6) repressing and re-sintering temperature: 300～800 ℃,
(7) repressing and re-sintering pressure: 400～700Mpa,
(8) squeeze pressure: 500-700MPa.
2, the method for preparing Cu-Al 2 O 3 composition according to claim 1, it is characterized in that: according to weight percent 0.53% aluminium powder, 2.34% cupric oxide powder, copper powder surplus is raw material, through behind 6 hours batch mixings, compression moulding in punching block, pressure is 550Mpa, is 2 * 10 in vacuum tightness after the moulding
-1Under the condition of Pa, after being incubated 2 hours down with 100 ℃ of temperature condition earlier, be warmed up to 850 ℃, that sintering reaction was carried out in insulation in 5 hours is synthetic, the synthetic materials ingot blank is that 500MPa, temperature are to carry out repressing and re-sintering under 500 ℃ of conditions through excess pressure, squeeze with 500MPa is extruded into the line bar then, and last cold drawing becomes line or silk material.
3, the method for preparing Cu-Al 2 O 3 composition according to claim 1, it is characterized in that: according to weight percent 8.0% copper-aluminium alloy powder, 9.36% cupric oxide powder, 0.04% lanthanum, copper powder surplus is raw material, through behind 2 hours batch mixings, compression moulding in punching block, pressure 600Mpa, after the moulding, be 1 * 10 in vacuum tightness
-1Under the condition of Pa, earlier with after being incubated 2 hours under 120 ℃ of temperature condition, be warmed up to 950 ℃, that sintering reaction was carried out in insulation in 3 hours is synthetic, synthetic ingot blank is that 550MPa, temperature are to carry out repressing and re-sintering under 600 ℃ of conditions through excess pressure, squeeze with 650MPa is extruded into the line bar or is rolled into strip then, finally is drawn into a material or makes band.
4, the method for preparing Cu-Al 2 O 3 composition according to claim 1, it is characterized in that: according to weight percent 8.0% copper-aluminium alloy powder, 9.36% cupric oxide powder, 0.04% cerium, copper powder surplus is raw material, through behind 2 hours batch mixings, compression moulding in punching block, pressure 600Mpa, after the moulding, be 1 * 10 in vacuum tightness
-1Under the condition of Pa, after being incubated 1 hour down with 180 ℃ of temperature condition earlier, be warmed up to 1000 ℃, that sintering reaction was carried out in insulation in 4 hours is synthetic, synthetic ingot blank is that 550MPa, temperature are to carry out repressing and re-sintering under 600 ℃ of conditions through excess pressure, squeeze with 650MPa is extruded into the line bar or is rolled into strip then, finally is drawn into a material or band.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021138168A CN1141406C (en) | 2002-05-30 | 2002-05-30 | Process for preparing Cu-Al2O3 composition |
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| CNB021138168A CN1141406C (en) | 2002-05-30 | 2002-05-30 | Process for preparing Cu-Al2O3 composition |
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| CN1141406C true CN1141406C (en) | 2004-03-10 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100354999C (en) * | 2005-10-07 | 2007-12-12 | 乐清市帕特尼触头有限公司 | Cleaning environment-friendly type copper-base contact material for low-voltage electrical apparatus and its contact preparing method |
| CN100395360C (en) * | 2006-07-22 | 2008-06-18 | 淮阴工学院 | Method for preparing copper base composite material by chemical precipitation method to obtain composite powder |
| CN100413993C (en) * | 2006-10-20 | 2008-08-27 | 西安理工大学 | Cu-La2O3/Al2O3 composite material and its preparing method |
| CN101178957B (en) * | 2007-12-04 | 2011-07-27 | 河南科技大学 | Method of producing the copper alloy contact wire |
| CN101653792B (en) * | 2009-09-22 | 2011-08-31 | 西北有色金属研究院 | Processing method of molybdenum and molybdenum alloy narrowband |
| CN101880814B (en) * | 2010-07-02 | 2012-11-28 | 北京工业大学 | Abrasion-resistant electricity and heat conducting material and preparation method thereof |
| CN102560172B (en) * | 2012-03-13 | 2013-07-03 | 北京科技大学 | Method for preparing dispersion-strengthened copper with high strength and high conductivity |
| CN106834792A (en) * | 2017-01-24 | 2017-06-13 | 付亚波 | Add high intensity, dispersion-strengthened Cu of high conductivity of Rare Earth Lanthanum and preparation method thereof |
| CN108526459B (en) * | 2018-04-16 | 2019-12-03 | 昆明理工大学 | A kind of preparation method of copper/aluminium oxide In-situ reaction cellular material |
| CN109082568A (en) * | 2018-08-29 | 2018-12-25 | 天津大学 | A kind of fabricated in situ nanometer CuAl2/Al2O3The preparation method of reinforced aluminum matrix composites |
| CN109536771B (en) * | 2018-11-23 | 2020-08-25 | 中铝洛阳铜加工有限公司 | Preparation method of dispersion-strengthened oxygen-free copper alloy plate |
| CN112391552A (en) * | 2020-12-07 | 2021-02-23 | 西安稀有金属材料研究院有限公司 | Preparation method of in-situ authigenic alumina reinforced copper-based composite material |
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