CN115121797B - Preparation method of porous aluminum composite plate - Google Patents

Preparation method of porous aluminum composite plate Download PDF

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Publication number
CN115121797B
CN115121797B CN202210689860.5A CN202210689860A CN115121797B CN 115121797 B CN115121797 B CN 115121797B CN 202210689860 A CN202210689860 A CN 202210689860A CN 115121797 B CN115121797 B CN 115121797B
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sintering
powder
aluminum alloy
aluminum
porous aluminum
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CN115121797A (en
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张爵灵
王林山
王蕊
郑逢时
梁雪冰
胡强
汪礼敏
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Beijing Youyan Powder New Materials Research Institute Co ltd
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Beijing Youyan Powder New Materials Research Institute Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/005Loading or unloading powder metal objects

Abstract

The invention relates to a preparation method of a porous aluminum composite board, which comprises the following steps: the method comprises the steps of taking potassium fluoroaluminate and Al12Si as sintering aids, uniformly mixing aluminum powder and the sintering aids, putting the mixed powder into a graphite mold, covering an aluminum alloy plate on the graphite mold, inverting or putting the mixed powder into a concave aluminum alloy plate to obtain a combined structure, sintering the combined structure, and controlling the grain size of the aluminum powder, the content of the sintering aids and sintering parameters to obtain the porous aluminum composite plate with certain porosity. The invention solves the technical problems of high preparation cost, complex process and the like in the prior art, and has simple process, lower cost, controllable pore size and porosity of porous aluminum and higher reliability.

Description

Preparation method of porous aluminum composite plate
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of a porous aluminum composite plate.
Background
The porous aluminum alloy has the excellent properties of low density, large specific surface area, high specific stiffness, high damping performance, high impact energy absorptivity and the like, and the porous aluminum and the metal plate are compounded to improve the service performance, so that the porous aluminum alloy has wide application prospect in the fields of aerospace, 3C and the like.
The pore size and pore shape of the porous aluminum alloy have a great influence on the structure and performance. The existing preparation methods include a seepage casting method, a melt foaming method, a non-water-based gel sol method, a discharge plasma sintering method and the like, but the porous aluminum materials which simultaneously meet the requirements of small pore diameter, high porosity, controllable pore diameter distribution, small thermal resistance, low cost and complex shape cannot be prepared by adopting the methods.
Current methods of compounding porous aluminum with sheet metal include brazing, rolling, and the like. The Chinese patent application publication No. CN112677621A discloses a preparation method for pressing a porous aluminum plate onto a metal plate by rolling, wherein the composite plate metal prepared by the method and the porous aluminum plate have higher connection strength, but the preparation method is complex, the pore diameter and the pore shape of the porous aluminum cannot be controlled, and the composite plate prepared by adopting a brazing method can increase interface contact thermal resistance.
Disclosure of Invention
In order to solve the technical problems of high preparation cost, complex process and the like in the prior art, the invention provides the preparation method of the porous aluminum composite board, which has the advantages of simple operation method, controllable pore size and porosity of the porous aluminum, low cost and higher reliability.
The invention provides a preparation method of a porous aluminum composite board, which comprises the following steps:
1) Raw materials: selecting aluminum powder with the granularity range of 1-200 mu m, and mixing the aluminum powder with a sintering aid to obtain uniformly mixed powder, wherein the sintering aid is a mixture of potassium fluoroaluminate powder and Al12Si powder;
2) Filling: the loading mode can be any one of the following two modes:
a) Filling the mixed powder into a graphite mold, coating an aluminum alloy plate on the surface of the graphite mold, and inverting the aluminum alloy plate and the graphite mold to obtain a combined structure;
b) Filling the mixed powder into a concave aluminum alloy plate to obtain a combined structure;
3) Sintering: and sintering the combined structure in an anti-oxidation environment, and cooling along with a furnace after sintering is finished to obtain the porous aluminum composite plate, wherein the mixed powder is converted into porous aluminum through sintering.
Preferably, the particle size of the aluminum powder is in the range of 20 to 150 μm.
Preferably, after sintering, the preparation method further comprises: and (3) washing the obtained porous aluminum composite board with dilute nitric acid to remove residual potassium fluoroaluminate, and then washing with alcohol and drying.
In step 1), the sintering aid is a mixture of potassium fluoroaluminate powder and Al12Si powder. The potassium fluoroaluminate has the function of removing an oxide film on the surface of aluminum powder, wherein the melting point of Al12Si is lower than that of pure Al, liquid phase sintering is formed during sintering, the brazing flux activity of the potassium fluoroaluminate is increased, and the sintering is promoted.
Preferably, the aluminum powder may be pure aluminum powder.
Preferably, the mass ratio of the aluminum powder to the sintering aid is 6: 1-3:1. The porosity and pore size of the porous aluminum alloy can be controlled by adjusting the addition amount of the sintering additive.
Preferably, the sintering aid has a powder particle size in the range of 1-100 μm, preferably 1-45 μm. The smaller the powder granularity of the sintering aid is, the smaller the addition content is, the uniformity of the mixing of the sintering aid can be ensured, and the sintering activity is larger.
Preferably, the potassium fluoroaluminate powder is added in a proportion of 5 to 15%, for example 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 15%, based on the total weight of the mixed powder. Preferably, the Al12Si powder is added in a proportion of 5 to 15%, such as 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 15%, based on the total weight of the mixed powder.
Preferably, in the sintering aid, the mass ratio of potassium fluoroaluminate powder to Al12Si powder may be 3:1 to 1:3, for example, may be 3:1, 2:1, 1:1, 1:2 or 1:3.
Preferably, sintering may be performed in a sintering furnace. Preferably, the sintering temperature may be 590 to 620 ℃, for example 590 ℃, 600 ℃, 610 ℃ or 620 ℃. Preferably, the sintering time may be 40 to 480min, preferably 40 to 100min. Preferably, the temperature is raised to the sintering temperature at a rate of 10 to 20 ℃/min. For example, the heating rate may be 10 ℃/min, 11 ℃/min, 12 ℃/min, 13 ℃/min, 14 ℃/min, 15 ℃/min, 16 ℃/min, 17 ℃/min, 18 ℃/min, 19 ℃/min, or 20 ℃/min.
Preferably, in step a), the aluminum alloy sheet is a flat sheet.
Preferably, in step b), the aluminum alloy sheet of concave shape comprises a concave structure. The concave structure may be circular or polygonal. The shape of the concave structure is not particularly limited as long as the mixed powder can be contained.
Preferably, the aluminum alloy plate is made of aluminum alloy with an overburning temperature of 580 ℃ or higher. The aluminum alloy plate can be 1060 aluminum alloy plate, 3003 aluminum alloy plate or 6063 aluminum alloy plate.
Preferably, in step 3), the oxidation preventing environment may be vacuum, a reducing atmosphere or an inert protective atmosphere. The reducing atmosphere can be one of hydrogen, carbon monoxide and nitrogen-hydrogen mixed gas. The inert protective atmosphere can be one of nitrogen, argon and helium.
The invention also provides a porous aluminum composite board, which is obtained by the preparation method.
Preferably, the porous aluminum in the porous aluminum alloy composite panel may have a porosity of 10% -70%, for example, 10%, 20%, 30%, 40%, 50%, 60% or 70%.
Preferably, the compressive strength of the porous aluminum alloy composite panel may be 15MPa or more.
Preferably, the maximum pore diameter of the porous aluminum in the porous aluminum alloy composite plate can be 5-50 μm, preferably 10-45 μm; the permeability can be 1X 10 -15 ~1×10 -10 m 2
Compared with the prior art, the invention has the advantages that:
1. according to the invention, potassium fluoroaluminate and Al12Si are used as sintering aids, and the porous aluminum or aluminum alloy plate with complex shape can be prepared under the condition of pressureless sintering. Because potassium fluoroaluminate is corrosion-free, the potassium fluoroaluminate does not need to be removed after sintering, and the problems that pore-forming agent residues, irregular pore shapes, influence on a matrix in the removal process and the like are solved.
2. The invention can control the porosity and pore size of the porous aluminum alloy by adjusting the addition amount of the sintering additive.
3. According to the invention, the porous aluminum composite plate is formed at one time, and the defect of increased contact thermal resistance caused by brazing is avoided under the condition of ensuring the reliability of materials.
4. The invention has simple process, flexible operation and lower cost.
Drawings
Fig. 1 is a scanning electron microscope photograph of porous aluminum in the porous aluminum composite panel prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope photograph of porous aluminum in the porous aluminum composite panel prepared in example 2 of the present invention.
Fig. 3 is a scanning electron microscope photograph of porous aluminum in the porous aluminum composite panel prepared in example 3 of the present invention.
FIG. 4 is a metallographic photograph of a section at an interface of porous aluminum and an aluminum alloy sheet in the porous aluminum composite panel prepared in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. It should be further noted that, for convenience of description, only some, but not all of the drawings related to the present invention are shown.
Example 1
The method comprises the steps of adopting a mixture of potassium fluoaluminate and Al12Si as a sintering aid (the particle size range is 1-45 mu m), and uniformly mixing Al powder with the particle size range of 74-150 mu m with the sintering aid to obtain mixed powder, wherein the mass fraction of the potassium fluoaluminate is 10%, the mass fraction of the Al12Si is 5% and the mass fraction of the Al powder is 85% based on the total weight of the mixed powder. Filling the mixed powder into a graphite mold, covering the 1060 aluminum alloy plate on the graphite mold, inverting the aluminum alloy plate and the graphite mold, placing the aluminum alloy plate and the graphite mold into a tubular sintering furnace, introducing nitrogen for 30min, sintering under the protection of nitrogen atmosphere, wherein the temperature rising rate is 10 ℃/min, the sintering temperature is 590 ℃ and the sintering time is 40min, and obtaining the porous aluminum composite plate, wherein the mixed powder is converted into porous aluminum through sintering, and the porosity of the porous aluminum is about 50%.
The product obtained in example 1 was subjected to compression performance test, and the compression strength was 15MPa, the maximum pore diameter was 43 μm, and the permeability was 4.7X10 -11 m 2
A scanning electron micrograph of the porous aluminum in the porous aluminum composite plate obtained in example 1 is shown in FIG. 1. A metallographic photograph of a section at the interface of the porous aluminum and the aluminum alloy plate is shown in FIG. 4.
Example 2
The method comprises the steps of adopting a mixture of potassium fluoaluminate and Al12Si as a sintering aid (the particle size range is 1-45 mu m), uniformly mixing Al powder with the particle size range of 45-74 mu m with the sintering aid to obtain mixed powder, wherein the mass fraction of the potassium fluoaluminate is 10%, the mass fraction of the Al12Si is 5% and the mass fraction of the Al powder is 85% based on the total weight of the mixed powder. And filling the mixed powder into 3003 aluminum alloy plates which are concave plates to obtain a combined structure. And (3) placing the combined structure into a tubular sintering furnace, introducing nitrogen for 30min, sintering under the protection of nitrogen atmosphere, wherein the heating rate is 10 ℃/min, the sintering temperature is 600 ℃, and the sintering time is 60min, so as to obtain the porous aluminum composite board, wherein the mixed powder is converted into porous aluminum through sintering, and the porosity of the porous aluminum is about 49.38%.
The product obtained in example 2 was subjected to compression performance test, and the compression strength was 20MPa, the maximum pore diameter was 37. Mu.m, and the permeability was 6.016X 10 -12 m 2
A scanning electron micrograph of the porous aluminum in the porous aluminum composite plate obtained in example 2 is shown in FIG. 2.
The product developed in example 2 can be used for heat dissipating components.
Example 3
The method comprises the steps of adopting a mixture of potassium fluoaluminate and Al12Si as a sintering aid (with the particle size range of 1-45 mu m), and uniformly mixing Al powder with the particle size range of 20-45 mu m with the sintering aid to obtain mixed powder, wherein the mass fraction of the potassium fluoaluminate is 10%, the mass fraction of the Al12Si is 10% and the mass fraction of the Al powder is 80% based on the total weight of the mixed powder. Filling the mixed powder into a graphite mold, covering the graphite mold with 6063 aluminum alloy plate, inverting the aluminum alloy plate and the graphite mold, placing into a tubular sintering furnace, introducing nitrogen for 30min, sintering under the protection of nitrogen atmosphere, wherein the temperature rising rate is 15 ℃/min, the sintering temperature is 620 ℃ and the sintering time is 90min, and obtaining the porous aluminum composite plate, wherein the mixed powder is converted into porous aluminum through sintering, and the porosity of the porous aluminum is about 25%.
The product obtained in example 3 was used as a treatment object, and compression performance test was performed on the product, and when the compressive strength reached 70MPa, the sample did not break, and the pressure was continuously increased until the compressive strength could not be measured, and the sample still did not break. As can be seen from the above, the compressive strength was 70MPa or more. The maximum pore diameter is 12 μm, and the permeability is 4.30X10 -14 m 2
A scanning electron micrograph of the porous aluminum in the porous aluminum composite plate obtained in example 3 is shown in FIG. 3.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the porous aluminum composite board is characterized by comprising the following steps of:
1) Raw materials: selecting aluminum powder with the granularity range of 1-200 mu m, and mixing the aluminum powder with a sintering aid to obtain uniformly mixed powder, wherein the sintering aid is a mixture of potassium fluoroaluminate powder and Al12Si powder;
2) Filling: the loading mode can be any one of the following two modes:
a) Filling the mixed powder into a graphite mold, coating an aluminum alloy plate on the surface of the graphite mold, and inverting the aluminum alloy plate and the graphite mold to obtain a combined structure;
b) Filling the mixed powder into a concave aluminum alloy plate to obtain a combined structure;
3) Sintering: sintering the combined structure in an anti-oxidation environment, and cooling along with a furnace after sintering is finished to obtain a porous aluminum composite plate, wherein the mixed powder is converted into porous aluminum through sintering;
the mass ratio of the aluminum powder to the sintering aid is 6: 1-3: 1.
2. the preparation method according to claim 1, wherein the sintering temperature is 590-620 ℃; heating to the sintering temperature at a heating rate of 10-20 ℃/min; the sintering time is 40-480 min.
3. The method of claim 1, wherein the sintering aid has a powder particle size in the range of 1-100 μm.
4. A method of preparation according to claim 3, characterized in that the sintering aid has a powder particle size in the range of 1-45 μm.
5. The production method according to claim 1, wherein the addition ratio of the potassium fluoroaluminate powder is 5 to 15% and the addition ratio of the Al12Si powder is 5 to 15% based on the total weight of the mixed powder.
6. The method of claim 1, wherein in step a), the aluminum alloy sheet is a flat sheet.
7. The method according to claim 1, wherein the aluminum alloy plate is made of an aluminum alloy having an overburning temperature of 580 ℃ or higher; the aluminum alloy plate can be 1060 aluminum alloy plate, 3003 aluminum alloy plate or 6063 aluminum alloy plate.
8. The method according to claim 1, wherein in step 3), the oxidation-preventing atmosphere is vacuum, a reducing atmosphere or a protective atmosphere; the reducing atmosphere is one of hydrogen, carbon monoxide and nitrogen-hydrogen mixed gas; the protective atmosphere is one of nitrogen, argon and helium.
9. A porous aluminum composite panel, characterized by being obtained by the production method according to any one of claims 1 to 8.
10. The porous aluminum composite panel according to claim 9, wherein the porous aluminum in the porous aluminum composite panel has a porosity of 10% -70%.
CN202210689860.5A 2022-06-17 2022-06-17 Preparation method of porous aluminum composite plate Active CN115121797B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1990006204A1 (en) * 1988-11-28 1990-06-14 Furukawa Aluminum Co., Ltd Gaseous phase brazing method of al or al alloy
CN102365143A (en) * 2009-03-30 2012-02-29 三菱综合材料株式会社 Process for producing porous sintered aluminum, and porous sintered aluminum
CN102458725A (en) * 2009-06-04 2012-05-16 三菱综合材料株式会社 Process for production of aluminum complex comprising sintered porous aluminum body
CN106583739A (en) * 2016-12-02 2017-04-26 北京有色金属研究总院 Aluminum foam sandwich plate with gradient interface and manufacturing method thereof
CN112122611A (en) * 2020-09-25 2020-12-25 航天特种材料及工艺技术研究所 Foam aluminum with sandwich structure and preparation method thereof
CN114131028A (en) * 2021-12-02 2022-03-04 广东省科学院新材料研究所 Aluminum-based porous composite sandwich structure and preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1990006204A1 (en) * 1988-11-28 1990-06-14 Furukawa Aluminum Co., Ltd Gaseous phase brazing method of al or al alloy
CN102365143A (en) * 2009-03-30 2012-02-29 三菱综合材料株式会社 Process for producing porous sintered aluminum, and porous sintered aluminum
CN102458725A (en) * 2009-06-04 2012-05-16 三菱综合材料株式会社 Process for production of aluminum complex comprising sintered porous aluminum body
CN106583739A (en) * 2016-12-02 2017-04-26 北京有色金属研究总院 Aluminum foam sandwich plate with gradient interface and manufacturing method thereof
CN112122611A (en) * 2020-09-25 2020-12-25 航天特种材料及工艺技术研究所 Foam aluminum with sandwich structure and preparation method thereof
CN114131028A (en) * 2021-12-02 2022-03-04 广东省科学院新材料研究所 Aluminum-based porous composite sandwich structure and preparation method and application thereof

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