CN102730730B - Submicron Al2O3 fibre and preparation method thereof - Google Patents

Submicron Al2O3 fibre and preparation method thereof Download PDF

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Publication number
CN102730730B
CN102730730B CN201210227025.6A CN201210227025A CN102730730B CN 102730730 B CN102730730 B CN 102730730B CN 201210227025 A CN201210227025 A CN 201210227025A CN 102730730 B CN102730730 B CN 102730730B
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powder
submicron
metal
fiber
preparation
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CN102730730A (en
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李享成
朱伯铨
张品为
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to a submicron Al2O3 fibre and a preparation method thereof. The technical proposal is as follow: 10-60wt% of metal Al powder and 40-90wt% of C powder are used as raw materials, mixed for 5-300min, then placed in ceramic crucible to be calcined for 2-8 hours in inert atmosphere at the temperature of 800-1400 DEG C, and cooled down; then the mixture is calcined for 1-3 hours in air atmosphere at the temperature of 500-1000 DEG C to obtain the submicron Al2O3 fibre. The metal Al powder is selected form more than one kind of analytical reagent of metal Al powder, chemically pure of metal Al powder and industrial metal Al powder, and the granularity is 1-100mum; C powder is selected form more than one kind of graphite powder, carbon black powder, asphalt powder and resin powder, and the granularity of C powder is smaller than 100mum; and the inert atmosphere is argon atmosphere or nitrogen atmosphere. The preparation method provided by the invention has the advantages of simple process and low energy consumption. The prepared submicron Al2O3 fibre not only is high in purity, but also is submicron grade, and is good for subsequent use as additives and reinforcing agents.

Description

A kind of submicron Al 2o 3fiber and preparation method thereof
Technical field
The invention belongs to Al 2o 3fibre technology field.Relate in particular to a kind of submicron Al 2o 3fiber and preparation method thereof.
Background technology
Al 2o 3fiber has high than superior over-all propertieies such as strong, high ratio modulus and high-temperature oxidation resistants, be high performance composite especially high temperature resistant structure ceramics get a good chance of one of strengthening agent with potentiality.But due to Al 2o 3the high susceptibility of whisker growth technique and practical technology fail to break through for a long time, it have been failed so far since coming out the fifties practical.In recent years, along with developing rapidly of high temperature application ceramic base and the research of metal matrix metal whisker composite, people are increasingly urgent to the demand of the high-strength whisker of high-temperature oxidation resistant.
" a kind of preparation method of alumina whisker " (CN200710018539.X) patented technology: aluminum feedstock is mixed according to mol ratio 1:0.25 ~ 1:12 with fusing assistant, roasting 2 ~ 8h at 900 ~ 1200 ℃, cooled sinter obtains product alumina whisker through molten after the operation such as soaking, be dried.The product impurity that this invention generates is more, and mean diameter is 0.5～3 μ m." a kind of method of preparing alumina whisker under low-temperature hydrothermal condition " (CN200810150680.X) patented technology, the method is that aluminum nitrate is dissolved in and in distilled water, is mixed with the solution that concentration is 0.5 ~ 1.5mol/L, in aluminum nitrate solution, add the urea of 2 ~ 10 times of aluminum nitrate molar weights, evenly obtain the colloidal sol of transparent clarification in stirring at normal temperature, then the colloidal sol of preparation is placed in to reactor, under 90 ~ 120 ℃ of conditions, keep 6 ~ 12h, obtain the white depositions of alumina whisker presoma, again by white depositions with after distilled water wash, roasting 2 ~ 12h under 1100 ~ 1300 ℃ of conditions, obtain alumina whisker.This invention complex procedures, reaction is not easy to control, and product mean diameter is 0.5 μ m." a kind of preparation method of hexagonal piece aluminum oxide whisker material " (CN200910117453.1) patented technology, take potassium aluminium sulfate as aluminium source, take vitriol or alkali metal chloride as fusing assistant, roasting at 900～1200 ℃, molten soaking, washing, filters, be dried to obtain hexagonal piece aluminum oxide material, but do not obtain submicron Al 2o 3whisker.This invention complex procedures, contaminate environment, whisker output is little.
Summary of the invention
The present invention is intended to overcome prior art defect, and task is to provide a kind of technique simply and the low submicron Al of energy consumption 2o 3the preparation method of fiber, the submicron Al preparing by the method 2o 3fiber fineness is high, diameter is submicron order and it is follow-up as additive and toughener utilization to be conducive to.
For completing above-mentioned task, the technical solution adopted in the present invention is: be first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 10 ~ 60wt% and 40 ~ 90wt%, be placed in ceramic crucible, under 800 ~ 1400 ℃ of conditions, calcination 2 ~ 8 hours in inert atmosphere, cooling again; Then under 500 ~ 1000 ℃ of conditions and in air atmosphere, calcine 1 ~ 3 hour except C, make submicron Al 2o 3fiber.
In technique scheme: metal A l powder is more than one in analytical pure metal A l powder, chemical pure metal A l powder, Industrial Metal Al powder, and granularity is 1 ~ 100 μ m; C powder is more than one in Graphite Powder 99, carbon powder, asphalt powder, resin-oatmeal, the granularity ﹤ 100 μ m of C powder; Inert atmosphere is argon gas atmosphere or nitrogen atmosphere.
Owing to adopting technique scheme, the present invention utilizes carbothermic method to prepare submicron Al 2o 3fiber, under protection of inert gas, only has micro-oxygen to infiltrate; And under the protection of C, metal A l reacts with trace oxygen and generates high price aluminum oxide steam, with VLS (solid gas-liquid-) principle reaction generation submicron Al 2o 3fiber.This method tool has the following advantages: whole technical process is only through mixing, burning till and de-carbon three steps, therefore technical process is simple; Can synthesizing submicron Al in the scope of 800 ~ 1400 ℃ 2o 3fiber, each synthetic soaking time is only 2 ~ 8 hours, and soaking time is shorter, and energy consumption is low; Synthetic submicron Al 2o 3fiber aluminum contained compound thing only has Al mutually 2o 3, therefore purity is high; Synthetic submicron Al 2o 3fibre diameter is 50nm ~ 1 μ m.
Therefore, the present invention has technique simply and the low feature of energy consumption, prepared submicron Al 2o 3fiber not only purity is high and be submicron order, is conducive to follow-up as additive and toughener utilization.
Accompanying drawing explanation
Fig. 1 is the prepared a kind of submicron Al of the present invention 2o 3the X ray diffracting spectrum of fiber;
Fig. 2 is submicron Al described in Fig. 1 2o 3the electron scanning micrograph of fiber.
Embodiment
Now the present invention will be further described with embodiment by reference to the accompanying drawings, not limiting the scope of the present invention.
For avoiding repetition, first the raw material granularity unification of this embodiment is described below, in following embodiment, repeat no more:
The granularity of metal A l powder is 1 ~ 100 μ m; The granularity ﹤ 100 μ m of C powder.
embodiment 1
A kind of submicron Al 2o 3fiber and preparation method thereof.Be first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 10 ~ 35wt% and 65 ~ 90wt%, be placed in again in ceramic crucible, calcination 2 ~ 5 hours in inert atmosphere under 800 ~ 1100 ℃ of conditions, cooling, then under 500 ~ 1000 ℃ of conditions and in air atmosphere, calcine 1 ~ 3 hour except C, make submicron Al 2o 3fiber.
In the present embodiment: metal A l powder is analytical pure metal A l powder; C powder is Graphite Powder 99; Inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 50nm ~ 100nm.
embodiment 2
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 1.
In the present embodiment: metal A l powder is chemical pure metal A l powder; C powder is carbon powder; Inert atmosphere is nitrogen atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 50nm ~ 120nm.
embodiment 3
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 1.
In the present embodiment: metal A l powder is Industrial Metal Al powder; C powder is asphalt powder; Inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 70nm ~ 200nm.
embodiment 4
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 1.
In the present embodiment: metal A l powder is analytical pure metal A l powder and chemical pure metal A l powder; C powder is resin-oatmeal; Inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 50nm ~ 100nm.
embodiment 5
A kind of submicron Al 2o 3fiber and preparation method thereof.Be first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 35 ~ 60wt% and 40 ~ 65wt%, then be placed in ceramic crucible, under 1100 ~ 1400 ℃ of conditions, calcination 5 ~ 8 hours in inert atmosphere, cooling; Then under 500 ~ 1000 ℃ of conditions and in air atmosphere, calcine 1 ~ 3 hour except C, make submicron Al 2o 3fiber.
In the present embodiment: metal A l powder is Industrial Metal Al powder and chemical pure metal A l powder; C powder is Graphite Powder 99 and carbon powder; Inert atmosphere is nitrogen atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 200nm ~ 500nm.
embodiment 6
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 5.
In the present embodiment: metal A l powder is Industrial Metal Al powder and analytical pure metal A l powder; C powder is asphalt powder and carbon powder; Inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 200nm ~ 400nm.
embodiment 7
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 5.
In the present embodiment: metal A l powder is Industrial Metal Al powder, analytical pure metal A l powder and chemical pure metal A l powder; C powder is asphalt powder and resin-oatmeal; Inert atmosphere is nitrogen atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 600nm ~ 800nm.
embodiment 8
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 5.
In the present embodiment: metal A l powder is analytical pure metal A l powder and chemical pure metal A l powder; C powder is Graphite Powder 99 and resin-oatmeal; Inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 400nm ~ 600nm.
embodiment 9
A kind of submicron Al 2o 3fiber and preparation method thereof.Be first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 35 ~ 60wt% and 40 ~ 65wt%, then be placed in ceramic crucible, under 800 ~ 1100 ℃ of conditions, calcination 5 ~ 8 hours in inert atmosphere, cooling; Then under 500 ~ 1000 ℃ of conditions and in air atmosphere, calcine 1 ~ 3 hour except C, make submicron Al 2o 3fiber.
In the present embodiment: metal A l powder is analytical pure metal A l powder and chemical pure metal A l powder, and C powder is Graphite Powder 99, carbon powder and asphalt powder, and inert atmosphere is nitrogen atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 200nm ~ 300nm.
embodiment 10
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 9.
In the present embodiment: metal A l powder is analytical pure metal A l powder and Industrial Metal Al powder, and C powder is resin-oatmeal, carbon powder and asphalt powder, and inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 150nm ~ 250nm.
embodiment 11
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 9.
In the present embodiment: metal A l powder is analytical pure metal A l powder and Industrial Metal Al powder, and C powder is resin-oatmeal, Graphite Powder 99 and asphalt powder, and inert atmosphere is nitrogen atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 100nm ~ 250nm.
embodiment 12
A kind of submicron Al 2o 3fiber and preparation method thereof.Except raw material and inert atmosphere, all the other are with embodiment 9.
In the present embodiment: metal A l powder is chemical pure metal A l powder and Industrial Metal Al powder, and C powder is resin-oatmeal, Graphite Powder 99 and carbon powder, and inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 100nm ~ 350nm.
embodiment 13
A kind of submicron Al 2o 3fiber and preparation method thereof.Be first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 10 ~ 35wt% and 65 ~ 90wt%, then be placed in ceramic crucible, under 1100 ~ 1400 ℃ of conditions, calcination 2 ~ 5 hours in inert atmosphere, cooling; Then under 500 ~ 1000 ℃ of conditions and in air atmosphere, calcine 1 ~ 3 hour except C, make submicron Al 2o 3fiber.
In the present embodiment: metal A l powder is analytical pure metal A l powder and chemical pure metal A l powder, and C powder is Graphite Powder 99, carbon powder, asphalt powder and resin-oatmeal, and inert atmosphere is argon gas atmosphere.
The submicron Al that the present embodiment is prepared 2o 3fibre diameter is 800nm ~ 1 μ m.
This embodiment utilizes carbothermic method to prepare submicron Al 2o 3fiber, under protection of inert gas, only has micro-oxygen to infiltrate; And under the protection of C, metal A l reacts with trace oxygen and generates high price aluminum oxide steam, with VLS (solid gas-liquid-) principle reaction generation submicron Al 2o 3fiber.This method tool has the following advantages: whole technical process is only through mixing, burning till and de-carbon three steps, therefore technical process is simple; Can synthesizing submicron Al in the scope of 800 ~ 1400 ℃ 2o 3fiber, each synthetic soaking time is only 2 ~ 8 hours, and soaking time is shorter, and energy consumption is low; Synthetic submicron Al 2o 3fiber as shown in Figure 1 aluminum contained compound thing only has Al mutually 2o 3, therefore purity is high; Synthetic submicron Al as shown in Figure 2 2o 3fibre diameter is 50nm ~ 1 μ m.
Therefore, this embodiment has technique simply and the low feature of energy consumption, prepared submicron Al 2o 3fiber not only purity is high and be submicron order, is conducive to follow-up as additive and toughener utilization.

Claims (4)

1. a submicron Al 2o 3the preparation method of fiber, is characterized in that being first that raw material mixes 5 ~ 300min by the C powder of the metal A l powder of 10 ~ 60wt% and 40 ~ 90wt%, then is placed in ceramic crucible, under 800 ~ 1400 ℃ of conditions, calcines 2 ~ 8 hours in inert atmosphere, cooling; Then under 500 ~ 1000 ℃ of conditions He in air atmosphere, calcine 1 ~ 3 hour, make submicron Al 2o 3fiber.
2. submicron Al according to claim 1 2o 3the preparation method of fiber, is characterized in that described metal A l powder is more than one in analytical pure metal A l powder, chemical pure metal A l powder, Industrial Metal Al powder, and granularity is 1 ~ 100 μ m.
3. submicron Al according to claim 1 2o 3the preparation method of fiber, is characterized in that described C powder is more than one in Graphite Powder 99, carbon powder, asphalt powder, resin-oatmeal, the granularity ﹤ 100 μ m of C powder.
4. submicron Al according to claim 1 2o 3the preparation method of fiber, is characterized in that described inert atmosphere is argon gas atmosphere or nitrogen atmosphere.
CN201210227025.6A 2012-07-03 2012-07-03 Submicron Al2O3 fibre and preparation method thereof Expired - Fee Related CN102730730B (en)

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CN113502596B (en) * 2021-06-28 2022-09-02 南通大学 Self-supporting MgTiO 3 Nano fiber chemical warfare agent degradation material and preparation method thereof
CN113502599B (en) * 2021-06-28 2022-09-02 南通大学 Flexible Y 2 Mo 3 O12/Al 2 O 3 High-temperature heat-insulation nanofiber membrane and preparation method thereof
CN113502598B (en) * 2021-06-28 2022-09-02 南通大学 Flexible MgAl for chemical warfare agent digestion 2 O 4 Preparation method of nanofiber membrane

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Publication number Priority date Publication date Assignee Title
CN1203209A (en) * 1998-07-24 1998-12-30 清华大学 Process for preparing aluminium nitride whisker
CN1775975A (en) * 2005-09-29 2006-05-24 陕西科技大学 Method for preparing Al 203 fiber-reinforced TiAl3 base composite material
CN102226298A (en) * 2011-06-17 2011-10-26 北京理工大学 Preparation method of metal oxide nanowires

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1203209A (en) * 1998-07-24 1998-12-30 清华大学 Process for preparing aluminium nitride whisker
CN1775975A (en) * 2005-09-29 2006-05-24 陕西科技大学 Method for preparing Al 203 fiber-reinforced TiAl3 base composite material
CN102226298A (en) * 2011-06-17 2011-10-26 北京理工大学 Preparation method of metal oxide nanowires

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