CN101109106A - Process for producing aluminum oxide crystal whisker - Google Patents
Process for producing aluminum oxide crystal whisker Download PDFInfo
- Publication number
- CN101109106A CN101109106A CNA200710018539XA CN200710018539A CN101109106A CN 101109106 A CN101109106 A CN 101109106A CN A200710018539X A CNA200710018539X A CN A200710018539XA CN 200710018539 A CN200710018539 A CN 200710018539A CN 101109106 A CN101109106 A CN 101109106A
- Authority
- CN
- China
- Prior art keywords
- alumina
- product
- whisker
- crystal whisker
- alumina whisker
- 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
- 239000013078 crystal Substances 0.000 title abstract description 10
- 238000000034 method Methods 0.000 title description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 36
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- 238000002441 X-ray diffraction Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 229940103272 aluminum potassium sulfate Drugs 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 abstract 1
- 229910052939 potassium sulfate Inorganic materials 0.000 abstract 1
- 235000011151 potassium sulphates Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- 238000001354 calcination Methods 0.000 description 7
- 238000002386 leaching Methods 0.000 description 7
- 208000006558 Dental Calculus Diseases 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007716 flux method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- ILRLTAZWFOQHRT-UHFFFAOYSA-N potassium;sulfuric acid Chemical compound [K].OS(O)(=O)=O ILRLTAZWFOQHRT-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a preparing way for alumina crystal whisker material. Wherein, aluminum material and fluxing agent are mixed evenly in mole ratio 1:0.25 swung dash 1:12, placed into a baking crucible, baked for 2 swung dash 8 hours under 900 swung dash 1200 Celsius system; the cooled sintered substance is solved and dried, then the product of alumina crystal whisker is obtained. The invention uses aluminum potassium sulfate as the source of aluminum, which is dissolved into active alumina and potassium sulfate under high temperature, the reaction temperature and time are effectively reduced, energy consumption is reduced; the product is of high purity and yield rate (up to 50% above). The alumina crystal whisker prepared by the invention is of pure phase according to test by X-ray diffraction, the average diameter is 0.5 swung dash 3 micrometer, and the average length is 10 swung dash 100 micrometer.
Description
Technical field
The invention belongs to inorganic salt material technology field, relate to a preparing way for alumina crystal whisker material.
Background technology
Whisker is meant the single crystal fibre material of several microns of diameters, tens microns of length.It is big that it has length-to-diameter ratio, no crystal grain (limit) boundary, and number of defects is less than characteristics such as polycrystalline.Whisker is just because of this intrinsic integrity, and its intensity is not subjected to the strict restriction of its surface integrity, therefore has been endowed with polycrystalline fibre and has compared very tough and tensile and not crisp character with glass fibre.The kind of whisker has much at present, and alumina whisker is exactly wherein a kind of.It is with its good performance, as excellent mechanical intensity, Young's modulus, thermotolerance, covalency, chemicals-resistant with metal and noticeable.Alumina whisker is a kind of pottery whisker, has superior mechanical properties such as high strength, high elastic coefficient, and does not have the high temperature oxidation problem, and is good with the ceramic matrix material consistency, is considered to extremely rising inorganic salt crystal whisker materials.
The preparation method of alumina whisker has a lot, can be divided into vapor phase process, hydrothermal method, scorification and the method for fluxing from operational path.Vapor phase process be the aluminum metal steam in moistening hydrogen, 1300 ℃～1500 ℃ down reaction make alumina whisker; Hydrothermal method is Al (OH)
3Colloid obtains fibrous boehmite crystal grain in 250 ℃ of thermostat(t)ed water thermal treatment 4h in water heating kettle, again in 600～800 ℃ of following normal pressure calcining preparation alumina whiskers; Scorification be with aluminum oxide 2100 ℃ of following fusions, cooling generates alumina whisker; The rule of fluxing is to add fusing assistant in the material of aluminum oxide, grow into the whisker method under 1000～1200 ℃.The whisker that different preparation methods produces, its component and varying in size, yield does not wait yet.Vapor phase process is difficult to control in industrial operation, hydrothermal method is difficult to reach because step is many, not easy to operate, and the scorification melt temperature is too high, and therefore, it is more favourable that industrial employing flux method is produced alumina whisker.
But main at present material Tai-Ace S 150, aluminum nitrate, aluminum chloride, aluminium hydroxide etc. for aluminum oxide, fusing assistant is mainly used alkali metal sulfates, halogenide, carbonate and nitrate etc., and the shortcoming of this method maximum is that mixing time is long.
Summary of the invention
It is short to the purpose of this invention is to provide a kind of preparation cycle, product purity height, quality better, the preparation method of the aluminum oxide whisker material that yield is high.
The preparation method of order aluminum oxide whisker material of the present invention contains following processing step:
1. calcining process: with aluminum feedstock and the fusing assistant molar ratio ingredient with 1: 0.25～1: 12, both are mixed, mixed material adds in the roasting crucible and sends into stoving oven, at 900～1200 ℃ of following roasting 2～8h; Wherein aluminum feedstock adopts potassium aluminium sulfate KAl (SO
4)
2, fusing assistant can adopt vitriol, alkali metal chloride or carbonate, preferably sulfuric acid potassium.
The SO that calcining process produced
3Gas is through SO
3Absorption system absorbs, and obtains the byproduct vitriol oil.
2. leaching prosess: place distilled water to soak 4～24 hours cooled crucible of roasting and material, make material under heating condition, dissolve fusing assistant, the wet product of alumina whisker.The slip that dissolving is finished carries out the multiple times of filtration washing.
The mother liquor that leaching prosess obtains is sent into the crystallisation by cooling groove and is cooled to 30 ℃, filters through whizzer, obtains the byproduct vitriolate of tartar, and mother liquor returns leaching prosess.
3. drying process: will wet product in 70～120 ℃ down oven dry promptly get alumina whisker.
The present invention has following advantage compared to existing technology:
1 the present invention is with potassium aluminium sulfate KAl (SO
4)
2For for alumina source, be fusing assistant with the vitriolate of tartar, react and produce alumina whisker.Because potassium aluminium sulfate at high temperature can be decomposed into activated alumina and vitriolate of tartar, has reduced temperature of reaction and time effectively, only need to get final product at 900～1200 ℃ of following roasting 2～8h, shortened preparation time simultaneously, reduced energy consumption, reduced production cost.
2, alumina whisker product purity height, the quality better of the present invention's preparation, yield reaches more than 50%.Crystal whisker products is accredited as pure phase through X-ray diffraction, and mean diameter is 0.5～3 μ m, and mean length is 10～100 μ m.
3, the present invention's while by-product potassium product and the vitriol oil: the SO that calcining process produced
3Gas is through SO
3Absorption system absorbs, and obtains the byproduct vitriol oil; The mother liquor that leaching prosess obtains through crystallisation by cooling centrifuging, obtains the byproduct vitriolate of tartar.
4, Fa Ming technology is easy to control, and is simple to operate, preparation cycle is short, production cost is low, energy consumption is little, good product quality, is easy to realize large-scale industrial production.
Description of drawings
Fig. 1 is the SEM scintigram of the alumina whisker product of the embodiment of the invention 1 preparation
Fig. 2 is the SEM scintigram of the alumina whisker product of the embodiment of the invention 2 preparations
Fig. 3 is the SEM scintigram of the alumina whisker product of the embodiment of the invention 3 preparations
Embodiment
Embodiment 1,
1. calcining process: with potassium aluminium sulfate with the molar ratio ingredient of vitriolate of tartar with 1: 0.25, stir 0.5～1h and make its thorough mixing, put into the roasting crucible then, send into stoving oven, and at 1200 ℃ of following roasting 5h;
2. leaching prosess: place distilled water to soak 24 hours cooled crucible of roasting and material, make material under heating condition, dissolve vitriolate of tartar, the wet product of alumina whisker;
3. drying process: the product that will wet is put into baking oven, adjusts the temperature to 70 ℃, dries 12 hours, promptly gets alumina whisker.
The alumina whisker product is accredited as pure phase through X-ray diffraction.The whisker mean diameter is 0.5～3 μ m, and mean length is 10～100 μ m.
Embodiment 2,
1. calcining process: with potassium aluminium sulfate with the molar ratio ingredient of Repone K with 1: 5, stir 0.5～1h and make its thorough mixing, put into the roasting crucible then, send into stoving oven, and at 900 ℃ of following roasting 5h;
2. leaching prosess: place distilled water to soak 12 hours cooled crucible of roasting and material, make material under heating condition, dissolve Repone K, the wet product of alumina whisker;
3. drying process: the product that will wet is put into baking oven, adjusts the temperature to 100 ℃, dries 10 hours, promptly gets alumina whisker.
The alumina whisker product is accredited as pure phase through X-ray diffraction.The whisker mean diameter is 0.5～3 μ m, and mean length is 12～95 μ m.
Embodiment 3,
1. calcining process: with potassium aluminium sulfate with the molar ratio ingredient of salt of wormwood with 1: 10, stir 0.5～1h and make its thorough mixing, put into the roasting crucible then, send into stoving oven, and at 1100 ℃ of following roasting 5h;
2. leaching prosess: place distilled water to soak 24 hours cooled crucible of roasting and material, make material under heating condition, dissolve Repone K, the wet product of alumina whisker;
3. drying process: the product that will wet is put into baking oven, adjusts the temperature to 120 ℃, dries 8 hours, promptly gets alumina whisker.
The alumina whisker product is accredited as pure phase through X-ray diffraction.The whisker mean diameter is 0.5～3 μ m, and mean length is 18～108 μ m.
Claims (3)
1. the preparation method of an alumina whisker comprises following processing step:
1. roasting: aluminum feedstock and fusing assistant is even with 1: 0.25～1: 12 mixed in molar ratio, put into the roasting crucible, in 900～1200 ℃ of following roasting 2～8h;
2. molten soaking: place distilled water to soak 4～24 hours cooled sinter, get the wet product of alumina whisker;
3. dry: the product that will wet is dried down in 70～120 ℃ and is promptly got alumina whisker.
2. alumina whisker gets the preparation method according to claim 1, it is characterized in that: described aluminum feedstock is potassium aluminium sulfate KAl (SO
4)
2
3. the preparation method of alumina whisker according to claim 1, it is characterized in that: described fusing assistant is vitriol, alkali metal chloride or carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710018539 CN100503901C (en) | 2007-07-25 | 2007-07-25 | Process for producing aluminum oxide crystal whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710018539 CN100503901C (en) | 2007-07-25 | 2007-07-25 | Process for producing aluminum oxide crystal whisker |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101109106A true CN101109106A (en) | 2008-01-23 |
| CN100503901C CN100503901C (en) | 2009-06-24 |
Family
ID=39041359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710018539 Expired - Fee Related CN100503901C (en) | 2007-07-25 | 2007-07-25 | Process for producing aluminum oxide crystal whisker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100503901C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974782A (en) * | 2010-11-19 | 2011-02-16 | 昆明理工大学 | Method for preparing α-Al2O3 whiskers by carbothermal reduction method |
| CN103896317A (en) * | 2014-03-27 | 2014-07-02 | 洛阳威乐美科技有限公司 | Method for preparing aluminum oxide whiskers |
| CN104024161A (en) * | 2011-11-30 | 2014-09-03 | 尼尔奥克S.L. | Method for purifying alpha-alumina fibers |
| CN110904494A (en) * | 2019-12-20 | 2020-03-24 | 武汉工程大学 | Preparation method of alumina whisker |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351227B (en) * | 2011-09-26 | 2013-08-21 | 西安航天华威化工生物工程有限公司 | Method for extracting aluminum oxide from fly ash by one-step process |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1153731C (en) * | 2002-08-19 | 2004-06-16 | 西安华创纳米化合物技术研究发展有限责任公司 | Method for mfg. alumina nanofibre |
| CN1197775C (en) * | 2003-07-10 | 2005-04-20 | 复旦大学 | Process for preparing aluminium oxide nano fibre |
-
2007
- 2007-07-25 CN CN 200710018539 patent/CN100503901C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974782A (en) * | 2010-11-19 | 2011-02-16 | 昆明理工大学 | Method for preparing α-Al2O3 whiskers by carbothermal reduction method |
| CN101974782B (en) * | 2010-11-19 | 2013-01-02 | 昆明理工大学 | Method for preparing α-Al2O3 whiskers by carbothermal reduction method |
| CN104024161A (en) * | 2011-11-30 | 2014-09-03 | 尼尔奥克S.L. | Method for purifying alpha-alumina fibers |
| CN104024161B (en) * | 2011-11-30 | 2016-08-17 | 纽卡有限公司 | Method for purification of alpha-alumina fibre |
| CN103896317A (en) * | 2014-03-27 | 2014-07-02 | 洛阳威乐美科技有限公司 | Method for preparing aluminum oxide whiskers |
| CN110904494A (en) * | 2019-12-20 | 2020-03-24 | 武汉工程大学 | Preparation method of alumina whisker |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100503901C (en) | 2009-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102849790B (en) | Preparation method of columnar potassium hexatitanate | |
| CN101338448B (en) | Hydrothermal preparation method for aluminum oxide whiskers at low temperature | |
| CN101935877A (en) | A method for synthesizing mullite whiskers by atmospheric pressure sintering | |
| CN100503901C (en) | Process for producing aluminum oxide crystal whisker | |
| CN102390864A (en) | Preparation method of flaky potassium hexatitanate | |
| CN101311372A (en) | Low-temperature molten salt thermal inversion preparation method of aporate-crystal antifungin whiskers | |
| CN102787355A (en) | A kind of preparation method of α-Bi2O3 single crystal microrod | |
| CN104477934A (en) | Method for low-temperature synthesis of pollucite | |
| CN102839424B (en) | Method for preparing potassium hexatitanate whisker | |
| CN106801256A (en) | A kind of method that solid phase method prepares potassium hexatitanate platelet | |
| CN102230223B (en) | Method for preparing magnesium potassium titanate by directly utilizing magnesium oxide | |
| CN107460545B (en) | A kind of preparation method of rod-shaped zirconia whiskers | |
| CN103318954B (en) | Method for preparing sodium trititanate nanorods through solid-phase chemical reaction | |
| CN103204524A (en) | Preparation method of magnesium oxide porous fiber | |
| CN101250751A (en) | A kind of method for preparing potassium hexatitanate whisker | |
| CN103882558B (en) | A kind of perovskite structure AgNbO 3fiber and preparation method thereof | |
| CN104961137A (en) | Method for preparing nanometer alkaline-earth metal boride | |
| CN113461054B (en) | BiOCl powder and preparation method and application thereof | |
| CN107916452A (en) | A kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern | |
| CN105036167A (en) | Calcium hexaluminate and preparation method thereof | |
| CN104176759B (en) | One prepares a cube block CeO 2the molte-salt synthesis of nano material | |
| CN101660204A (en) | Preparation method of hexagonal piece aluminum oxide whisker material | |
| CN102716701A (en) | Method for preparing nickel-doped bismuth silicon oxide microspheres by ultrasonic spray | |
| CN108315810A (en) | A method of using kaliophilite as Material synthesis mullite crystal whisker | |
| CN101700979A (en) | Method for preparing nano-mullite powder by sol-gel-sonic chemical method |
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: 20090624 Termination date: 20120725 |