CN101935877A - Method for synthesizing mullite whiskers by normal pressure sintering - Google Patents
Method for synthesizing mullite whiskers by normal pressure sintering Download PDFInfo
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- CN101935877A CN101935877A CN201010270806.4A CN201010270806A CN101935877A CN 101935877 A CN101935877 A CN 101935877A CN 201010270806 A CN201010270806 A CN 201010270806A CN 101935877 A CN101935877 A CN 101935877A
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- mullite
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 title claims abstract description 11
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000013078 crystal Substances 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 10
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 6
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 230000002708 enhancing effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 10
- 230000003014 reinforcing effect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910016569 AlF 3 Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 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 2
- 230000004913 activation Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
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Abstract
The invention relates to a method for synthesizing mullite whiskers by normal pressure sintering. A second phase whisker material capable of enhancing and toughening a metal or ceramic matrix at the temperature of over 1,200 DEG C is prepared by using the high-temperature creep resistance of the mullite whiskers. The method for synthesizing the mullite whiskers by the normal pressure powder sintering has simple process; and the synthesized mullite whiskers have the advantages of high dispersion degree, uniform granule size distribution and high length-diameter ratio and purity, and can be used as enhancing and toughening whiskers for metal and ceramic materials.
Description
Technical field
The present invention relates to a kind of method of normal pressure-sintered mullite synthesizing whisker, belong to field of material preparation.
Background technology
Mullite crystal whisker is owing to have outstanding advantages such as high temperature resistant, wear-resistant, anti-oxidant, that thermal expansivity is low, thermal shock resistance is good, and its excellent high-temperature creep resistance makes it be particularly suitable as hot environment to use with the toughness reinforcing whisker of the enhancing of metal, stupalith.
About existing many documents of the preparation of mullite crystal whisker and patent report.Japan Okada etc. are with the Al of tetraethoxy and aluminum nitrate preparation
2O
3-SiO
2Xerogel, same AlF
3In airtight container the calcining synthesized mullite crystal whisker (referring to Materials science communication .8[9] (1989): 1052-1054).This method adopts tetraethoxy and aluminum nitrate to cost an arm and a leg, preparation collosol and gel complex procedures, and the operational cycle is long.China applies for a patent CN92102982.9 and discloses a kind of high purity mullite crystal whisker preparation method, and this method is dissolved in aluminium salt in the alcoholic solution, presses SiO
2: Al
2O
3=2: 3 mol ratio drips the alkoxide of silicon, and adds HF solution, with the gel oven dry that obtains, broken, sieve, calcine, obtain the mullite crystal whisker of various length-to-diameter ratios at last.This method preparation process adopts twice calcining, big and its complicated process of preparation of energy consumption, and the mullite crystal whisker productive rate is not high.United States Patent (USP) 4910172 and 4948766 discloses with powder sintering (Al
2O
3, SiO
2, AlF
3) preparation mullite crystal whisker method.The mullite crystal whisker skewness that this method is prepared, the calcining temperature height, the mullite crystal whisker length-to-diameter ratio that grows is shorter.Xu Xiaohong etc. are with kaolin, industrial aluminium hydroxide, AlF
3, V
2O
5For the synthetic preparation of raw material original position mullite crystal whisker (referring to original position mullite synthesizing whisker and Study on Microstructure, Wuhan University of Technology's journal, 2007,28 (2): 89-92).The mullite crystal whisker that this method is prepared impure many, purity is low, is difficult to be applied to strengthen toughness reinforcing metal, stupalith.
The present invention is that the gas that utilizes aluminum fluoride at high temperature to form carries out gas-solid reaction, help the crystalline different growth, synthetic whisker according to the specific direction growth, Vanadium Pentoxide in FLAKES will volatilize and promote gas-solid reaction in high-temperature heating process mass transfer process and activation increase aluminum oxide lattice imperfection, the activation lattice promotes mullite to form.The whisker of growing among the present invention is grown by following gas-solid reaction.
Al(OH)
3→Al
2O
3+H
2O
(1)
6AlF
3+3O
2→6AlOF+12F (2)
Al
2O
3+2F→2AlOF+0.5O
2 (3)
2SiO
2+8F→2SiF4+2O
2 (4)
6AlOF+2SiF
4+3.5O
2→3Al
2O
3·2SiO
2+14F (5)
The mullite that generates in this reaction process is separated out nucleation reach certain saturation degree in the aluminum fluoride high-temperature gas after, and the mullite nucleus forms the rod-like mullite whisker according to the growth of crystal growth habit plane under the gaseous environment that gas provides.
Summary of the invention
The object of the present invention is to provide a kind of method of normal pressure-sintered mullite synthesizing whisker, utilize the normal pressure-sintered method mullite synthesizing of powder whisker, utilize the high-temperature creep resistance of mullite crystal whisker, preparation can be at the second phase crystal whisker materials that is used to strengthen toughness reinforcing metal, ceramic matrix more than 1200 ℃.
The present invention is achieved through the following technical solutions
Raw material and additive are formed and mass percent
Primary industry aluminium hydroxide 75.5%-85.5%, silica 1 4.5%-24.5%, total amount is 100%,
The additive aluminum fluoride is the 2-6% of raw material weight, Vanadium Pentoxide in FLAKES be raw material weight 2-6%;
Finish according to the following steps according to above-mentioned formulation mullite crystal whisker
(1) ball milling: raw material and additive are prepared burden by the mass percent of prescription, and press raw material again: alcohol: ball=1-4: 4-8: 8-12 adds in the ball mill, carries out wet ball grinding 6-10h, obtains the powder that granularity is 75-100um, and alcohol is ball-milling medium;
(2) oven dry: the powder that ball milling is good is in baking oven, and under 80-100 ℃, oven dry 4-6h sloughs the alcohol in the powder behind the ball milling, obtains the powder that mixes;
(3) mix grinding: add the 3-5% of raw material weight in the powder that mixes, concentration expressed in percentage by weight is the polyvinyl alcohol solution (PVA) of 10-15%, with going into ageing 12-24h in the encloses container behind the grinding rod mixed grinding 15-45min;
(4) compressing tablet: the pressure with 15-25MPa on the powder type tabletting machine of the powder after the ageing is pressed into the sheet stock of diameter * highly=10-15mm * 5-10mm;
(5) sintering: the sheet stock that presses is placed in the airtight alumina-ceramic crucible, temperature rise rate with 3-5 ℃/min in retort furnace is raised to 800-1000 ℃ from room temperature, behind the heat preservation sintering 1-2h, temperature rise rate with 5-10 ℃/min is raised to 1250 ℃ of-1450 ℃ of heat preservation sintering 2-3h again, furnace cooling obtains the mullite crystal whisker product.
The invention has the advantages that: mullite crystal whisker simple by its technology of normal pressure powder sintering mullite synthesizing whisker, that synthesize have degree of scatter height, size distribution evenly, length-to-diameter ratio and purity advantage of higher, can well use as the toughness reinforcing whisker of the enhancing of metal, stupalith.
Description of drawings
Fig. 1,2 is that the electron microscope scanning of embodiment 1 mullite crystal whisker product structure shows figure; Fig. 3 is that the electron microscope scanning of embodiment 2 mullite crystal whisker product structures shows figure.
Embodiment
Embodiment 1: raw material adopts industrial aluminium hydroxide 75.5%, silicon-dioxide 24.5%, add 4% Vanadium Pentoxide in FLAKES of 2% aluminum fluoride of raw materials quality and raw materials quality, by raw material: alcohol: ball=add planetary ball mill carry out wet ball grinding 8h at 2: 4: 8, obtain the mixed powder that granularity is 75-100um, the powder that ball milling is good is dried 4h down at 100 ℃ in baking oven, slough the alcohol in the powder behind the ball milling, obtain the powder that mixes; 3% concentration expressed in percentage by weight that again this powder is added raw materials quality is 15% polyvinyl alcohol solution mixing, with behind the grinding rod mixed grinding 25min, behind the ageing 24h, be pressed into the sheet stock of 10-15mm * 5-10mm with the powder type tabletting machine, putting into airtight alumina-ceramic crucible again reenters retort furnace and is raised to 800 ℃ with the temperature rise rate of 3 ℃/min from room temperature, behind the insulation 2h, be raised to 1250 ℃ and be incubated 3h with 5 ℃/min temperature rise rate again, furnace cooling promptly gets the mullite crystal whisker product afterwards.The mullite crystal whisker good dispersion that generates, whisker length is 20-30 μ m, and diameter is 1.5-2 μ m, and length-to-diameter ratio reaches 12-15, is applicable to strengthen toughness reinforcing metal, stupalith.See Fig. 1, Fig. 2.
Embodiment 2: raw material adopts industrial aluminium hydroxide 80.5%, silica 1 9.5%, additive aluminum fluoride and Vanadium Pentoxide in FLAKES are respectively 6% and 2% of raw materials quality, wet ball grinding in planetary ball mill, the powder that acquisition mixes, dry by the fire 6h down at 80 ℃, this powder being added 4% concentration expressed in percentage by weight again and be 12% polyvinyl alcohol solution mixes with after going in the encloses container also ageing 18h behind the grinding rod mixed grinding 40min, be pressed into the sheet stock of 10-15mm * 5-10mm with the powder type tabletting machine, be placed on to reenter in the retort furnace in the airtight alumina-ceramic crucible and be raised to 900 ℃ from room temperature with 4 ℃/min temperature rise rate, behind the insulation 1.5h, be raised to 1350 ℃ and be incubated 2.5h with 8 ℃/min temperature rise rate again, the sample furnace cooling promptly obtains the product of wanting afterwards.Scanning electronic microscope shows, the mullite crystal whisker good dispersion of generation, and whisker length is 50-70 μ m, and diameter is 2.5-4 μ m, and length-to-diameter ratio reaches 15-20, is applicable to strengthen toughness reinforcing metal, stupalith, sees Fig. 3.
Claims (1)
1. the method for a normal pressure-sintered mullite synthesizing whisker, it is characterized in that: the present invention is achieved through the following technical solutions,
1), raw material and additive are formed and mass percent
Primary industry aluminium hydroxide 75.5%-85.5%, silica 1 4.5%-24.5%, total amount is 100%,
The additive aluminum fluoride is the 2-6% of raw material weight, Vanadium Pentoxide in FLAKES be raw material weight 2-6%;
2), finish according to the following steps according to above-mentioned formulation mullite crystal whisker
(1), ball milling: raw material and additive are prepared burden by the mass percent of prescription, and press raw material again: alcohol: ball=1-4: 4-8: 8-12 adds in the ball mill, carries out wet ball grinding 6-10h, obtains the powder that granularity is 75-100um, and alcohol is ball-milling medium;
(2), oven dry: the powder that ball milling is good is in baking oven, and under 80-100 ℃, oven dry 4-6h sloughs the alcohol in the powder behind the ball milling, obtains the powder that mixes;
(3), mix grinding: add the 3-5% of raw material weight in the powder that mixes, concentration expressed in percentage by weight is the polyvinyl alcohol solution of 10-15%, with going into ageing 12-24h in the encloses container behind the grinding rod mixed grinding 15-45min;
(4), compressing tablet: the pressure with 15-25MPa on the powder type tabletting machine of the powder after the ageing is pressed into the sheet stock of diameter * highly=10-15mm * 5-10mm;
(5), sintering: the sheet stock that presses is placed in the airtight alumina-ceramic crucible, temperature rise rate with 3-5 ℃/min in retort furnace is raised to 800-1000 ℃ from room temperature, behind the heat preservation sintering 1-2h, temperature rise rate with 5-10 ℃/min is raised to 1250 ℃-1450 ℃ again, heat preservation sintering 2-3h, furnace cooling obtains the mullite crystal whisker product.
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| CN2010102708064A CN101935877B (en) | 2010-09-03 | 2010-09-03 | Method for synthesizing mullite whiskers by normal pressure sintering |
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| CN105036720A (en) * | 2015-07-28 | 2015-11-11 | 景德镇陶瓷学院 | Preparation method for synthesizing mullite whiskers through adopting borides as additives |
| CN105084878A (en) * | 2015-03-31 | 2015-11-25 | 海南大学 | Preparation method of acicular mullite porous ceramic block material with superhigh amount of porosity |
| CN105088345A (en) * | 2015-07-28 | 2015-11-25 | 景德镇陶瓷学院 | Preparation method for utilizing desert sand to synthesize mullite whiskers at low temperature |
| CN106167413A (en) * | 2016-07-06 | 2016-11-30 | 江西省工业陶瓷工程技术研究中心 | A kind of toughness reinforcing 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker and preparation method |
| CN106630987A (en) * | 2016-09-19 | 2017-05-10 | 齐鲁工业大学 | Oxide catalyst for preparation of mullite ceramic whiskers |
| CN106915749A (en) * | 2017-04-07 | 2017-07-04 | 武汉科技大学 | A kind of rod-like mullite tabular alumina composite granule and preparation method thereof |
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| CN105088345B (en) * | 2015-07-28 | 2017-09-19 | 景德镇陶瓷大学 | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker |
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| CN108315810A (en) * | 2018-02-24 | 2018-07-24 | 陕西大秦钾业有限公司 | A method of using kaliophilite as Material synthesis mullite crystal whisker |
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