CN116589269A - Preparation method and application of mullite whisker - Google Patents
Preparation method and application of mullite whisker Download PDFInfo
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- CN116589269A CN116589269A CN202310422781.2A CN202310422781A CN116589269A CN 116589269 A CN116589269 A CN 116589269A CN 202310422781 A CN202310422781 A CN 202310422781A CN 116589269 A CN116589269 A CN 116589269A
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- aluminum
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- mullite
- containing compound
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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 51
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 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 abstract description 17
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000012798 spherical particle Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 238000001694 spray drying Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000011265 semifinished product Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 229940118662 aluminum carbonate Drugs 0.000 claims description 6
- PBZOHMHCJBXLTP-UHFFFAOYSA-K aluminum;acetic acid;triacetate Chemical compound [Al+3].CC(O)=O.CC([O-])=O.CC([O-])=O.CC([O-])=O PBZOHMHCJBXLTP-UHFFFAOYSA-K 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- -1 aluminum alkoxide Chemical class 0.000 claims description 4
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000003014 reinforcing effect Effects 0.000 claims description 4
- 230000002572 peristaltic effect Effects 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 2
- 239000007790 solid phase Substances 0.000 abstract description 2
- 238000011049 filling Methods 0.000 description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 239000004576 sand Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000002783 friction material Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction 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
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/6224—Fibres based on silica
- C04B35/62245—Fibres based on silica rich in aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/34—Silicates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method and application of mullite whiskers, comprising the following steps: step (1): mixing a high-purity active aluminum-containing compound, active silicon dioxide and aluminum fluoride according to a proportion by a wet method, grinding by a sanding mixer, and preparing spherical particles from the fully ground materials by a spray drying process to obtain a precursor A; step (2): fully drying the precursor A in a bowl, charging the dried material into a furnace, and sintering at high temperature to obtain a semi-finished product B; step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker. The preparation method adopts the active aluminum-containing compound, the active silicon oxide and the aluminum fluoride as raw materials, prepares the precursor through liquid-phase grinding, and then prepares the mullite whisker material through a solid-phase sintering process.
Description
Technical Field
The invention belongs to the field of ceramic materials, and relates to a preparation method of mullite whiskers.
Background
Whiskers are a single crystal in the form of fibers having a diameter of less than a few microns to tens of microns and a length of up to a few centimeters. It can be produced in nature or made by man-made. As the crystal of the whisker is complete, the whisker does not contain defects such as holes, dislocation, particle interfaces and the like existing in common materials, has highly ordered atomic arrangement, has density and strength close to theoretical values of ideal crystals, and has extremely high strength and elastic modulus.
Whiskers are mainly used as reinforcements for composite materials to reinforce, metals, ceramics, resins, glass, and the like. In the aerospace field, whisker reinforced metal-based and resin-based composites are useful as rotors, wings and tails of helicopters, space shells, aircraft landing gear and other aerospace parts due to their light weight and high specific strength. The whisker is also used as medical material, sports equipment, special functional material, etc.
Methods for preparing whiskers generally include gas phase methods, liquid phase methods and solid phase methods. Various whiskers adopt different preparation methods, and metal whiskers adopt a hydrogen reduction method of metal salt or an evaporation and condensation method of metal; the preparation method of the oxide whisker comprises a vapor transfer method and a chemical vapor phase growth method; siC, si 3 N 4 、TiN、TiB 2 Ceramic material whiskers such as AlN and the like are generally prepared by a chemical vapor phase method.
Mullite (or mullite, aluminum silicate) refers to a series of minerals consisting of aluminosilicates collectively called, notably SiO 2 -Al 2 O 3 The ceramic is the most important binary system in ceramics, ten or more different phase diagrams are sequentially published from the first mullite phase diagram published in 1909, the focus of the debate is that the intermediate mullite is a stable compound or an unstable compound, the later problems are unified, the mullite component is not fixed, and the alumina content of the mullite fluctuates between 72% and 78%. Mullite is a good refractory material and is a rare mineral of this type. Mullite is a mineral that aluminosilicates produce at high temperatures and forms mullite when the aluminosilicates are artificially heated. The natural mullite crystals are long and thin needle-shaped and are in radial cluster shape. Mullite ores are used to produce high temperature refractory materials. The C/C composite material is widely used as a thermal barrier coating. Mullite AI 2 O 3 -SiO 2 A binary solid solution stable under normal pressure in a primary system has a chemical formula of AI 2 O 3 -SiO 2 The natural mullite is very little, and is usually artificially synthesized by a sintering method, an electric melting method and the like. The ceramic material has the characteristics of high temperature resistance, high strength, small heat conductivity coefficient, obvious energy saving effect and the like, is suitable for lining of petroleum cracking furnaces, metallurgical hot blast stoves, ceramic roller kilns, tunnel kilns, electroceramic drawer kilns, glass crucible kilns and various electric furnaces, can be directly contacted with flame, is detected and used by related technical supervision departments, and achieves the technical indexes of similar foreign products. Mullite has the advantages of high temperature resistance, oxidation resistance, small thermal expansion coefficient, high-temperature strength, good thermal shock resistance and the like, and is an important engineering material. Mullite whisker as one kind of reinforced and toughened material for ceramic base, metal base and polymer base composite material may be used widely in high temperature structural material, friction material and other fields.
Mullite whisker as one kind of reinforced and toughened material for ceramic base, metal base and polymer base composite material may be used widely in high temperature structural material, friction material and other fields.
Disclosure of Invention
The published data show that in the mullite whisker preparation process, the main raw materials used are silicate, aluminum nitrate, fluoride salt and other raw materials, and the finished powder is prepared by adopting a solid phase method. According to the preparation method, the silicon source material is expensive, the mixing uniformity is insufficient, the aluminum source material has large volatilization of corrosive gas, and the overflow of nitrogen oxides is large, so that the environment is damaged, and the large-scale preparation is not facilitated.
The invention provides a mullite whisker preparation method, which adopts active alumina and acid
According to the preparation method of the mullite whisker, the molar ratio of aluminum to silicon in the mullite whisker is 2.5-3.1, the diameter is 1-4 mu m, the length is 7-26 mu m, and the length-diameter ratio is 4-15.
The invention provides a preparation method of mullite whiskers, which comprises the following steps:
step (1): mixing a high-purity active aluminum-containing compound, active silicon dioxide and aluminum fluoride according to a proportion by a wet method, grinding by a sanding mixer, and preparing spherical particles from the fully ground materials by a spray drying process to obtain a precursor A;
step (2): and (3) filling the precursor A into a pot, fully drying, filling the dried material into a furnace, and sintering at a high temperature to obtain a semi-finished product B.
Step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
In the step (1), the dosage of the high-purity active aluminum-containing compound and the active silicon dioxide is 2.5-3 according to the molar ratio of aluminum element to silicon element: 1, and the aluminum fluoride accounts for 10 to 25 percent of the total mass of the powder. The mass concentration of the high-purity activity is more than 99%.
In the step (1), the purity of the high-purity active aluminum-containing compound, the purity of the active silicon dioxide and the purity of the aluminum fluoride are all more than 99.9%, the high-purity active aluminum-containing compound is formed by mixing active aluminum oxide with other aluminum-containing compounds according to any proportion, and the other aluminum-containing compounds adopt at least one of aluminum carbonate, organic aluminum alkoxide, aluminum oxalate, aluminum tetraacetate and aluminum hydroxide.
In the step (1), the crystal form of the activated alumina is gamma-alumina, the activated silica is amorphous silica, and the specific surface area is between 10 and 100m 2 /g。
In the step (1), the high-purity activated alumina and other aluminum-containing compounds can be mixed in any mass ratio, and preferably, the mass ratio of the high-purity activated alumina to the other aluminum-containing compounds is 1:2-5.
In the step (1), water is adopted as a dispersion medium for wet mixing, and the solid content of the slurry is 40-60%.
In the step (1), the sand milling and mixing are carried out for 2-4 hours, and the particle size after grinding is 200-500 nanometers.
In the step (1), the air inlet temperature of the spray drying process is 200-220 ℃, the air outlet temperature is 70-90 ℃, the spray speed is 10000-15000 r/min, and the peristaltic feeding is 300-600 ml/min.
In the step (2), the sintering temperature is 1200-1400 ℃ and the sintering time is 2-4 hours.
The invention also provides the mullite whisker used as a reinforcing and toughening material in Zn 2 TiO 4 /K 2 SiO 3 The coating material is applied to the coating material.
The invention also provides application of the mullite whisker in a mullite sagger as a reinforcing and toughening material.
The preparation method adopts the active aluminum-containing compound, the active silicon oxide and the aluminum fluoride as raw materials, prepares the precursor through liquid-phase grinding, and then prepares the mullite whisker material through a solid-phase sintering process.
Drawings
Fig. 1 is an SEM image of mullite whiskers prepared according to example 1.
Fig. 2 is an SEM image of mullite whiskers prepared according to example 2.
Fig. 3 is an SEM image of mullite whiskers prepared according to example 3.
Fig. 4 is an SEM image of mullite whiskers prepared according to example 4.
Fig. 5 is an XRD pattern of mullite whiskers prepared according to example 1.
Description of the embodiments
Preferred embodiments of the present invention will be described in further detail below with reference to the attached drawings:
example 1
Step (1): mixing high-purity active aluminum oxide, aluminum hydroxide, active silicon dioxide and aluminum fluoride according to a proportion by wet method, wherein the molar ratio of aluminum to silicon is 2.5:1, the mass ratio of the high-purity active aluminum oxide to the aluminum hydroxide is 1:2, and the aluminum fluoride accounts for 10% of the total mass of the powder. Grinding for 2 hours by adopting a sand mill mixer, preparing spherical particles by adopting a spray drying process from the fully ground material, and obtaining a precursor A, wherein the particle size of the spherical particles is 200 nanometers after grinding.
Step (2): and (3) filling the precursor A into a pot for full drying, filling the dried material into a furnace, and sintering at a high temperature of 1200 ℃ for 2 hours to obtain a semi-finished product B.
Step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
Example 2
Step (1): mixing high-purity active aluminum oxide, aluminum carbonate, organic aluminum alkoxide, aluminum hydroxide, active silicon dioxide and aluminum fluoride according to a proportion by wet method, wherein the molar ratio of aluminum to silicon is 3:1, high-purity active aluminum oxide, aluminum carbonate, organic aluminum alkoxide and aluminum hydroxide with the mass ratio of 1:1:1:2, wherein aluminum fluoride accounts for 25% of the total mass of the powder. Grinding for 4 hours by adopting a sand mill mixer, preparing spherical particles by adopting a spray drying process from the fully ground material, and obtaining a precursor A, wherein the particle size of the spherical particles is 500 nanometers after grinding.
Step (2): and (3) filling the precursor A into a pot, fully drying, filling the dried material into a furnace, and sintering at a high temperature of 1400 ℃ for 4 hours to obtain a semi-finished product B.
Step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
Example 3
Step (1): mixing high-purity active aluminum oxide, aluminum oxalate, aluminum tetraacetate, aluminum hydroxide, active silicon dioxide and aluminum fluoride according to a proportion by wet method, wherein the molar ratio of aluminum to silicon is 2.9:1, high-purity active aluminum oxide, aluminum oxalate and aluminum tetraacetate, wherein the mass ratio of aluminum hydroxide is 1:1:1:3, and aluminum fluoride accounts for 20% of the total mass of the powder. Grinding for 3 hours by adopting a sand mill mixer, preparing spherical particles by adopting a spray drying process from the fully ground material, and obtaining a precursor A by adopting the particle size of 300 nanometers after grinding.
Step (2): and (3) filling the precursor A into a pot for full drying, filling the dried material into a furnace, and sintering at a high temperature of 1300 ℃ for 3 hours to obtain a semi-finished product B.
Step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
Example 4
Step (1): mixing high-purity active aluminum oxide, aluminum carbonate, aluminum tetraacetate, aluminum hydroxide, active silicon dioxide and aluminum fluoride according to a proportion by wet method, wherein the molar ratio of aluminum to silicon is 2.7:1, high-purity active aluminum oxide, aluminum carbonate and aluminum tetraacetate, wherein the mass ratio of aluminum hydroxide is 1:2:1:1, and aluminum fluoride accounts for 15% of the total mass of the powder. Grinding for 2.5 hours by adopting a sand mill mixer, preparing spherical particles by adopting a spray drying process from the fully ground material, and obtaining a precursor A, wherein the particle size of the spherical particles is 250 nanometers after grinding.
Step (2): and (3) filling the precursor A into a pot for full drying, filling the dried material into a furnace, and sintering at a high temperature of 1350 ℃ for 2.5 hours to obtain a semi-finished product B.
Step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
Fig. 1 to 4 are SEM images of mullite whiskers prepared in examples 1 to 4 of the present invention, and it can be seen that the mullite whiskers prepared by the method have a diameter of about 1 to 4 μm and a length of about 7 to 26 μm, and fig. 5 is an XRD image of mullite whiskers prepared in example 1 of the present invention, and it can be seen that the characteristic peaks of example 1 completely coincide with characteristic peaks of standard mullite whiskers, which proves that the mullite whiskers are successfully prepared by the method of the present invention.
Claims (10)
1. The preparation method of the mullite whisker is characterized by comprising the following steps of:
step (1): mixing a high-purity active aluminum-containing compound, active silicon dioxide and aluminum fluoride according to a proportion by a wet method, grinding by a sanding mixer, and preparing spherical particles from the fully ground materials by a spray drying process to obtain a precursor A;
step (2): fully drying the precursor A in a bowl, charging the dried material into a furnace, and sintering at high temperature to obtain a semi-finished product B;
step (3): and crushing, washing and grading the sintered material to obtain the mullite whisker.
2. The method according to claim 1, wherein in the step (1), the amount of the highly pure active aluminum-containing compound and the amount of the active silica are used in a molar ratio of aluminum to silicon of 2.5 to 3:1, aluminum fluoride accounts for 10-25% of the total mass of the powder.
3. The method of claim 1, wherein the high purity active aluminum-containing compound, the active silica and the aluminum fluoride in step (1) are all more than 99.9% pure.
4. The method according to claim 1, wherein the high-purity active aluminum-containing compound is at least one of active alumina, aluminum carbonate, organic aluminum alkoxide, aluminum oxalate, aluminum tetraacetate, and aluminum hydroxide, and the other aluminum-containing compound is mixed in an arbitrary ratio.
5. The method according to claim 1, wherein in the step (1), the mixture is sanded for 2 to 4 hours, and the particle size after grinding is 200 to 500 nm.
6. The method according to claim 1, wherein in the step (2), the sintering temperature is 1200 to 1400 ℃ and the sintering time is 2 to 4 hours.
7. The process according to claim 3, wherein the active alumina is gamma-alumina in the form of crystals, the active silica is amorphous silica and has a specific surface area of 10 to 100m 2 /g。
8. The method of claim 1, wherein in the step (1), the air inlet temperature of the spray drying process is 200-220 ℃, the air outlet temperature is 70-90 ℃, the spray speed is 10000-15000 rpm, and the peristaltic feeding is 300-600 ml/min.
9. Mullite whiskers as claimed in claim 1 as reinforcing and toughening material in Zn 2 TiO 4 /K 2 SiO 3 The coating material is applied to the coating material.
10. The use of mullite whiskers according to claim 1 as reinforcing and toughening material in a mullite sagger.
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