CN108526459B - A kind of preparation method of copper/aluminium oxide In-situ reaction cellular material - Google Patents

A kind of preparation method of copper/aluminium oxide In-situ reaction cellular material Download PDF

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CN108526459B
CN108526459B CN201810339595.1A CN201810339595A CN108526459B CN 108526459 B CN108526459 B CN 108526459B CN 201810339595 A CN201810339595 A CN 201810339595A CN 108526459 B CN108526459 B CN 108526459B
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powder
copper
aluminium
mixed
cellular material
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CN108526459A (en
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张芳杰
张磊
左孝青
周芸
罗晓旭
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Kunming University of Science and Technology
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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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F3/001—Starting from powder comprising reducible metal compounds
    • 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
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • B22F3/1115—Making porous workpieces or articles with particular physical characteristics comprising complex forms, e.g. honeycombs
    • 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
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1143—Making porous workpieces or articles involving an oxidation, reduction or reaction step
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • 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
    • C22C32/0015—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 with only single oxides as main non-metallic constituents
    • C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Abstract

The present invention discloses a kind of preparation method of copper/aluminium oxide In-situ reaction cellular material, belong to composite porous field, plasticizer is added in the method for the invention after mixing using aluminium powder, cupric oxide powder and water is kneaded, mixing materials are squeezed into honeycomb structure, by vacuum and the reduction sintering of two step of reducing atmosphere after honeycomb structure after extruding is dry, copper/aluminium oxide In-situ reaction cellular material is made；Copper prepared by the present invention/aluminium oxide In-situ reaction cellular material, generated in-situ aluminium oxide and Copper substrate interface cohesion are good, have the characteristics such as high temperature resistant, high-strength, high thermal conductivity, and production cost is low, it can be achieved that industrialized production.

Description

A kind of preparation method of copper/aluminium oxide In-situ reaction cellular material
Technical field
The present invention relates to a kind of copper/aluminium oxide In-situ reaction cellular material preparation methods, belong to composite porous neck Domain.
Background technique
The metal/ceramic composite honeycomb material prepared using powder plastic extrusion method, has both metal beehive and ceramic honeycomb Characteristic not only has the metallic characters such as high-termal conductivity and obdurability, also has the ceramic characteristics such as high temperature resistant, heat shock resistance, be one The novel and multifunctional composite material of kind high comprehensive performance is led in vehicle maintenance service, high efficiency and heat radiation material and aerospace etc. Domain has a wide range of applications.
However, conventional powder plastic extrusion method prepares the compound cellular material of metal/ceramic, ceramic particle and metal The poor compatibility of matrix, interface bond strength are low, thus to the mechanical property and high-temperature behavior of metal/ceramic composite honeycomb material It has a negative impact；In addition, conventional powder plastic extrusion method prepares the compound cellular material of metal/ceramic, there is also main bodys The high deficiency of cost of material, results in higher production cost.
Summary of the invention
The shortcomings that overcome above-mentioned metal/ceramic composite honeycomb material preparation technology, the present invention provides a kind of copper/oxidations Two steps of aluminium In-situ reaction cellular material restore sintering preparation method, use aluminium powder, cupric oxide powder for raw material, after raw material is drifted along or through Plasticizer and water is added to be kneaded, mixing materials are squeezed into honeycomb structure, after honeycomb structure after extruding is dry by vacuum and The reduction sintering of two step of reducing atmosphere, is made copper/aluminium oxide In-situ reaction cellular material.
The present invention provides a kind of preparation method of copper/aluminium oxide In-situ reaction cellular material, the specific steps are as follows:
(1) aluminium powder and cupric oxide powder mixed, refining material: are accounted for the 1.3- of aluminium powder and cupric oxide powder gross mass according to aluminium powder first 4.0% ratio is uniformly mixed and obtains mixed-powder, and plasticizer and water are then accounted for plasticizer and water gross mass according to plasticizer The ratio of 25-40% be uniformly mixed and obtain mixture, finally by aluminium powder, the mixed-powder of cupric oxide powder and plasticizer, water Mixture accounts for the ratio mixing refining material of the 80-86% of mixed-powder and mixture gross mass according to mixed-powder；
(2) honeycomb structure squeezes: mixing materials prepared by step (1) are put into porous shunting mold to be squeezed into hole close Degree be 10-20PPI, the honeycomb structure that aperture is 1-2mm；
(3) dry: step (2) resulting honeycomb structure is put into thermostatic drying chamber in 130-160 DEG C of dry 1.25- 2h；
(4) vacuum reduction is sintered: the honeycomb structure after will be dry obtained by step (3) carries out vacuum reduction sintering, first Furnace temperature, which is risen to 250-400 DEG C of heat preservation 15-30min, decomposes plasticizer, then heat to 550-700 DEG C of heat preservation 15-30min into Row is pre-sintered, and being finally warming up to 800-950 DEG C of heat preservation 3.5-5h for the aluminium powder in-situ oxidation in honeycomb structure is aluminium oxide, is obtained Obtain honeycomb precast body；
(5) hydrogen atmosphere reduction sintering: the precast body that step (4) is obtained, in the vacuum atmosphere oven for being passed through hydrogen atmosphere Continue reduction sintering 3.25-4h in 800-950 DEG C, is elemental copper by remaining cupric oxide powder in-situ reducing, copper/oxygen is finally made Change aluminium In-situ reaction cellular material.
Step (1) cupric oxide powder is the commercially available industrial oxidation copper powder of granularity 200-400 purpose；Aluminium powder is granularity 400- The commercially available technical pure aluminium powder of 600 purposes.
Step (1) the plasticizer is commercial polyethylene alcohol or methylcellulose.
Step (4) the vacuum reduction sintering, vacuum degree 10-4-10-2Pa。
Step (5) hydrogen is commercially available plant hydrogen, hydrogen flowing quantity 0.25-1L/min.
The copper that the present invention is prepared/aluminium oxide In-situ reaction cellular material, void density 13-28PPI, aperture is 0.72-1.54mm, the mass fraction of aluminium oxide are 3-9%.
Inventive principle:
1, copper/aluminium oxide reaction in-situ and quality proportioning principle
The honeycomb structure of extrusion forming is placed in vacuum after reduction sintering, aluminium powder and copper oxide in honeycomb structure Powder generates aluminium oxide and copper, the excessive cupric oxide powder of remainder, the reaction in-situ of aluminium powder and cupric oxide powder by reaction in-situ Formula is as follows:
2Al+3CuO=Al2O3+3Cu (1)
Aluminium oxide and copper oxide honeycomb after vacuum-sintering are placed in hydrogen reducing atmosphere after reduction sintering, in reaction (1) Remaining cupric oxide powder is reduced to elemental copper by hydrogen in-situ, and the reaction in-situ formula of copper oxide and hydrogen is as follows:
CuO+H2=Cu+H2O (2)
By reaction (1) and reaction (2), mass fraction Y, Al powder of the CuO powder in mixed-powder can be established respectively mixed Close mass fraction Z and Al in powder2O3In the relational expression in composite honeycomb material between mass fraction X:
In formula: X:Al2O3Mass fraction (3.0wt.%≤X≤9.0wt.%) in composite metal honeycomb
Mass fraction (96.0wt.%≤Y≤98.7wt.%) of the Y:CuO powder in mixed powder
Mass fraction (1.3wt.%≤Z≤4.0wt.%) of the Z:Al powder in mixed powder
2, honeycomb sintering shrinkage principle
For metal beehive when through vacuum and the reduction sintering of two step of hydrogen atmosphere, honeycomb can generate contraction, to draw The aperture for playing metal beehive reduces and void density increases, the shrinking percentage and sintering temperature, total sintering time of metal honeycomb structure The relationship of (the sum of vacuum and two step of hydrogen atmosphere reduction sintering time under sintering temperature) is as follows:
η=0.4145ln (T+8)+0.004t2-0.0528t-2.3961
In formula: η: honeycomb shrinking percentage (20%≤η≤30%)
T: sintering temperature (DEG C, 800 DEG C≤T≤950 DEG C)
T: total sintering time (h, 6.75h≤t≤9h), t=t1+t2
t1: vacuum-sintering time (h, 3.5h≤t1≤5h)
t2: hydrogen atmosphere sintering time (h, 3.25h≤t2≤4h)
Beneficial effects of the present invention
The present invention occurs reaction in-situ and generates oxidation by vacuum and the reduction sintering of two step of hydrogen atmosphere, metal beehive inside Aluminium reinforcement and Copper substrate, interface cohesion is good between generated in-situ alumina particle and Copper substrate, and alumina particle plays Dispersion-strengthened action improves the intensity of composite honeycomb, overcomes ceramic particle and metallic matrix interface in conventional composite honeycomb The problem that bond strength is low, cost of material is high has the excellent performances such as high temperature resistant, high-strength, high thermal conductivity, and production cost is low, can be real Existing industrialized production.
Detailed description of the invention
Fig. 1 is two steps of copper/aluminium oxide In-situ reaction cellular material reduction sintering preparation technology flow chart.
Specific embodiment
The present invention will be further described for mode in the following with reference to the drawings and specific embodiments.
Embodiment 1
A kind of copper of the present embodiment/aluminium oxide In-situ reaction cellular material preparation method, as shown in Figure 1, specific steps are such as Under:
(1) mixed, refine material: first by the commercially available technical pure aluminium powder of 200 purposes and the commercially available industrial oxidation copper powder of 400 purposes according to 1.3% ratio that aluminium powder accounts for aluminium powder and cupric oxide powder gross mass, which is uniformly mixed, obtains mixed-powder, then by plasticizer and water It is uniformly mixed according to 25% ratio that plasticizer accounts for plasticizer and water gross mass and obtains mixture, finally by aluminium powder, copper oxide The mixed-powder and plasticizer of powder, the mixture of water account for 80% ratio of mixed-powder and mixture gross mass according to mixed-powder Example mixing refining material, plasticizer is polyvinyl alcohol；
(2) honeycomb structure squeezes: mixing materials prepared by step (1) are put into porous shunting mold to be squeezed into hole close Degree be 10PPI, the honeycomb structure that aperture is 2mm；
(3) dry: step (2) resulting honeycomb structure is put into thermostatic drying chamber in 130 DEG C of dry 2h；
(4) vacuum reduction is sintered: it is 10 that the honeycomb structure after will be dry obtained by step (3), which is placed in vacuum degree,-2Pa's is true Vacuum reduction sintering is carried out in air atmosphere furnace, furnace temperature, which is raised to 250 DEG C of heat preservation 30min, first decomposes plasticizer, then heats up It is pre-sintered to 550 DEG C of heat preservation 30min, is finally warming up to 800 DEG C of heat preservation 5h for the aluminium powder in-situ oxidation in honeycomb structure For aluminium oxide, honeycomb precast body is obtained；
(5) hydrogen atmosphere reduction sintering: the precast body that step (4) is obtained, be passed through hydrogen flowing quantity be 0.25L/min also Continue reduction sintering 4h for 800 DEG C in the vacuum atmosphere oven of Primordial Qi atmosphere, is elemental copper by remaining cupric oxide powder in-situ reducing, finally Copper/aluminium oxide In-situ reaction bee that void density is 13PPI, aperture 1.54mm, quality of alumina score are 3% is prepared Nest material.
Embodiment 2
A kind of copper of the present embodiment/aluminium oxide In-situ reaction cellular material preparation method, the specific steps are as follows:
(1) mixed, refine material: first by the commercially available technical pure aluminium powder of 300 purposes and the commercially available industrial oxidation copper powder of 500 purposes according to 2.3% ratio that aluminium powder accounts for aluminium powder and cupric oxide powder gross mass, which is uniformly mixed, obtains mixed-powder, then by plasticizer and water It is uniformly mixed according to 30% ratio that plasticizer accounts for plasticizer and water gross mass and obtains mixture, finally by aluminium powder, copper oxide The mixed-powder and plasticizer of powder, the mixture of water account for 82% ratio of mixed-powder and mixture gross mass according to mixed-powder Example mixing refining material, plasticizer is polyvinyl alcohol；
(2) honeycomb structure squeezes: mixing materials prepared by step (1) are put into porous shunting mold to be squeezed into hole close Degree be 13PPI, the honeycomb structure that aperture is 1.7mm；
(3) dry: step (2) resulting honeycomb structure is put into thermostatic drying chamber in 140 DEG C of dry 1.75h；
(4) vacuum reduction is sintered: it is 10 that the honeycomb structure after will be dry obtained by step (3), which is placed in vacuum degree,-3Pa's is true Vacuum reduction sintering is carried out in air atmosphere furnace, furnace temperature, which is raised to 300 DEG C of heat preservation 25min, first decomposes plasticizer, then heats up It is pre-sintered to 600 DEG C of heat preservation 25min, is finally warming up to 850 DEG C of heat preservation 4.5h for the aluminium powder situ oxygen in honeycomb structure Aluminium oxide is turned to, honeycomb precast body is obtained；
(5) hydrogen atmosphere reduction sintering: the precast body that step (4) is obtained, be passed through hydrogen flowing quantity be 0.5L/min also Continue reduction sintering 3.75h for 800 DEG C in the vacuum atmosphere oven of Primordial Qi atmosphere, be elemental copper by remaining cupric oxide powder in-situ reducing, It is multiple in situ that copper/aluminium oxide that void density is 17PPI, aperture 1.29mm, quality of alumina score are 5% is finally prepared Close cellular material.
Embodiment 3
A kind of copper of the present embodiment/aluminium oxide In-situ reaction cellular material preparation method, the specific steps are as follows:
(1) mixed, refine material: first by the commercially available technical pure aluminium powder of 300 purposes and the commercially available industrial oxidation copper powder of 500 purposes according to 3.1% ratio that aluminium powder accounts for aluminium powder and cupric oxide powder gross mass, which is uniformly mixed, obtains mixed-powder, then by plasticizer and water It is uniformly mixed according to 35% ratio that plasticizer accounts for plasticizer and water gross mass and obtains mixture, finally by aluminium powder, copper oxide The mixed-powder and plasticizer of powder, the mixture of water account for 84% ratio of mixed-powder and mixture gross mass according to mixed-powder Example mixing refining material, plasticizer is methylcellulose；
(2) honeycomb structure squeezes: mixing materials prepared by step (1) are put into porous shunting mold to be squeezed into hole close Degree be 17PPI, the honeycomb structure that aperture is 1.3mm；
(3) dry: step (2) resulting honeycomb structure is put into thermostatic drying chamber in 150 DEG C of dry 1.5h；
(4) vacuum reduction is sintered: it is 10 that the honeycomb structure after will be dry obtained by step (3), which is placed in vacuum degree,-3Pa's is true Vacuum reduction sintering is carried out in air atmosphere furnace, furnace temperature, which is raised to 350 DEG C of heat preservation 20min, first decomposes plasticizer, then heats up It is pre-sintered to 650 DEG C of heat preservation 20min, is finally warming up to 900 DEG C of heat preservation 4h for the aluminium powder in-situ oxidation in honeycomb structure For aluminium oxide, honeycomb precast body is obtained；
(5) hydrogen atmosphere reduction sintering: the precast body that step (4) is obtained, be passed through hydrogen flowing quantity be 0.75L/min also Continue reduction sintering 3.5h for 900 DEG C in the vacuum atmosphere oven of Primordial Qi atmosphere, is elemental copper by remaining cupric oxide powder in-situ reducing, most Copper/aluminium oxide In-situ reaction that void density is 23PPI, aperture 0.96mm, quality of alumina score are 7% is prepared afterwards Cellular material.
Embodiment 4
A kind of copper of the present embodiment/aluminium oxide In-situ reaction cellular material preparation method, the specific steps are as follows:
(1) mixed, refine material: first by the commercially available technical pure aluminium powder of 400 purposes and the commercially available industrial oxidation copper powder of 600 purposes according to 4% ratio that aluminium powder accounts for aluminium powder and cupric oxide powder gross mass, which is uniformly mixed, obtains mixed-powder, then presses plasticizer and water It is uniformly mixed according to 40% ratio that plasticizer accounts for plasticizer and water gross mass and obtains mixture, finally by aluminium powder, cupric oxide powder Mixed-powder and the mixture of plasticizer, water 86% ratio of mixed-powder and mixture gross mass is accounted for according to mixed-powder Mixing refining material, plasticizer is methylcellulose；
(2) honeycomb structure squeezes: mixing materials prepared by step (1) are put into porous shunting mold to be squeezed into hole close Degree be 20PPI, the honeycomb structure that aperture is 1mm；
(3) dry: step (2) resulting honeycomb structure is put into thermostatic drying chamber in 160 DEG C of dry 1.25h；
(4) vacuum reduction is sintered: it is 10 that the honeycomb structure after will be dry obtained by step (3), which is placed in vacuum degree,-4Pa's is true Vacuum reduction sintering is carried out in air atmosphere furnace, furnace temperature, which is raised to 400 DEG C of heat preservation 15min, first decomposes plasticizer, then heats up It is pre-sintered to 700 DEG C of heat preservation 15min, is finally warming up to 950 DEG C of heat preservation 3.5h for the aluminium powder situ oxygen in honeycomb structure Aluminium oxide is turned to, honeycomb precast body is obtained；
(5) hydrogen atmosphere reduction sintering: the precast body that step (4) is obtained is being passed through hydrogen flowing quantity as 1L/min reduction Continue reduction sintering 3.25h for 950 DEG C in the vacuum atmosphere oven of atmosphere, is elemental copper by remaining cupric oxide powder in-situ reducing, most Copper/aluminium oxide In-situ reaction that void density is 28PPI, aperture 0.72mm, quality of alumina score are 9% is prepared afterwards Cellular material.

Claims (4)

1. a kind of copper/aluminium oxide In-situ reaction cellular material preparation method, it is characterised in that: carry out as follows:
(1) aluminium powder and cupric oxide powder mixed, refining material: are accounted for the 1.3-4.0% of aluminium powder and cupric oxide powder gross mass according to aluminium powder first Ratio be uniformly mixed obtain mixed-powder, then plasticizer and water are accounted for the 25- of plasticizer and water gross mass according to plasticizer 40% ratio is uniformly mixed and obtains mixture, and mixed-powder and mixture are finally accounted for mixed-powder according to mixed-powder and mixed Close the ratio mixing refining material of the 80-86% of object gross mass；
(2) honeycomb structure squeezes: mixing materials prepared by step (1), which are put into compact making hole gap density in porous shunting mold, is 10-20PPI, the honeycomb structure that aperture is 1-2mm；
(3) dry: by step (2) resulting honeycomb structure in 130-160 DEG C of dry 1.25-2h；
(4) vacuum reduction is sintered: the honeycomb structure vacuum reduction after will be dry obtained by step (3) is sintered, and is warming up to first 250-400 DEG C of heat preservation 15-30min then heats to 550-700 DEG C of heat preservation 15-30min and is pre-sintered, be finally warming up to 800-950 DEG C of heat preservation 3.5-5h obtains honeycomb precast body；The vacuum reduction sintering, vacuum degree 10-4-10-2Pa；
(5) hydrogen atmosphere reduction is sintered: the precast body that step (4) is obtained, in a hydrogen atmosphere 800-950 DEG C of sintering 3.25- Copper/aluminium oxide In-situ reaction cellular material is finally made in 4h.
2. copper/aluminium oxide In-situ reaction cellular material preparation method according to claim 1, it is characterised in that: step (1) The cupric oxide powder is the commercially available industrial oxidation copper powder of granularity 200-400 purpose；Aluminium powder is the commercially available technical pure of granularity 400-600 purpose Aluminium powder.
3. copper/aluminium oxide In-situ reaction cellular material preparation method according to claim 1, it is characterised in that: step (1) The plasticizer is polyvinyl alcohol or methylcellulose.
4. copper/aluminium oxide In-situ reaction cellular material preparation method according to claim 1, it is characterised in that: step (5) The hydrogen flowing quantity is 0.25-1L/min.
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CN110744058A (en) * 2019-11-01 2020-02-04 昆明理工大学 Preparation method for in-situ synthesis of copper-based composite material
CN112091207B (en) * 2020-09-10 2024-04-26 安徽德诠新材料科技有限公司 Composite porous copper powder and preparation method and application thereof
CN113458396B (en) * 2021-04-01 2023-05-05 昆明理工大学 Preparation method of copper-based metal honeycomb heat dissipation material

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CN1382816A (en) * 2002-05-30 2002-12-04 昆明理工大学 Process for preparing Cu-Al2O3 composition
CN102631952A (en) * 2012-04-01 2012-08-15 昆明理工大学 Method for preparing iron-based metal honeycomb carrier material

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Publication number Priority date Publication date Assignee Title
CN1382816A (en) * 2002-05-30 2002-12-04 昆明理工大学 Process for preparing Cu-Al2O3 composition
CN102631952A (en) * 2012-04-01 2012-08-15 昆明理工大学 Method for preparing iron-based metal honeycomb carrier material

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