CN101935877B - Method for synthesizing mullite whiskers by normal pressure sintering - Google Patents
Method for synthesizing mullite whiskers by normal pressure sintering Download PDFInfo
- Publication number
- CN101935877B CN101935877B CN2010102708064A CN201010270806A CN101935877B CN 101935877 B CN101935877 B CN 101935877B CN 2010102708064 A CN2010102708064 A CN 2010102708064A CN 201010270806 A CN201010270806 A CN 201010270806A CN 101935877 B CN101935877 B CN 101935877B
- Authority
- CN
- China
- Prior art keywords
- powder
- raw material
- ball
- mullite
- grinding
- 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.)
- Expired - Fee Related
Links
- 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 19
- 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 21
- 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 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
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 229910021502 aluminium hydroxide Inorganic materials 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 9
- 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
- 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
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
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 is particularly suitable for as hot environment with the toughness reinforcing whisker use of the enhancing of metal, stupalith it.
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
3Calcining has been synthesized mullite crystal whisker (referring to Materials science communication .8 [9] (1989): 1052-1054) in airtight container.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 prepares process and adopts twice calcining, big and its complicated process of preparation of energy consumption, and the mullite crystal whisker productive rate is not high.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, calcining temperature is high, and 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 ALUMNIUM 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 through 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 after in the ALUMNIUM FLUORIDE high-temperature gas, reaching certain saturation degree, 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 realizes through following technical proposals
Raw material and additive are formed and mass percent
Primary industry white lake 75.5%-85.5%, silica 1 4.5%-24.5%, total amount is 100%,
The additive ALUMNIUM FLUORIDE is the 2-6% of raw material weight, Vanadium Pentoxide in FLAKES be raw material weight 2-6%;
Accomplish 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: in the powder that mixes, add the 3-5% of raw material weight, 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, and furnace cooling obtains the mullite crystal whisker product.
The invention has the advantages that: mullite crystal whisker simple through 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%, and silicon-dioxide 24.5% adds 4% Vanadium Pentoxide in FLAKES of 2% ALUMNIUM FLUORIDE and the raw materials quality of 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 that 15% polyvinyl alcohol solution mixes; 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, put into airtight alumina-ceramic crucible again and reenter retort furnace and be raised to 800 ℃ from room temperature with the temperature rise rate of 3 ℃/min; 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%, and silica 1 9.5%, additive ALUMNIUM 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, at 80 ℃ of following baking 6h, again this powder being added 4% concentration expressed in percentage by weight is that 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, behind the insulation 1.5h, be raised to 1350 ℃ and be incubated 2.5h with 8 ℃/min temperature rise rate again with 4 ℃/min temperature rise rate; The sample furnace cooling promptly obtains the product of wanting afterwards.Sem 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 is characterized in that: the present invention realizes through following technical proposals,
1), raw material and additive are formed and mass percent
Raw material: industrial aluminium hydroxide 75.5%-85.5%, silica 1 4.5%-24.5%, total amount is 100%,
Additive: ALUMNIUM FLUORIDE is the 2-6% of raw material weight, Vanadium Pentoxide in FLAKES be raw material weight 2-6%;
2), accomplish 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: in the powder that mixes, add the 3-5% of raw material weight, 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, the temperature rise rate with 5-10 ℃/min is raised to 1250 ℃-1450 ℃, heat preservation sintering 2-3h again; Furnace cooling obtains the mullite crystal whisker product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102708064A CN101935877B (en) | 2010-09-03 | 2010-09-03 | Method for synthesizing mullite whiskers by normal pressure sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102708064A CN101935877B (en) | 2010-09-03 | 2010-09-03 | Method for synthesizing mullite whiskers by normal pressure sintering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101935877A CN101935877A (en) | 2011-01-05 |
| CN101935877B true CN101935877B (en) | 2012-05-23 |
Family
ID=43389435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102708064A Expired - Fee Related CN101935877B (en) | 2010-09-03 | 2010-09-03 | Method for synthesizing mullite whiskers by normal pressure sintering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101935877B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN105036720B (en) * | 2015-07-28 | 2017-03-08 | 景德镇陶瓷大学 | A kind of preparation method by the use of boride as additive mullite synthesizing whisker |
| CN106167413B (en) * | 2016-07-06 | 2018-09-28 | 江西省工业陶瓷工程技术研究中心 | A kind of 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker toughening 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 |
| CN106915749B (en) * | 2017-04-07 | 2019-03-01 | 武汉科技大学 | A kind of rod-like mullite-tabular alumina composite granule and preparation method thereof |
| CN108315810B (en) * | 2018-02-24 | 2020-09-22 | 陕西大秦钾业有限公司 | Method for synthesizing mullite whisker by taking kaliophilite as raw material |
| CN108484149B (en) * | 2018-03-30 | 2020-12-01 | 滁州学院 | Preparation method of NaA molecular sieve membrane support |
| CN108854589B (en) * | 2018-07-10 | 2020-06-26 | 天津工业大学 | Mullite whisker hollow fiber membrane for oil-water separation and preparation method thereof |
| CN110938862A (en) * | 2019-12-23 | 2020-03-31 | 苏州纳迪微电子有限公司 | High-purity monocrystalline corundum powder and preparation method thereof |
| CN111659855A (en) * | 2020-05-21 | 2020-09-15 | 上海交通大学 | Preparation method of mullite whisker reinforced ceramic shell for directional solidification of NbSi alloy generated in situ |
| CN112280538B (en) * | 2020-10-28 | 2021-11-16 | 武汉科技大学 | Whisker toughened phase change heat storage microcapsule and preparation method thereof |
| CN115521135B (en) * | 2022-09-19 | 2023-08-25 | 杭州诺贝尔陶瓷有限公司 | Preparation method of lightweight building ceramic tile |
| CN115650762A (en) * | 2022-09-27 | 2023-01-31 | 深圳市吉迩科技有限公司 | Ceramic slurry and preparation method of porous ceramic atomizing core |
| CN116063066A (en) * | 2023-01-31 | 2023-05-05 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of mullite ceramic material reinforced by gas phase infiltration method |
| CN116375455B (en) * | 2023-04-10 | 2024-05-28 | 萍乡市江华环保设备填料有限公司 | Preparation method of alumina ceramic propping agent with ultralow volatility coefficient by high-temperature sintering |
| CN116589269A (en) * | 2023-04-19 | 2023-08-15 | 福建省云智新材料科技有限公司 | Preparation method and application of mullite whisker |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01212299A (en) * | 1988-02-17 | 1989-08-25 | Kiyoshi Okada | Production of mullite whisker |
| US4948766A (en) * | 1988-08-05 | 1990-08-14 | The United States Of America As Represented By The Secretary Of The Navy | Rigid mullite=whisker felt and method of preparation |
| US4910172A (en) * | 1989-02-08 | 1990-03-20 | The United States Of America As Represented By The Secretary Of The Navy | Preparation of mullite whiskers from AlF3, SiO2, and Al2 O3 powders |
| CN1028776C (en) * | 1992-04-30 | 1995-06-07 | 清华大学 | Process for preparation of highly pure mullite crystal whisker |
| CN100551869C (en) * | 2007-07-17 | 2009-10-21 | 昆明理工大学 | The ceramic-base wave-permeation supporting body and the production method that are used for microwave heating |
| CN100497762C (en) * | 2007-07-25 | 2009-06-10 | 濮阳濮耐高温材料（集团）股份有限公司 | Method for preparing mullite crystal whisker from coal refuse and aluminum oxide |
-
2010
- 2010-09-03 CN CN2010102708064A patent/CN101935877B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101935877A (en) | 2011-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101935877B (en) | Method for synthesizing mullite whiskers by normal pressure sintering | |
| CN101498049B (en) | Method for preparing mullite crystal whisker by non-hydrolytic sol-gel process | |
| CN107640776B (en) | Preparation method of MFI molecular sieve with micro-mesoporous structure | |
| CN107522404B (en) | Dental lithium-aluminum-silicon microcrystalline glass and preparation method thereof | |
| Ma et al. | Low cost synthesis of mesoporous molecular sieve MCM-41 from wheat straw ash using CTAB as surfactant | |
| CN114455952B (en) | AlON powder, direct nitridation method high-pressure synthesis method and application thereof | |
| CN101845668B (en) | Method for preparing nano nickel borate whiskers | |
| CN101531520A (en) | Method for preparing gamma-AlON ceramic powder based on carbon thermal reduction nitridation | |
| CN102275942A (en) | Preparation method of bismuth silicate nanopowder | |
| CN108640676B (en) | Preparation of pyrochlore structure Bi by solid-phase reaction method2Ti2O7Method for producing ceramic | |
| CN107285332B (en) | Synthesis method of ZSM-22 molecular sieve and ZSM-22 molecular sieve synthesized by same | |
| CN101391796A (en) | Method for preparing yttrium silicate nano powder | |
| CN110590389A (en) | Silicon nitride whisker-aluminum nitride-corundum ternary composite ceramic material using natural minerals as raw materials and preparation method thereof | |
| CN108585887A (en) | A kind of TixZr1-xB2Superhigh temperature solid solution ceramic raw powder's production technology | |
| CN109574680A (en) | A kind of method that gas-solid reaction combination lqiuid phase sintering method prepares porous silicon nitride ceramic | |
| CN101555619A (en) | Preparation method of controllable yttrium silicate nano-rod | |
| CN101700977A (en) | Method for rapidly preparing MgAlON transparent ceramic powder | |
| CN101717262B (en) | Method for preparing nano mullite powder by sol-gel and solvothermal method | |
| CN100503901C (en) | Process for producing aluminum oxide crystal whisker | |
| CN108892476A (en) | Porous cordierite and its preparation method and application | |
| CN101700980B (en) | Method for preparing nano-mullite powder by sol-gel-hydrothermal method | |
| CN114538913B (en) | Pure-phase nano MgAl with high sintering activity 2 O 4 Powder and preparation method and application thereof | |
| CN104073918A (en) | Method for synthesizing polycrystalline mullite fibers under low temperature condition | |
| CN108212134B (en) | Catalyst carrier containing silicon boehmite and preparation method thereof | |
| CN109811415A (en) | A method of from kaolin low temperature preparation mullite crystal whisker |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120523 Termination date: 20140903 |
|
| EXPY | Termination of patent right or utility model |