CN108640660A - A method of preparing foamed alumina and foamed aluminium/alumina composite material - Google Patents

A method of preparing foamed alumina and foamed aluminium/alumina composite material Download PDF

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Publication number
CN108640660A
CN108640660A CN201810384689.0A CN201810384689A CN108640660A CN 108640660 A CN108640660 A CN 108640660A CN 201810384689 A CN201810384689 A CN 201810384689A CN 108640660 A CN108640660 A CN 108640660A
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foamed
aluminium
alumina
composite material
prepared
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CN108640660B (en
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杨金龙
霍文龙
张笑妍
干科
陈谷雨
席小庆
王亚利
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New Mstar Technology Ltd (tianjin) New Mstar Technology Ltd
Tsinghua University
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New Mstar Technology Ltd (tianjin) New Mstar Technology Ltd
Tsinghua University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • B22F3/11Making porous workpieces or articles
    • B22F3/1121Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1125Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers involving a foaming process
    • 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
    • B22F3/11Making porous workpieces or articles
    • B22F3/1143Making porous workpieces or articles involving an oxidation, reduction or reaction step
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/10Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40Metallic constituents or additives not added as binding phase
    • C04B2235/402Aluminium
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562Heating rate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention develops a kind of method preparing foamed alumina aluminium and foamed aluminium/alumina composite material by reaction-sintered metallic aluminium near net-shape, and this method comprises the following steps:Using metallic aluminium powder as material powder, the metallic aluminium water-based slurry that total solid concentration is 10~50wt% is prepared.Lauryl sodium sulfate (SDS) of the 0.02~0.4wt% of stock quality as surfactant is added in above-mentioned slurry, adjusts pH to 5~8.Slurry is foamed by mechanical agitation mode to obtain stable foam, is sintered after dry and can get foamed alumina and foamed aluminium/alumina composite material.It is to be accumulated by hollow ball that the foaming structure, which has hierarchical porous structure, hole wall,.Preparation process of the present invention is simple, of low cost, can prepare the composite material of different aluminum/alumina composition.Prepared foamed material has the characteristics that near-net-shape, sintering shrinkage are only 5~5%.

Description

A method of preparing foamed alumina and foamed aluminium/alumina composite material
Technical field
The present invention relates to metal/ceramic composite, multi-stage porous foamed material, hollow ball material, near-net-shape materials The preparation of material, and in particular to one kind preparing foamed aluminium and foamed aluminium/alumina composite by reaction-sintered metallic aluminium near net-shape The method of material.
Background technology
The advantages of porous oxide Ceramic bond foamed material and oxide ceramics, has heat preservation heat-insulating property good, close Spend small, many features such as chemical stabilization under high temperature resistant, the corrosion-resistant, condition of high temperature.With the rapid development of modern industry, especially The progress of high-tech proposes increasingly higher demands to the Good All-around Property of material.Metal/ceramic composite is because of knot Close both the advantages of and become a kind of important composite material.However how to realize that uniform compound be still filled with of two kinds of materials is chosen War.
On the other hand, in sintering process there is very big contraction in ceramic material, and especially high pore foam ceramic is shunk Rate is up to 20%, therefore be easy to cause the strain cracking of sample.How to prepare lower shrinkage near net-shape and prepares foamed ceramics always Since be all a problem.
Invention content
For above-mentioned background technology there are the problem of, the present invention develop one kind by reaction-sintered metallic aluminium near net-shape The method for preparing foamed aluminium and foamed aluminium/alumina composite material.Prepared foamed material has the characteristics that near net-shape, burns It is only -5~5% to tie shrinking percentage.On the one hand ultralow shrinking percentage is since reaction-sintered expands, more important is due to metallic aluminium Powder diffuses to form hollow structure outward after melting.Further, preparation process is simple, of low cost, without at high price Production equipment, have potential using value.
The present invention is as follows using technology path:
It is a kind of that foamed alumina and foamed aluminium/alumina composite material are prepared by reaction-sintered metallic aluminium near net-shape Method, described method includes following steps:
(1) metallic aluminium powder for being 0.3~5 μm using particle size range is material powder, prepare total solid concentration be 10~ The metallic aluminium water-based slurry of 50wt%.
(2) dodecyl sulphates of the 0.02~0.4wt% of stock quality as surfactant is added in above-mentioned slurry Sodium (SDS) adjusts pH to 5~8.
(3) slurry is foamed by mechanical agitation mode to obtain stable foam, rotating speed is 1200~5000rmp.Institute The time for stating stirring is 5-20 minutes.
(4) dry body after drying is sintered in air atmosphere, 700 are heated to 0.5~2 DEG C/min heating rates~ 1500 DEG C, keep the temperature 0.5~5h.The time of the drying is 5-40h, obtains dry body
Foamed material prepared by the present invention had both had the level-one macro pore structure based on tens microns of hole-closing structures, simultaneously With the second hole structure hole wall made of hollow ball accumulation closely.
The controllable adjustment to foamed alumina and foamed aluminium/alumina composition may be implemented by regulating and controlling sintering temperature, when Foamed aluminium/alumina composite material can be obtained when being 650~900 DEG C in sintering temperature, when sintering temperature is more than 1200 DEG C, metal Aluminium is completely converted into aluminium oxide, foamed alumina ceramic hollow ball foamed material is prepared, therefore the present invention can both be prepared Aluminium/alumina composite foamed material, can also prepare Alumina Foam Ceramics.
Prepared foamed material has the characteristics that near net-shape, sintering shrinkage are only -5~5%.
The beneficial effects of the invention are as follows:1. the foamed material hole wall prepared by this method be accumulated by hollow sphere powder and At effectively reducing the unit weight of foamed material, improve heat-insulating property and toughness.2. may be implemented by regulating and controlling sintering temperature To the controllable adjustment of aluminium/alumina composition.3. each production link of this method does not generate poisonous and harmful substances, environmental-friendly, and Its preparation process is simple, of low cost, is not necessarily to expensive production equipment.4. prepared foamed material has near net-shape special Point, sintering shrinkage are only 0~5%, effectively inhibit cracking and the deformation of sample.
Description of the drawings
Fig. 1 be the embodiment of the present invention 1 prepare foamed aluminium/alumina composite material photomacrograph (left side is sintered body, Right side is green body).
Fig. 2 is the SEM photograph of foamed aluminium/alumina composite material prepared by the embodiment of the present invention 1, it is shown that uniform one Grade pore structure.
Fig. 3 is the SEM photograph of foamed aluminium/alumina composite material prepared by the embodiment of the present invention 1, it is shown that hole wall is hollow Structure.
Specific implementation mode
With reference to the accompanying drawings and examples, the present invention is described in more detail.
Embodiment 1
(1) it is 40wt% metal aluminum slurries to prepare solid concentration, and the lauryl sodium sulfate of 0.04wt% is added, then uses Hydrochloric acid and ammonium hydroxide adjust pH to 6.8.
(2) foaming 10min is stirred under 2000rmp rotating speeds using machine mixer and obtains stable ceramic foam slurry, Obtain overstable foam as shown in Figure 2.Dry 18h, obtains dry body.
(3) green body is heated to 800 DEG C with 1 DEG C/min heating rates, keeps the temperature 2h.
(4) foamed aluminium/alumina composite material shrinking percentage prepared by is less than 1%, photomacrograph as shown in Figure 1, its Middle left side sample is sintered body, and right side sample is green body, it can be seen that the length of sample is almost without any difference after sintering. Sample microstructure is as shown in Figures 2 and 3.
Technical scheme of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.

Claims (9)

1. a kind of side preparing foamed alumina and foamed aluminium/alumina composite material by reaction-sintered metallic aluminium near net-shape Method, which is characterized in that described method includes following steps:
(1) using metallic aluminium powder as material powder, the metallic aluminium water-based slurry that total solid concentration is 10~50wt% is prepared;
(2) dodecanes of the 0.02~0.4wt% of stock quality as surfactant is added in slurry obtained by step (1) Base sodium sulphate adjusts pH to 5~8;
(3) it foams to slurry obtained by step (2) under mechanical agitation, obtains stable foam, the rotating speed of the stirring For 1200~5000rmp;
(4) it is sintered after being dried for step (3) gains, obtains aluminium oxide and foamed aluminium/alumina composite material.
2. according to the method for claim 1, which is characterized in that the particle size range of step (1) described metallic aluminium powder be 0.3~ 5μm。
3. according to method as claimed in claim 1 or 2, which is characterized in that the time stirred described in step (3) is 5-20 points Clock.
4. according to method as claimed in claim 1 or 2, which is characterized in that the dry time is 5-40h described in step (4), is obtained To dry body.
5. according to method as claimed in claim 1 or 2, which is characterized in that the atmosphere being sintered described in step (4) is air, is burnt Knot heating rate is 0.5~2 DEG C/min, is warming up to 700~1500 DEG C, keeps the temperature 0.5~5h.
6. according to method as claimed in claim 1 or 2, which is characterized in that by regulating and controlling sintering temperature realization pair in step (4) The controllable adjustment of aluminium/alumina composition, the temperature of the sintering obtain foamed aluminium/alumina composite material when being 650~900 DEG C Material, when the temperature of the sintering is more than 1200 DEG C, metallic aluminium is completely converted into aluminium oxide, and hollow ball foamed alumina is prepared Ceramics.
7. according to method as claimed in claim 1 or 2, which is characterized in that prepared foamed material has the characteristics that near net-shape, Its sintering shrinkage is only -5~5%.
8. according to method as claimed in claim 1 or 2, which is characterized in that prepared foamed material, which has, can be achieved negative contraction, That is, the characteristics of sintering grow.
9. according to method as claimed in claim 1 or 2, which is characterized in that prepared foamed material is tied with new multistage hole Structure had both had the level-one macro pore structure based on tens microns of hole-closing structures, while having and closely being formed by hollow ball accumulation Second hole structure hole wall.
CN201810384689.0A 2018-04-26 2018-04-26 Method for preparing foamed aluminum oxide and foamed aluminum/aluminum oxide composite material Active CN108640660B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110303158A (en) * 2019-08-13 2019-10-08 广西大学 A kind of novel method for preparing foamed aluminium
CN114539978A (en) * 2020-11-26 2022-05-27 中国科学院大连化学物理研究所 Aluminum foam-based composite sizing phase-change material and preparation and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001354793A (en) * 2000-06-12 2001-12-25 Kansai Research Institute Blowing agent
CN101876017A (en) * 2009-12-15 2010-11-03 哈尔滨工业大学 Nano-ceramic particle reinforced aluminum foam matrix composite material and preparation method thereof
CN103898348A (en) * 2014-03-19 2014-07-02 苏州宇希新材料科技有限公司 Method for preparing aluminum foam material
CN104016703A (en) * 2014-06-09 2014-09-03 清华大学 Preparation method of superlight closed-pore ceramic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001354793A (en) * 2000-06-12 2001-12-25 Kansai Research Institute Blowing agent
CN101876017A (en) * 2009-12-15 2010-11-03 哈尔滨工业大学 Nano-ceramic particle reinforced aluminum foam matrix composite material and preparation method thereof
CN103898348A (en) * 2014-03-19 2014-07-02 苏州宇希新材料科技有限公司 Method for preparing aluminum foam material
CN104016703A (en) * 2014-06-09 2014-09-03 清华大学 Preparation method of superlight closed-pore ceramic

Non-Patent Citations (1)

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Title
WENLONG HUO ET AL.: "Mechanical strength of highly porous ceramic foams with thin and lamellate cell wall from particle-stabilized foams", 《CERAMICS INTERNATIONAL》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110303158A (en) * 2019-08-13 2019-10-08 广西大学 A kind of novel method for preparing foamed aluminium
CN114539978A (en) * 2020-11-26 2022-05-27 中国科学院大连化学物理研究所 Aluminum foam-based composite sizing phase-change material and preparation and application thereof

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