CN106747447A - One kind synthesis Al4SiC4The new method of powder body material - Google Patents
One kind synthesis Al4SiC4The new method of powder body material Download PDFInfo
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Abstract
Present invention relates particularly to a kind of refractory ceramics Al4SiC4The synthetic method of powder body material.The method by microwave by by the well mixed rear briquetting of raw material, using homemade reactor, Al being synthesized under the protection of inert atmosphere4SiC4Powder.By this method, Al can quickly be prepared4SiC4Ceramic powder, sintering time is greatly shortened, and efficiency improves decades of times compared with traditional ceramics preparation method.Preferably single-phase sample is obtained simultaneously.The inventive method energy saving, production efficiency are high, environment friendly and pollution-free, process is simple, products obtained therefrom purity are higher, with application value very high.
Description
Technical field
Present invention relates particularly to a kind of refractory ceramics Al4SiC4The synthetic method of powder body material.
Background technology
Double carbide carbon silicated aluminum is a kind of compound of new covalent bond, Al4SiC4Ceramics have that fusing point is high, hardness
It is high, intensity is big, electrical and thermal conductivity is good, low-expansion coefficient, anti-oxidant and strong corrosion resistance the features such as, therefore in refractory material row
Industry has good DEVELOPMENT PROSPECT.
, Barzak et al. [Xiaomei Xi, Xiaofeng Yang.Spontaneous infiltration in 1961
of aluninum-silicon alloy into silicon carbide performs in air[J]. J. Am.
Ceram. Soc., 1996, 79(1):102-108.] use the aluminium of 4: 1 mol ratios and the mixed-powder of silicon, distilation
Al is obtained first afterwards4SiC4.Subsequent Inou et al. [Akira Yamaguchi, Shaowei Zhang.Synthsis and
some properties of Al4SiC4[J]. J. Am.Ceram. Soc., 1995, 103(1):20-24.] use X
The method of ray single crystal diffraction and X ray powder diffractions obtains Al4SiC4Crystallographic data:Space group is demarcated as
P63mc, hexagonal crystallographic texture unit size is a=0.32771 ± 0.00001nm, c=2.16716 ± 0.0002nm.In recent years
Come, Al4SiC4Ceramics are because of its relatively low density(3.03g/cm3), fusing point (2037 DEG C of >) higher, there is stabilization at high temperature
Physicochemical property and the characteristic such as excellent mechanical performance and gradually paid close attention to by people.Yet with the difficulty in making, one
Al since straight4SiC4Synthesis and performance report it is very limited.
Up to now, Al4SiC4At home and abroad there are two kinds of corresponding preparation methods:One kind is solid-solid synthesis, and another kind is
Solid-liquid synthesis.Solid-solid synthesis, specific method has self-propagating high-temperature method, hot pressing sintering method, plasma spraying method, solid phase reaction to burn
Connection etc.;Solid-liquid synthesis, mainly including electric arc process, osmosis etc..The common drawback of these methods is synthesis temperature high,
Reaction time is long, wastes the energy, high cost.2009, Zhou Jun, Wang Gang, Li Hongxia et al. were in patent(CN 101619554 A)
In provide a kind of Al4SiC4The preparation method of powder body material, its raw materials by weight ball milling mixing 16-30h;It is cold-pressed into
The prefabricated section of 30%-60% relative compactions;Drying 6-8h is incubated at a temperature of 100-200 DEG C;Prefabricated section is placed in the appearance of carbon felt
Device internal layer, outer layer inserts secondary incendiary agent, after vacuumizing, is passed through nitrogen, powder needed for SHS process.The process
The consuming time is long, and the material density of synthesis is low.
Wen Guangwu et al. is by hot pressed sintering mode [G. W. Wen, X. X. Huang.Increased high
temperature strength and oxidation resistance of Al4SiC4 ceramics[J]. J. Eur.
Ceram. Soc, 2006, 26:1281-1286.], using native graphite, metallic aluminium powder and poly- carbonization silane(PCS)It is original
Material, is made the sample of mm × 5 mm of Φ 55, then leads to Al, SiC, C that raw material decomposes are high activity under ar gas environment
Cross hot pressing sintering processing to be reacted, generate Al4SiC4Material.The process productivity ratio is low, high cost.
2013, Du Wenxian, Zhou Liping et al. were in patent(CN 103304237 A)In provide a kind of Al4SiC4Powder
The preparation method of material, the method with gangue, metallic aluminium powder and carbon dust as raw material, using plasma spraying method direct spraying system
Standby Al4SiC4Material.The process has the disadvantage that noise is big, dust is more, harmful.
K.Itatani et al. solid phase reactions sintering process [K. Itatani, F. Takahashi, M. Aizawa, et
al. Densification and microstructural developments during the sintering of
aluminium silicon carbide[J]. J. Mater. Sci., 2002, 37:335-342.] with 4: 1 : 4
Ratio mixing Al powder, Si powder and activated carbon powder, pulverize it is last be heated to 1600 DEG C under an argon atmosphere, it is constant
After 10 hours, you can obtain Al4SiC4Powder.The production efficiency is low.
2012, Ruan Guozhi, Zhang Zhihui et al. were in patent(CN 102730690 A)In provide a kind of Al4SiC4Material
Preparation method, the technical scheme for being used is:By weight percentage composition by 45~65% Al powder, 20~35% SiC powder,
After 15~30% carbon dusts add absolute ethyl alcohol well mixed in ball milling, dried at 80~120 DEG C, then be embedded in for sample by shaping
In graphite crucible equipped with metallic aluminium powder, then graphite crucible is put into stove under the conditions of carbon is buried, in 1500~1700 DEG C of heating
And 2~7 hours are incubated, and after cooling, take out sample from graphite crucible and remove the impurity layer on surface, that is, obtain Al4SiC4Material
Material.The technique prepares inconvenience, and purity is relatively low.
A. Urena et al. electric arc processes [A.Urena, P.Rodrigo, L.Gil. Interfacial
reactions in an Al-Cu-Mg(2009)/SiCw composite during liquid processing[J]. J.
Mater. Sci., 2001, 36:429-439.] when being tested using SiC whiskers, chance on and utilize arc welding
The high energy of generation occurs in that the β-Al of needle-like on the contact surface4SiC4.The process electric arc flowing velocity is high, and reactant is in height
The warm area residence time is short, there is a problem of the life-span, and synthetic product purity is low.
Xiaofeng Yang et al. osmosis [Xiaomei Xi, Xiaofeng Yang. Spontaneous
infiltration of aluninum-silicon alloy into silicon carbide performs in air
[J]. J. Am. Ceram. Soc., 1996, 79(1):102-108.] Al-Si alloy solutions are heated to 1200
DEG C, Si-C prefabricated components are then immersed in, then 1500 DEG C ~ 1600 DEG C are heated rapidly to, and permeate within ten minutes, so that it may
To the thick Al of 5 mm4SiC4, but contain a small amount of Al, α-SiC and SiC phases.The technique synthetic material contains a small amount of impurity
Phase, purity is low.
To by Al4SiC4 ceramic applications to engineering field, it is necessary to a large amount of, high-purity, inexpensive Al4SiC4Ceramic fire resistant
Material.The present invention just prepares purity Al very high using the method for Microwave Hybrid Heating in the very short time4SiC4Ceramic powder
Material, greatly reduces production cost.
Compared with common microwave-assisted synthesis, Microwave Hybrid Heating technology has many advantages:Be first it is applied widely,
Both the very poor and readily volatilized reactant of microwave absorbing property can have been heated, the sample of easy oxidation can have also been prepared;Next to that
Equipment is simple, in addition to vacuum atmosphere microwave agglomerating furnace, it is only necessary to the common material such as alumina crucible;In addition, the technology section
Can be time saving, the heat time typically only needs a few minutes, only dozens of minutes most long.Therefore, in order to energy saving, reduction are produced into
This, it is necessary to explore a kind of low cost, the Al of process is simple4SiC4The preparation method of powder body material, preferably to meet
Al4SiC4The need for ceramic refractory adapts to high request smelting iron and steel.
The content of the invention
It is an object of the present invention to provide a kind of Al4SiC4The synthetic method of powder body material.
The purpose of the present invention is to be achieved through the following technical solutions, using Microwave Hybrid Heating technology.
Mainly wrapped following steps:
1. raw material and sample preparation:
2. graphite powder, aluminium powder, carborundum powder are weighed and mixed according to a certain percentage, then compressing tablet.
3. compressing tablet is put into small crucible, is wrapped up with demoulding medium, then small crucible is put into equipped with the big of heating medium
In crucible.
4. the sample that will be assembled is put into vacuum atmosphere microwave agglomerating furnace, mixed by microwave under the protection of inert atmosphere
Close the single-phase Al of heating synthesis4SiC4Powder body material.
2. evaluate:Sample is characterized with XRD
3. advantage:
4. present device is simple, and technique is easily controlled, and energy consumption is relatively low.
5. Al in the sample prepared by4SiC4Phase content is higher, close to single-phase.
6. preparation time is short, and compared with traditional preparation methods, efficiency improves decades of times.
4. illustrate:
3. sample strip is suppressed with appropriate pressure, microwave heating time is shorter.
4. inert gas is gas not with example reaction.
5. the heating medium described in is the material that can absorb microwave.
Brief description of the drawings:
Fig. 1 is the XRD spectrum of sample obtained after the embodiment that the present invention is provided.
Specific embodiment:
Embodiment 1:
With aluminium powder, carborundum powder, graphite powder as raw material.According to=(4.1:1:Or (4 3):1.2:Or (4 3):1:2.8) mole
Than weighing, mixed powder is placed in after being ground 10-30 minutes in mortar, after powder is pressed into bar shape, briquetting put
In homemade reactor, the crucible lid of aluminum oxide is covered, fully assembled sample to be sintered is put into microwave sintering
After stove, fire door is closed, after extracting vacuum extremely -0.1, turn off vavuum pump.Argon flow amount 16-160L/h is passed through until reaching positive normal pressure
Power, turns down after being passed through argon flow amount, starts microwave sintering, and sintering time is certain, 1200 DEG C of sintering temperature, soaking time 10min.
The same manner takes same crucible, and ibid, soaking time is constant for dispensing, assembling mode and sintering condition, but sintering temperature is set to
1300 DEG C, taken out after after sample cooling, polished with abrasive paper for metallograph surface, finally ground so as to obtain Al4SiC4Powder.
Embodiment 2:
With aluminium powder, carborundum powder, graphite powder as raw material.According to=(4.1:1:Or (4 3):1.2:Or (4 3):1:2.8) mol ratio
Weigh, mixed powder is placed in after being ground 10-30 minutes in mortar, after powder is pressed into bar shape, briquetting is put in
In homemade reactor, the crucible lid of aluminum oxide is covered, after fully assembled sample to be sintered is put into micro-wave oven, closed
Closed furnace door, after extracting vacuum extremely -0.1, turns off vavuum pump.Argon flow amount 16-160L/h is passed through until reaching normal pressure, is turned down
After being passed through argon flow amount, start microwave sintering, 1200 DEG C of sintering temperature is incubated 10min.The same manner takes same crucible, dispensing,
Ibid, sintering temperature is constant for assembling mode and sintering condition, but soaking time is 15min.Taken out after after sample cooling, use metallographic
Coated abrasive surface is polished, and is finally ground so as to obtain Al4SiC4Powder.
Embodiment 3:
With aluminium powder, carborundum powder, graphite powder as raw material.According to=4.05:1:3 mol ratio is weighed, and mixed powder is put
In mortar grind 10-30 minutes, after powder is pressed into bar shape material.Briquetting is put in homemade reactor, is covered
The crucible lid of aluminum oxide, after fully assembled sample to be sintered is put into microwave agglomerating furnace, closes fire door, extracts vacuum
After to -0.1, turn off vavuum pump.Argon flow amount 16-160L/h is passed through until reaching normal pressure, is turned down after being passed through argon flow amount,
Start microwave sintering, sintering time is certain.Sintering temperature is set to 1200 DEG C, and soaking time 10min when testing every time, sinters temperature
Degree, soaking time are identical, but constantly adjust raw material proportioning.Taken out after after sample cooling, polished with abrasive paper for metallograph surface, finally ground
It is broken so as to obtain Al4SiC4Powder.
Claims (5)
1. a kind of microwave synthesizes Al4SiC4The preparation method of powder body material, it is characterised in that:The Al4SiC4It is prepared by powder body material
Method is comprised the following steps that:
(1)With metal Al powder, SiC powder and carbon black or graphite as raw material, metal Al powder, SiC powder and carbon black or graphite are pressed
Mol ratio(4.0~4.4):(1~1.1):(2.8~3)Above-mentioned three kinds of materials are sufficiently mixed:
(2)Using mould by step(1)Compound be pressed into bar shape material;
(3)The bar shape material that step (2) is suppressed is placed in the self-control reactor with heating medium;
(4)The sample assembled in step (3) is put into vacuum atmosphere microwave agglomerating furnace, is not being sent out with raw material and product
In sintering, held for some time under uniform temperature under the protection of the inert gas of biochemical reaction;
(5) by step(4)Sintered product crushed in mortar, Al is obtained4SiC4Powder.
2. microwave synthesizes Al according to claim 14SiC4The preparation method of powder body material, it is characterised in that:Described raw material
SiC powder can be green silicon carbide powder, black silicon carbide silica flour, yellow carborundum powder etc..
3. microwave synthesizes Al according to claim 14SiC4The preparation method of powder body material, it is characterised in that:Described self-control
Reactor is in small crucible, the raw material for suppressing to be wrapped up with demoulding medium, and then small crucible is put into equipped with heating medium
In big crucible.
4. microwave synthesizes Al according to claim 14SiC4The preparation method of powder body material, it is characterised in that:Described heating
Medium can be a kind of or their mixture in graphite, cupric oxide, carborundum.
5. microwave synthesizes Al according to claim 14SiC4The preparation method of powder body material, it is characterised in that:Heat time is
5~20 minutes, heating-up temperature was 1100~1500 °C.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108928821A (en) * | 2018-08-21 | 2018-12-04 | 西安石油大学 | A kind of new A l4SiC4The preparation method of stratified material |
CN109251033A (en) * | 2018-10-29 | 2019-01-22 | 河南工业大学 | A kind of microwave synthesis Ti2The method of AlC block materials |
CN109467448A (en) * | 2018-10-31 | 2019-03-15 | 武汉科技大学 | A kind of Al4SiC4Refractory material and preparation method |
CN111681815A (en) * | 2020-05-26 | 2020-09-18 | 浙江万马股份有限公司 | High-carrying-capacity modified polypropylene insulating multi-core cable |
CN111681816A (en) * | 2020-05-26 | 2020-09-18 | 浙江万马股份有限公司 | High-current-carrying-capacity modified polypropylene insulated cable and modified polypropylene insulating material used by same |
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CN101565322A (en) * | 2009-01-21 | 2009-10-28 | 徐艳姬 | Ceramic fiber fabric-reinforced microwave heating plate and chamber and manufacturing method thereof |
CN102730690A (en) * | 2012-06-16 | 2012-10-17 | 山东科技大学 | Al4SiC4 material synthetic method |
CN103304237A (en) * | 2013-05-07 | 2013-09-18 | 山东科技大学 | Synthesis method of Al4SiC4 material |
JP6131625B2 (en) * | 2013-02-14 | 2017-05-24 | 新日鐵住金株式会社 | Method for producing Al4SiC4 powder and method for producing MgO-C brick |
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CN101423215A (en) * | 2008-11-27 | 2009-05-06 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing Al4SiC4 powder |
CN101565322A (en) * | 2009-01-21 | 2009-10-28 | 徐艳姬 | Ceramic fiber fabric-reinforced microwave heating plate and chamber and manufacturing method thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108928821A (en) * | 2018-08-21 | 2018-12-04 | 西安石油大学 | A kind of new A l4SiC4The preparation method of stratified material |
CN109251033A (en) * | 2018-10-29 | 2019-01-22 | 河南工业大学 | A kind of microwave synthesis Ti2The method of AlC block materials |
CN109467448A (en) * | 2018-10-31 | 2019-03-15 | 武汉科技大学 | A kind of Al4SiC4Refractory material and preparation method |
CN111681815A (en) * | 2020-05-26 | 2020-09-18 | 浙江万马股份有限公司 | High-carrying-capacity modified polypropylene insulating multi-core cable |
CN111681816A (en) * | 2020-05-26 | 2020-09-18 | 浙江万马股份有限公司 | High-current-carrying-capacity modified polypropylene insulated cable and modified polypropylene insulating material used by same |
CN111681815B (en) * | 2020-05-26 | 2022-03-01 | 浙江万马股份有限公司 | High-carrying-capacity modified polypropylene insulating multi-core cable |
CN111681816B (en) * | 2020-05-26 | 2022-03-01 | 浙江万马股份有限公司 | High-current-carrying-capacity modified polypropylene insulated cable and modified polypropylene insulating material used by same |
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