CN101698487A - Method for preparing mullite powder - Google Patents
Method for preparing mullite powder Download PDFInfo
- Publication number
- CN101698487A CN101698487A CN200910218859A CN200910218859A CN101698487A CN 101698487 A CN101698487 A CN 101698487A CN 200910218859 A CN200910218859 A CN 200910218859A CN 200910218859 A CN200910218859 A CN 200910218859A CN 101698487 A CN101698487 A CN 101698487A
- Authority
- CN
- China
- Prior art keywords
- solution
- distilled water
- mullite powder
- placing
- mullite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing mullite powder, and the method comprises the following steps: dissolving tetraethyl orthosilicate in ethanol solution, further adding distilled water into the solution, using hydrochloric acid for regulating pH value to be 2-4, and then carrying out magnetic stirring, thereby obtaining mixed solution; then dissolving Al(NO3)3.9H2O in the distilled water; adding the Al(NO3)3.9H2O solution into the mixed solution, carrying out the magnetic stirring, mixing evenly, then using ammonia for regulating the pH value to be 4.5-5.5, placing in a baking oven for obtaining a dried gel, placing the dried gel in a hydrothermal kettle, further adding the distilled water into the hydrothermal kettle, carrying out hydrothermal treatment at 200 DEG C, taking out a sample and placing in the baking oven for drying; and placing the dried sample in an aluminium oxide crucible, placing in a muffle furnace, increasing the temperature to 1150-1200 DEG C and keeping the temperature for 2h, thereby obtaining the nano-mullite powder. The sol-gel-ultrasonic method is firstly used in the method for preparing the mullite dried gel, then water is selected as a solvent, the hydrothermal treatment is carried out for a period of time, and then the calcination is carried out in the muffle furnace. The obtained nano-mullite powder has the advantages of uniform distraction of the particle size, controllable shape, short reaction cycle and good repeatability, thereby having broad development prospects.
Description
Technical field
The invention belongs to field of material preparation, be specifically related to a kind of preparation method of mullite powder.
Background technology
Mullite (mullite) is a kind of very practical 26S Proteasome Structure and Function material, have the good characteristic that other ceramic does not possess, as lower heat-conduction coefficient and thermal expansivity, high creep resistance and thermal shock resistance, excellent electric insulation, chemical stability and hot strength etc., can be used as high-temperature structural material, infrared transparent window, microelectronics base material also can be used as catalyst support material.Be widely used in making engineering materials, refractory materials and supercoat material, the Mullite porcelain that with the mullite is principal crystalline phase is then because the ideal material that low specific inductivity, low thermal expansivity and good electrical insulation properties are considered to modern novel computer component package.Mullite material (comprising mullite ceramic and based on mullite matrix material etc.) is that raw material makes with the mullite powder normally, and its performance depends on the quality of mullite powder.High-purity, superfine mullite powder can not only reduce the firing temperature of mullite material, and can improve the microstructure of material, improves its performance greatly.So preparation, especially the purity height of mullite powder, the preparation of the ultra-fine mullite powder of fine particles and hard aggregation-free just occupies crucial status in mullite material research.
Up to the present, the mullite nano crystalline substance is synthesized by several methods, as sol-gel method [Bulzar D, Lebdetter H, Crystal structure and compressibility of 3:2 mullite, American Mineralogist[J] .1993,78:1192-1196], coprecipitation method [Zhou M H, Jose M F, etal.Coprecipitation and processing of mullite precursor phases[J] .J.Am.Ceram.Soc.1996,79 (7): 1756], hydrolysis-precipitator method [Xu Mingxia, Cui Feng, Deng. ultra micro mullite powdered preparation novel process [J]. silicate journal, 1991,19 (1): 80], hydrothermal crystallization method [Xue Rujun, Wang faithful and upright person, high China. the research [J] of hydro-thermal mullite synthesizing ultrafine powder particle stability. Anhui University of Science and Technology's journal, 2006,26 (2): 58-60], spray pyrolysis [Kanzaki S, Tabata H.Sintering and mechanicalproperties of stoichiometric mullite[J] .J.Am.Ceram.Soc., 1985,68 (1): C6] or the like.These methods or to the equipment requirements height, equipment and instrument are relatively more expensive; Very little to utilization ratio of raw materials; Perhaps complex process, preparation cycle is long, and is repeatable poor.In order to reach the purpose of practicability, the preparation technology of the nano mullite powder that necessary Development and Production cost is low, simple to operate, the cycle is short.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of mullite powder, the mullite powder that obtains by preparation method of the present invention is evenly distributed, and particle diameter is less, and pattern is controlled.This method not only greatly reduces preparation cost, and simple to operate, reaction time is short, good reproducibility.
For achieving the above object, the technical solution used in the present invention is:
1) at first, getting the 5-10ml tetraethoxy is dissolved in the analytically pure ethanolic soln, get solution A to wherein adding distilled water again, tetraethoxy wherein: ethanol: the volume ratio of distilled water is 1: 4: 2～4, transferring the pH value of solution A with hydrochloric acid is 2～4, solution A after will regulating with hydrochloric acid then places the beaker that seals with preservative film, and magnetic agitation makes tetraethoxy prehydrolysis obtain mixing solutions B at normal temperatures;
2) then, according to Si: the mol ratio of Al is that 1: 3 ratio is got analytically pure Al (NO
3)
39H
2O puts into beaker, and adds the distilled water of 10-20ml in beaker, and magnetic agitation makes Al (NO at normal temperatures
3)
39H
2O dissolve fully Al (NO
3)
39H
2O solution;
3) with Al (NO
3)
39H
2O solution mixes to be placed in the ultrasound reactor with solution B and reacts, the power of ultrasound reactor is that 300-500W, bath temperature are 60-80 ℃, irradiation time is 2-4h, stirs simultaneously 30-60 minute, regulates making that the pH value of solution is that 4.5-5.5 gets mixed solution C again with ammoniacal liquor;
4) mixed solution C is placed baking oven, drying down at 60-80 ℃ is xerogel, and xerogel is placed water heating kettle, in water heating kettle, add distilled water again, add to water heating kettle volumetrical 1/2-2/3 place,, take out sample and place baking oven to dry then at 200 ℃ of following hydrothermal treatment consists 12h-16h;
5) sample after will drying places alumina crucible, places retort furnace, and it is 5 ℃/min that temperature rise rate is set, and makes it be warming up to 1150-1200 ℃, insulation 2h, then at the stove internal cooling to room temperature, promptly get nano mullite powder.
The present invention prepares the mullite xerogel with collosol and gel-ultrasonic method earlier, and selecting water then for use is solvent, and hydrothermal treatment consists places retort furnace to calcine after for some time again.Gained nano mullite size distribution is even, and pattern is controlled, and reaction time is short, and therefore good reproducibility has vast potential for future development.
Description of drawings
Fig. 1 is the XRD figure spectrum of the nano mullite powder that makes of the present invention;
Fig. 2 is the SEM picture of the nano mullite powder that makes of the present invention.
Embodiment
Embodiment 1:
1) at first, getting the 10ml tetraethoxy is dissolved in the analytically pure ethanolic soln, get solution A to wherein adding distilled water again, tetraethoxy wherein: ethanol: the volume ratio of distilled water is 1: 4: 4, transferring the pH value of solution A with hydrochloric acid is 2, solution A after will regulating with hydrochloric acid then places the beaker that seals with preservative film, and magnetic agitation makes tetraethoxy prehydrolysis obtain mixing solutions B at normal temperatures;
2) then, according to Si: the mol ratio of Al is that 1: 3 ratio is got analytically pure Al (NO
3)
39H
2O puts into beaker, and adds the distilled water of 20ml in beaker, and magnetic agitation makes Al (NO at normal temperatures
3)
39H
2O dissolve fully Al (NO
3)
39H
2O solution;
3) with Al (NO
3)
39H
2O solution mixes to be placed in the ultrasound reactor with solution B and reacts, and the power of ultrasound reactor is that 300W, bath temperature are 80 ℃, and irradiation time is 2h, stirs simultaneously 30 minutes, regulates making that the pH value of solution is 5 must mixed solution C again with ammoniacal liquor;
4) mixed solution C is placed baking oven, drying down at 80 ℃ is xerogel, and xerogel is placed water heating kettle, in water heating kettle, add distilled water again, add to water heating kettle volumetrical 1/2-2/3 place,, take out sample and place baking oven to dry then at 200 ℃ of following hydrothermal treatment consists 12h;
5) sample after will drying places alumina crucible, places retort furnace, and it is 5 ℃/min that temperature rise rate is set, and makes it be warming up to 1200 ℃, insulation 2h, then at the stove internal cooling to room temperature, promptly get nano mullite powder.
Embodiment 2:
1) at first, getting the 8ml tetraethoxy is dissolved in the analytically pure ethanolic soln, get solution A to wherein adding distilled water again, tetraethoxy wherein: ethanol: the volume ratio of distilled water is 1: 4: 3, transferring the pH value of solution A with hydrochloric acid is 3, solution A after will regulating with hydrochloric acid then places the beaker that seals with preservative film, and magnetic agitation makes tetraethoxy prehydrolysis obtain mixing solutions B at normal temperatures;
2) then, according to Si: the mol ratio of Al is that 1: 3 ratio is got analytically pure Al (NO
3)
39H
2O puts into beaker, and adds the distilled water of 15ml in beaker, and magnetic agitation makes Al (NO at normal temperatures
3)
39H
2O dissolve fully Al (NO
3)
39H
2O solution;
3) with Al (NO
3)
39H
2O solution mixes to be placed in the ultrasound reactor with solution B and reacts, and the power of ultrasound reactor is that 400W, bath temperature are 70 ℃, and irradiation time is 3h, stirs simultaneously 45 minutes, regulates making that the pH value of solution is 4.5 must mixed solution C again with ammoniacal liquor;
4) mixed solution C is placed baking oven, drying down at 70 ℃ is xerogel, and xerogel is placed water heating kettle, in water heating kettle, add distilled water again, add to water heating kettle volumetrical 1/2-2/3 place,, take out sample and place baking oven to dry then at 200 ℃ of following hydrothermal treatment consists 16h;
5) sample after will drying places alumina crucible, places retort furnace, and it is 5 ℃/min that temperature rise rate is set, and makes it be warming up to 1150 ℃, insulation 2h, then at the stove internal cooling to room temperature, promptly get nano mullite powder.
Embodiment 3:
1) at first, getting the 5ml tetraethoxy is dissolved in the analytically pure ethanolic soln, get solution A to wherein adding distilled water again, tetraethoxy wherein: ethanol: the volume ratio of distilled water is 1: 4: 2, transferring the pH value of solution A with hydrochloric acid is 4, solution A after will regulating with hydrochloric acid then places the beaker that seals with preservative film, and magnetic agitation makes tetraethoxy prehydrolysis obtain mixing solutions B at normal temperatures;
2) then, according to Si: the mol ratio of Al is that 1: 3 ratio is got analytically pure Al (NO
3)
39H
2O puts into beaker, and adds the distilled water of 10ml in beaker, and magnetic agitation makes Al (NO at normal temperatures
3)
39H
2O dissolve fully Al (NO
3)
39H
2O solution;
3) with Al (NO
3)
39H
2O solution mixes to be placed in the ultrasound reactor with solution B and reacts, and the power of ultrasound reactor is that 500W, bath temperature are 60 ℃, and irradiation time is 4h, stirs simultaneously 60 minutes, regulates making that the pH value of solution is 5.5 must mixed solution C again with ammoniacal liquor;
4) mixed solution C is placed baking oven, drying down at 60 ℃ is xerogel, and xerogel is placed water heating kettle, in water heating kettle, add distilled water again, add to water heating kettle volumetrical 1/2-2/3 place,, take out sample and place baking oven to dry then at 200 ℃ of following hydrothermal treatment consists 14h;
5) sample after will drying places alumina crucible, places retort furnace, and it is 5 ℃/min that temperature rise rate is set, and makes it be warming up to 1180 ℃, insulation 2h, then at the stove internal cooling to room temperature, promptly get nano mullite powder.
Referring to Fig. 1, prepared as seen from Figure 1 sample does not have dephasign, be pure mullite powder, and the peak type is sharp-pointed, proves that crystal property is relatively good.
Referring to Fig. 2, prepared as seen from Figure 2 sample topography is a club shaped structure, and particle size is smaller, and it is more even to distribute.
Claims (1)
1. the preparation method of a mullite powder is characterized in that:
1) at first, getting the 5-10ml tetraethoxy is dissolved in the analytically pure ethanolic soln, get solution A to wherein adding distilled water again, tetraethoxy wherein: ethanol: the volume ratio of distilled water is 1: 4: 2～4, transferring the pH value of solution A with hydrochloric acid is 2～4, solution A after will regulating with hydrochloric acid then places the beaker that seals with preservative film, and magnetic agitation makes tetraethoxy prehydrolysis obtain mixing solutions B at normal temperatures;
2) then, according to Si: the mol ratio of Al is that 1: 3 ratio is got analytically pure Al (NO
3)
39H
2O puts into beaker, and adds the distilled water of 10-20ml in beaker, and magnetic agitation makes Al (NO at normal temperatures
3)
39H
2O dissolve fully Al (NO
3)
39H
2O solution;
3) with Al (NO
3)
39H
2O solution mixes to be placed in the ultrasound reactor with solution B and reacts, the power of ultrasound reactor is that 300-500W, bath temperature are 60-80 ℃, irradiation time is 2-4h, stirs simultaneously 30-60 minute, regulates making that the pH value of solution is that 4.5-5.5 gets mixed solution C again with ammoniacal liquor;
4) mixed solution C is placed baking oven, drying down at 60-80 ℃ is xerogel, and xerogel is placed water heating kettle, in water heating kettle, add distilled water again, add to water heating kettle volumetrical 1/2-2/3 place,, take out sample and place baking oven to dry then at 200 ℃ of following hydrothermal treatment consists 12h-16h;
5) sample after will drying places alumina crucible, places retort furnace, and it is 5 ℃/min that temperature rise rate is set, and makes it be warming up to 1150-1200 ℃, insulation 2h, then at the stove internal cooling to room temperature, promptly get nano mullite powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102188599A CN101698487B (en) | 2009-10-30 | 2009-10-30 | Method for preparing mullite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102188599A CN101698487B (en) | 2009-10-30 | 2009-10-30 | Method for preparing mullite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101698487A true CN101698487A (en) | 2010-04-28 |
| CN101698487B CN101698487B (en) | 2011-06-29 |
Family
ID=42146947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102188599A Expired - Fee Related CN101698487B (en) | 2009-10-30 | 2009-10-30 | Method for preparing mullite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101698487B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016668A (en) * | 2014-06-09 | 2014-09-03 | 河海大学 | Preparation method of mullite ceramic powder |
| CN108517714A (en) * | 2018-04-04 | 2018-09-11 | 黄智慧 | A kind of preparation method of high tenacity inorganic refractory paper material |
| CN108601110A (en) * | 2018-05-03 | 2018-09-28 | 杨诚龙 | Anti-thermal shock heating element |
| CN110468453A (en) * | 2019-09-23 | 2019-11-19 | 哈工大(北京)军民融合创新研究院有限公司 | A kind of preparation method of growth in situ high length-diameter ratio mullite crystal whisker |
| CN113773105A (en) * | 2021-09-06 | 2021-12-10 | 深圳星光点点科技有限公司 | Porous ceramic atomizing core for electronic cigarette and preparation method and application thereof |
| CN114149695A (en) * | 2021-12-17 | 2022-03-08 | 景德镇陶瓷大学 | Mullite coated gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method |
-
2009
- 2009-10-30 CN CN2009102188599A patent/CN101698487B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016668A (en) * | 2014-06-09 | 2014-09-03 | 河海大学 | Preparation method of mullite ceramic powder |
| CN104016668B (en) * | 2014-06-09 | 2015-12-09 | 河海大学 | A kind of mullite ceramic raw powder's production technology |
| CN108517714A (en) * | 2018-04-04 | 2018-09-11 | 黄智慧 | A kind of preparation method of high tenacity inorganic refractory paper material |
| CN108601110A (en) * | 2018-05-03 | 2018-09-28 | 杨诚龙 | Anti-thermal shock heating element |
| CN110468453A (en) * | 2019-09-23 | 2019-11-19 | 哈工大(北京)军民融合创新研究院有限公司 | A kind of preparation method of growth in situ high length-diameter ratio mullite crystal whisker |
| CN110468453B (en) * | 2019-09-23 | 2020-09-29 | 哈工大(北京)军民融合创新研究院有限公司 | Preparation method for in-situ growth of high-length-diameter-ratio mullite whiskers |
| CN113773105A (en) * | 2021-09-06 | 2021-12-10 | 深圳星光点点科技有限公司 | Porous ceramic atomizing core for electronic cigarette and preparation method and application thereof |
| CN113773105B (en) * | 2021-09-06 | 2022-11-25 | 深圳星光点点科技有限公司 | Porous ceramic atomizing core for electronic cigarette and preparation method and application thereof |
| CN114149695A (en) * | 2021-12-17 | 2022-03-08 | 景德镇陶瓷大学 | Mullite coated gamma-Ce2S3Preparation method of red pigment and product prepared by preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101698487B (en) | 2011-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101698487B (en) | Method for preparing mullite powder | |
| CN101717262B (en) | Method for preparing nano mullite powder by sol-gel and solvothermal method | |
| CN101898906B (en) | Preparation method of SiO2-mullite-Al2O3 gradient outer coating for carbon/carbon composite material | |
| CN101700980B (en) | Method for preparing nano-mullite powder by sol-gel-hydrothermal method | |
| Ansar et al. | Development of mullite and spinel coatings on graphite for improved water-wettability and oxidation resistance | |
| CN101935877A (en) | Method for synthesizing mullite whiskers by normal pressure sintering | |
| CN101845668B (en) | Method for preparing nano nickel borate whiskers | |
| CN102502538B (en) | Method for synthesizing ultrafine aluminum nitride powder at low temperature under assistance of calcium | |
| CN107721429A (en) | Zirconium carbide silicon carbide composite powder body material and preparation method thereof | |
| CN104649709A (en) | Method for manufacturing porous silicon carbide ceramic | |
| CN102964128B (en) | Sol-gel preparation method of Yb2Si2O7 powder | |
| CN101700979B (en) | Method for preparing nano-mullite powder by sol-gel-ultrasonic chemistry method | |
| CN115872725A (en) | Al-Y-Cr-Fe-Zr-Nb-Ti-Ta-O high-entropy composite oxide hydrogen-resistant coating | |
| CN101700887B (en) | Method for preparing nano-mullite powder by sol-gel-microwave hydrothermal method | |
| CN104016668B (en) | A kind of mullite ceramic raw powder's production technology | |
| CN101838157B (en) | Method for preparing carbon/carbon composite material nanometer silicon carbide-mullite composite external coating | |
| CN102557055B (en) | Preparation method of zirconium silicate powder | |
| CN103922354A (en) | High-yield zirconium silicate powder synthesized by sol-gel method | |
| CN104045108A (en) | Method for preparing TiO powder material | |
| CN101456561A (en) | Method for preparing nano mullite powder | |
| CN102502675B (en) | Preparation method of spherical zirconium silicate nanocrystal | |
| CN105884370B (en) | A kind of zirconium diboride raw powder's production technology | |
| CN109422528A (en) | A kind of preparation method of aluminum oxide-silicon carbide high-temperature ceramic materials | |
| CN113548898A (en) | (Mo)0.2W0.2V0.2Cr0.2Ni0.2) B high-entropy ceramic powder and preparation method thereof | |
| CN108358641B (en) | Al (aluminum)4SiC4Method for preparing ceramic material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110629 Termination date: 20131030 |