CN106316348B - A kind of nano ceramic microwave aqueous synthesis method - Google Patents

A kind of nano ceramic microwave aqueous synthesis method Download PDF

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CN106316348B
CN106316348B CN201610674629.3A CN201610674629A CN106316348B CN 106316348 B CN106316348 B CN 106316348B CN 201610674629 A CN201610674629 A CN 201610674629A CN 106316348 B CN106316348 B CN 106316348B
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silicate
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synthesis method
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高羽
朱寅中
马小波
高申元
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TIANDONG HAORUN NEW MATERIAL TECHNOLOGY Co.,Ltd.
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Guizhou Yuping Marvell Technology Co Ltd
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Abstract

The present invention relates to ceramic materials preparation technology fields, especially a kind of nano ceramic microwave aqueous synthesis method, after being mixed by raw material, in a high pressure reaction kettle, after adding water to be configured to mixed liquor, microwave heating is used again, it is passed through ammonia processing, so that mixed liquor ammonification, after sealing again, microwave continuous heating, so that temperature is quickly improved, simultaneously, pressure in reaction kettle also increases, so that water ionizes, show weak-alkaline and weak-acidic, so that material environment changes, promote the quick chemical combination and gelling reaction of each raw material, promote the particle powder of reactant, in conjunction with the microwave sintering processing under normal pressure, so that the performance of ceramic material is improved, improve ceramic material toughness.

Description

A kind of nano ceramic microwave aqueous synthesis method
Technical field
The present invention relates to ceramic materials preparation technology fields, especially a kind of nano ceramic microwave synthesis in water side Method.
Background technique
The preparation method of nanometer materials has physics the preparation method: including vacuum condensation method, physical crushing method, mechanical attrition method Deng；Chemical preparation method includes the methods of vapour deposition process, solution deposit, hydrothermal synthesis method, microemulsion method, solution-gel method.
In the prior art, the preparation process about ceramic material nanometer materials is more, such as CN200510094233.3 public affairs A kind of metal/ceramic nano composite additive of self-rehabilitation and preparation method have been opened, has been by nanoscale micro mist and the natural mine of nanoscale Mountain flour is that the materials such as the additional detergent-dispersant additive of primary raw material, liquefier, solvent are prepared by certain process conditions and production stage It forms；CN011167149 discloses a kind of preparation method of nanometer metal ceramic composite powder, including nano-ceramic powder is added Enter conventional treatment solution, be roughened, be sensitized, activated and applied ultrasonication, then uses main salt, reducing agent, complexing agent, pH Buffer, stabilizer composition；CN200610011690.6 discloses self-propagating high-temperature synthesis of nano tungsten carbide powder method, will receive Rice WO3Powder, nanometer carbon black, magnesium powder mixing, are added phenolic resin as self-propagating reaction activator, in argon gas or vacuum certainly After spreading pyroreaction, then with chemical Treatment at nano powder of tungsten carbide；CN200810106085.6 discloses a kind of synthesis The method of nano-scale oxide ceramic powder body, this method use sugaring pyrolysismethod, and metal ion source is dissolved in appropriate solvent, is added Enter sugar and foaming agent ammonium nitrate, then obtained solution is dry, obtained substance carries out pre-burning synthesis at a lower temperature Nano-powder.
Nevertheless, the demand in market cannot be still fully met for the preparation process of nano ceramic, so that It also needs to make continuous research to the processing technology of nano ceramic, for this purpose, there is researcher to synthesize for Nano-sized Artificial Ceramic material carries out technological design, so that ceramic particle even size distribution, and production cost is low；Specifically with stratiform Structured calcium silicate mineral are after raw material are ground into powder to raw material, to be sufficiently mixed with two kinds of raw materials or three kinds of raw materials；Again to divide Powder is surface-treated to mixture powder and is added a small amount of rare earths material and activator pollopas or urea；Utilize self- propagating skill Art handles the above-mentioned powder granule being surface-treated, and controls argon pressure, the temperature and time of spherical reactor；After reaction treatment Material be cooled to and the pure water of several times is added after room temperature is uniformly mixed and uses ultrasonic standing wave with certain frequency, certain sound intensity, place The impurity such as magnetic iron ore, rutile, quartz and feldspar are removed in several minutes of reason, separation；Above-mentioned material is heated and is kept for a period of time Ripening；The material of ripening is filtered, isolated filter cake with pure water repeatedly stirring and washing for several times, separation Solid content is obtained, Nano-sized Artificial synthesis ceramic material is obtained after which dry, pulverize.
Summary of the invention
On the basis of existing technology, the present invention provides a kind of nano ceramic microwave aqueous synthesis method.
It is achieved particular by following technical scheme:
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 2- thereto 4 times of water, stirs evenly, and obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, is passed through speed For 3-5mL/min, heat 10-20min, stops ammonia and be passed through, seal autoclave, continuous heating, so that temperature is 150-230 DEG C, constant temperature handles 30-50min, after decompression, autoclave is opened, under normal pressure, using microwave continuous heating 20- 30min crushes, obtains the ceramic material of 200-400nm.
The silicate powder is at least one of calcium silicates, sodium metasilicate, potassium silicate.
The mixture, raw material mixing mass ratio are silicate powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder =1-3:0.01-0.06:0.016-0.12:0.08-0.19:0.8-1.2.
The microwave, power 500-1000W.
The silicate powder, wherein the mass content of silicon is calculated as >=80% with silica.
The tungsten oxide powder, purity are >=80%.
The aluminium powder, the quality containing aluminum oxide are 8-15%.
The iron powder, the quality of two iron Han three oxygen are 3-7%.
Compared with prior art, technical effect of the invention is embodied in:
After mixing by raw material, in a high pressure reaction kettle, after adding water to be configured to mixed liquor, then microwave is used to add Heat is passed through ammonia processing, so that mixed liquor ammonification, then after sealing, microwave continuous heating, so that temperature is quickly improved, Meanwhile the pressure in reaction kettle also increases, so that water ionizes, shows weak-alkaline and weak-acidic, so that material environment becomes Change, promotes the quick chemical combination and gelling reaction of each raw material, promote the particle powder of reactant, in conjunction with micro- under normal pressure Wave sintering processes improve ceramic material toughness so that the performance of ceramic material is improved.
The invention uses microwave heating treatment, and reaction temperature is rapidly achieved, and at microwave heating Under reason, so that microwave plays the role of catalysis reaction, the process of reaction is accelerated, while the performance of ceramic material is obtained Improve, especially improves the toughness of ceramic material, improve the quality of ceramic material.
The process flow of the invention is simple, and process cycle is short, and cost is relatively low.
Silicate powder in the invention, tungsten oxide powder, aluminium powder, iron powder etc. are not pure silicate and oxidation Tungsten promotes the process of reaction product so that easily forming gum material in a kettle in reaction process, improves ceramic material Toughness.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed Range is not only limited to made description.
Embodiment 1
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 2 thereto Water again, stirs evenly, obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, and being passed through speed is 3mL/min heats 10min, stops ammonia and is passed through, and seals autoclave, continuous heating, so that temperature is 150 DEG C, it is permanent Temperature processing 30min, after decompression, opens autoclave, under normal pressure, using microwave continuous heating 20min, crushes, obtains The ceramic material of 200nm.
The mixture, raw material mixing mass ratio are silicate powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder =1:0.01:0.016:0.08:0.8.The microwave, power 500W.The silicate powder, the wherein quality of silicon Content is calculated as >=80% with silica.The tungsten oxide powder, purity are >=80%.The aluminium powder contains three oxygen The quality for changing two aluminium is 8%.The iron powder, the quality of two iron Han three oxygen are 3%.
Silicate powder is silicate ore, specifically the crushed material of talcum mineral or galapectite mineral.
Embodiment 2
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 2- thereto 4 times of water, stirs evenly, and obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, is passed through speed For 5mL/min, heat 20min, stop ammonia and be passed through, seals autoclave, continuous heating, so that temperature is 230 DEG C, Constant temperature handles 50min, after decompression, opens autoclave, under normal pressure, using microwave continuous heating 30min, crushes, obtains The ceramic material of 400nm.
The silicate powder is calcium silicates.The mixture, raw material mixing mass ratio are silicate powder: oxygen Change tungsten powder: aluminium powder: iron powder: graphite powder=3:0.06:0.12:0.19:1.2.The microwave, power 1000W.It is described Silicate powder, wherein the mass content of silicon is calculated as >=80% with silica.The tungsten oxide powder, purity be >= 80%.The aluminium powder, the quality containing aluminum oxide are 15%.The quality of the iron powder, two iron Han three oxygen is 7%.
Embodiment 3
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 3 thereto Water again, stirs evenly, obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, and being passed through speed is 4mL/min heats 15min, stops ammonia and is passed through, and seals autoclave, continuous heating, so that temperature is 190 DEG C, it is permanent Temperature processing 40min, after decompression, opens autoclave, under normal pressure, using microwave continuous heating 25min, crushes, obtains The ceramic material of 300nm.The silicate powder is sodium metasilicate.The mixture, raw material mixing mass ratio are silicic acid Salt powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder=2:0.05:0.08:0.13:0.9.The microwave, power are 700W.Above-mentioned silicate powder is not pure sodium metasilicate powder, but the quality that the silicate powder meets silicon contains Amount is calculated as >=80% with silica.The tungsten oxide powder, purity are >=80%.The aluminium powder, containing three oxidations The quality of two aluminium is 11%.The iron powder, the quality of two iron Han three oxygen are 5%.
Embodiment 4
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 2 thereto Water again, stirs evenly, obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, and being passed through speed is 5mL/min heats 20min, stops ammonia and is passed through, and seals autoclave, continuous heating, so that temperature is 150 DEG C, it is permanent Temperature processing 50min, after decompression, opens autoclave, under normal pressure, using microwave continuous heating 30min, crushes, obtains The ceramic material of 200nm.
The silicate powder is calcium silicates, sodium metasilicate arbitrarily mixes.The mixture, raw material mixing mass ratio For silicate powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder=1:0.06:0.016:0.08:1.2.The microwave, Power is 500W.Above-mentioned silicate powder is not pure sodium metasilicate powder, but the silicate powder will meet silicon Mass content be calculated as >=80% with silica.The tungsten oxide powder, purity are >=80%.The aluminium powder, Quality containing aluminum oxide is 8%.The iron powder, the quality of two iron Han three oxygen are 7%.
Embodiment 5
A kind of nano ceramic microwave aqueous synthesis method, by silicate powder, tungsten oxide powder, aluminium powder, iron powder, Graphite powder is uniformly mixed, and obtains mixture；Mixture is placed in autoclave, and is added accounts for mixture quality 4 thereto Water again, stirs evenly, obtains mixed liquor；Microwave heating treatment is used again, while being passed through ammonia into mixed liquor, and being passed through speed is 3mL/min heats 10min, stops ammonia and is passed through, and seals autoclave, continuous heating, so that temperature is 230 DEG C, it is permanent Temperature processing 50min, after decompression, opens autoclave, under normal pressure, using microwave continuous heating 20min, crushes, obtains The ceramic material of 400nm.
The silicate powder is calcium silicates, sodium metasilicate, potassium silicate arbitrarily mix.The mixture, raw material are mixed Conjunction mass ratio is silicate powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder=3:0.06:0.016:0.19:0.8.It is described Microwave, power 500W.The silicate powder, wherein the mass content of silicon is calculated as >=80% with silica.Institute The tungsten oxide powder stated, purity are >=80%.The aluminium powder, the quality containing aluminum oxide are 15%.The iron Powder, the quality of two iron Han three oxygen are 3%.

Claims (3)

1. a kind of nano ceramic microwave aqueous synthesis method, which is characterized in that by silicate powder, tungsten oxide powder, Aluminium powder, iron powder, graphite powder are uniformly mixed, and obtain mixture；Mixture is placed in autoclave, and thereto be added account for it is mixed The water for closing 2-4 times of amount of substance, stirs evenly, obtains mixed liquor；Microwave heating treatment is used again, while ammonia is passed through into mixed liquor Gas, being passed through speed is 3-5mL/min, heats 10-20min, stops ammonia and is passed through, sealing autoclave, continuous heating, So that temperature is 150-230 DEG C, constant temperature handles 30-50min, after decompression, autoclave is opened, under normal pressure, using microwave Continuous heating 20-30min crushes, obtains the ceramic material of 200-400nm；
The microwave, power 500-1000W；
The silicate powder, wherein the mass content of silicon is calculated as >=80% with silica；
The tungsten oxide powder, purity are >=80%；
The aluminium powder, the quality containing aluminum oxide are 8-15%；
The iron powder, the quality of two iron Han three oxygen are 3-7%.
2. nano ceramic microwave aqueous synthesis method as described in claim 1, which is characterized in that the silicate Powder is at least one of calcium silicates, sodium metasilicate, potassium silicate.
3. nano ceramic microwave aqueous synthesis method as described in claim 1, which is characterized in that the mixing Object, raw material mixing mass ratio are silicate powder: tungsten oxide powder: aluminium powder: iron powder: graphite powder=1-3:0.01-0.06: 0.016-0.12:0.08-0.19:0.8-1.2。
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