CN108017405A - A kind of preparation method of In-situ Mullite Whisker ceramic material - Google Patents

A kind of preparation method of In-situ Mullite Whisker ceramic material Download PDF

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CN108017405A
CN108017405A CN201711172952.1A CN201711172952A CN108017405A CN 108017405 A CN108017405 A CN 108017405A CN 201711172952 A CN201711172952 A CN 201711172952A CN 108017405 A CN108017405 A CN 108017405A
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ceramic material
preparation
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mullite
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鲁庭志
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MA'ANSHAN LIRUN METALLURGY MATERIAL CO Ltd
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MA'ANSHAN LIRUN METALLURGY MATERIAL CO Ltd
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    • 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
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • 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
    • C04B35/624—Sol-gel processing
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    • 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
    • C04B35/64—Burning or sintering processes
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5276—Whiskers, spindles, needles or pins
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    • 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
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661—Multi-step sintering

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Abstract

The invention discloses a kind of preparation method of In-situ Mullite Whisker ceramic material, the present invention is using gangue, alumine as raw material, polycrystalline mullite fibre is added as crystal seed, chlorine fluoride as whisker growth catalyst, the generation of mullite crystal whisker during acceleration of sintering；The crystal structure of potassium feldspar is destroyed after acidifying, reduces the liquid phase forming temperature of ceramic batch system, is promoted the melting of material in ceramic batch, is promoted the formation of mullite crystal and grow up, and is achieveed the purpose that to reduce ceramic firing temperature, is reduced energy consumption；After gel casting forming, two-part high temperature sintering, In-situ Mullite Whisker development is perfect, three-dimensional net structure has been internally formed in ceramic material, make ceramic material that there is higher porosity, the gas cell distribution state of final ceramics can be regulated and controled using Gelcasting Technique at the same time, improve the lightweight heat-proof performance of ceramic material.

Description

A kind of preparation method of In-situ Mullite Whisker ceramic material
Technical field
The present invention relates to refractory ceramic material technical field, and in particular to a kind of In-situ Mullite Whisker ceramic material Preparation method.
Background technology
Up to the present, the ceramic fibre refractory material of development and production, its technical process is substantially by ceramic fiber cotton It is directly incorporated into after broken in various indefinite form fire resisting bulk cargos, through moulding by casting.Broken ceramic fibre dispersion degree is bad, mostly all Exist in the form of cloud sheet shape or the cotton-shaped size of group are non-uniform.Although ceramic fibre pouring material light insulating, ceramic fibre Fibre porosity can be destroyed mostly after being mixed with fire resisting bulk material, and many places are filled by refractory wass, directly influence production The integral strength of product and optimal heat insulation.
For mullite fiber temperature in use at 1500-1600 DEG C, particularly high-temperature creep resistance and thermal shock resistance are excellent, resistance to Hot, corrosion-resistant and heat-insulating property is splendid.It may be used as heat-resistant component, high temperature thermal insulation material.Mullite fiber and ceramic matrix circle Face coefficient of thermal expansion and thermal conductivity are very close, and the addition of mullite fiber can improve the toughness of ceramic matrix, increase impact by force Degree, is often the first choice of heat-resisting composite research and development.
The content of the invention
The present invention provides a kind of preparation method of In-situ Mullite Whisker ceramic material.
The present invention is achieved by the following technical solutions：
A kind of preparation method of In-situ Mullite Whisker ceramic material, using gangue, alumine as raw material, it is living to introduce acid Change potassium feldspar, polycrystalline mullite fibre and chlorine fluoride, after being molded by Gelcasting Technique, high temperature sintering, in-situ preparation Mullite crystal whisker ceramic material.
Concrete technology step is as follows：
（1）The preparation of acid activation potassium feldspar：
After 8-16 parts of potassium feldspar powder are heated 4-8 minutes at 105 DEG C, according to 1:The solid-to-liquid ratio of 15-20, is added to 8-15% Acid solution in, be placed under 50-70 DEG C of water bath condition, stirring reaction 1-3 it is small when, after filtering, using ethanol clean 3-5 times, When drying 1-2 is small at 105-115 DEG C, acid activation potassium feldspar is obtained；
（2）The premixing of material powder：
28-46 parts of alumines, 18-34 parts of gangues are crossed into 80 mesh sieves after broken, ball milling, then carry out carbonization treatment, will Powder material and step after decarburization（1）Potassium feldspar is placed in ball mill after acid activation, adds appropriate distilled water wet ball grinding 8- 15 it is small when, through being dehydrated, dry, obtain premix powders；
（3）Premix the preparation of slurry：
By organic monomer acrylamide and crosslinking agent N,N methylene bis acrylamide according to 20:1 molar ratio be added to from Premixed liquid is obtained in sub- water, adds the dispersant ammonium citrate of powder quality 0.3%, and pH to 8.5- will be adjusted with ammonium hydroxide 9.5, the polyvinyl alcohol of stock quality 1-2% is added, obtains premix slurry；
（4）Casting：
By step（3）Premix powders, 5-12 part polycrystalline mullite fibre and 2-6 parts of aluminum fluorides are added in above-mentioned premix slurry, Ball milling 3-6 hours to powder lot dispersing it is uniform after, add catalyst TMEDA and the 0.8-1.5% persulfuric acid of premix slurry 0.5-1% Ammonium, stirs evenly rear injection molding, when curing 2-5 is small at room temperature, carries out gelation；
（5）Drying and sintering：
Material after the demoulding is dried in the shade 2-3 days, when then forced air drying 18-25 is small in 30-45 DEG C, then is placed under high temperature and carries out two Segmentation sinters, and with being taken out after stove natural cooling, that is, obtains In-situ Mullite Whisker ceramic material.
Wherein, the step（1）Middle acid solution refers to one kind or more in hydrochloric acid, sulfuric acid, oxalic acid, citric acid or malic acid Kind combination.
Wherein, the step（2）Middle wet ball grinding is to powder particle size in 0.045-0.075mm.
Wherein, the step（5）Middle two-part sintering concrete technology is as follows：It is small that 2-3 is kept the temperature at a temperature of 1270-1340 DEG C When, keep the temperature at a temperature of 1430-1560 DEG C 3-5 it is small when.
The present invention has the beneficial effect that：
Using gangue, alumine as raw material in the present invention, a small amount of polycrystalline mullite fibre is added as crystal seed, introduces chlorine fluoride As the catalyst of mullite crystal whisker growth, the generation of mullite crystal whisker during acceleration of sintering；Use inorganic acid or organic acid Activation process is carried out to potassium feldspar, destroys the crystal structure of potassium feldspar, the liquid phase for reaching reduction ceramic batch system forms temperature Degree, promotes the melting of material in ceramic batch, promotes the formation of mullite crystal and grow up, and reaching reduces ceramic firing temperature Purpose, reduces energy consumption；After gel casting forming, two-part high temperature sintering, In-situ Mullite Whisker development is perfect, Columnar crystal structure integrality is high, disorderly arranged in ceramic material inner homogeneous, forms three-dimensional net structure, makes ceramic material With higher porosity, while can be by controlling the solid content in pre- slurry using Gelcasting Technique, regulation and control are most The gas cell distribution state of ceramics eventually, improves the lightweight heat-proof performance of ceramic material, while have excellent heat-resistant knocking stability, height Warm mechanical property.
Embodiment
A kind of preparation method of In-situ Mullite Whisker ceramic material, using gangue, alumine as raw material, introduces Acid activation potassium feldspar, polycrystalline mullite fibre and chlorine fluoride, after being molded by Gelcasting Technique, high temperature sintering is in situ Generate mullite crystal whisker ceramic material.
Concrete technology step is as follows：
（1）The preparation of acid activation potassium feldspar：
After 12 parts of potassium feldspar powder are heated 6 minutes at 105 DEG C, according to 1:15 solid-to-liquid ratio, is added to 8% oxalic acid solution In, it is placed under 60 DEG C of water bath condition, when stirring reaction 1 is small, after filtering, is cleaned 4 times using ethanol, dry 2 is small at 110 DEG C When, obtain acid activation potassium feldspar；
（2）The premixing of material powder：
42 parts of alumines, 34 parts of gangues are crossed into 80 mesh sieves after broken, ball milling, carbonization treatment are then carried out, after decarburization Powder material and step（1）Potassium feldspar is placed in ball mill after acid activation, add appropriate distilled water wet ball grinding 12 it is small when, warp Dehydration, drying, obtain premix powders；
（3）Premix the preparation of slurry：
By organic monomer acrylamide and crosslinking agent N,N methylene bis acrylamide according to 20:1 molar ratio be added to from Premixed liquid is obtained in sub- water, adds the dispersant ammonium citrate of powder quality 0.3%, and pH to 9.2 will be adjusted with ammonium hydroxide, then The polyvinyl alcohol of stock quality 1.5% is added, obtains premix slurry；
（4）Casting：
By step（3）Premix powders, 12 parts of polycrystalline mullite fibres and 4 parts of aluminum fluorides are added in above-mentioned premix slurry, ball milling 4 Hour to powder lot dispersing it is uniform after, add premix slurry 0.8% catalyst TMEDA and 1.0% ammonium persulfate, noted after stirring evenly Mould, when curing 5 is small at room temperature, carries out gelation；
（5）Drying and sintering：
Material after the demoulding is dried in the shade 2 days, when then forced air drying 22 is small in 35 DEG C, then is placed in progress two-part burning under high temperature Knot, with being taken out after stove natural cooling, that is, obtains In-situ Mullite Whisker ceramic material.
Wherein, the step（2）Middle wet ball grinding is to powder particle size in 0.045-0.075mm.
Wherein, the step（5）Middle two-part sintering concrete technology is as follows：When insulation 3 is small at a temperature of 1335 DEG C, 1520 When insulation 4 is small at a temperature of DEG C.

Claims (5)

  1. A kind of 1. preparation method of In-situ Mullite Whisker ceramic material, it is characterised in that using gangue, alumine as Raw material, introduces acid activation potassium feldspar, polycrystalline mullite fibre and chlorine fluoride, after being molded by Gelcasting Technique, high temperature Sintering, In-situ Mullite Whisker ceramic material.
  2. A kind of 2. preparation method of In-situ Mullite Whisker ceramic material according to claim 1, it is characterised in that Concrete technology step is as follows：
    （1）The preparation of acid activation potassium feldspar：
    After 8-16 parts of potassium feldspar powder are heated 4-8 minutes at 105 DEG C, according to 1:The solid-to-liquid ratio of 15-20, is added to 8-15% Acid solution in, be placed under 50-70 DEG C of water bath condition, stirring reaction 1-3 it is small when, after filtering, using ethanol clean 3-5 times, When drying 1-2 is small at 105-115 DEG C, acid activation potassium feldspar is obtained；
    （2）The premixing of material powder：
    28-46 parts of alumines, 18-34 parts of gangues are crossed into 80 mesh sieves after broken, ball milling, then carry out carbonization treatment, will Powder material and step after decarburization（1）Potassium feldspar is placed in ball mill after acid activation, adds appropriate distilled water wet ball grinding 8- 15 it is small when, through being dehydrated, dry, obtain premix powders；
    （3）Premix the preparation of slurry：
    By organic monomer acrylamide and crosslinking agent N,N methylene bis acrylamide according to 20:1 molar ratio be added to from Premixed liquid is obtained in sub- water, adds the dispersant ammonium citrate of powder quality 0.3%, and pH to 8.5- will be adjusted with ammonium hydroxide 9.5, the polyvinyl alcohol of stock quality 1-2% is added, obtains premix slurry；
    （4）Casting：
    By step（3）Premix powders, 5-12 part polycrystalline mullite fibre and 2-6 parts of aluminum fluorides are added in above-mentioned premix slurry, Ball milling 3-6 hours to powder lot dispersing it is uniform after, add catalyst TMEDA and the 0.8-1.5% persulfuric acid of premix slurry 0.5-1% Ammonium, stirs evenly rear injection molding, when curing 2-5 is small at room temperature, carries out gelation；
    （5）Drying and sintering：
    Material after the demoulding is dried in the shade 2-3 days, when then forced air drying 18-25 is small in 30-45 DEG C, then is placed under high temperature and carries out two Segmentation sinters, and with being taken out after stove natural cooling, that is, obtains In-situ Mullite Whisker ceramic material.
  3. A kind of 3. preparation method of In-situ Mullite Whisker ceramic material according to claim 2, it is characterised in that The step（1）Middle acid solution refers to one or more combinations in hydrochloric acid, sulfuric acid, oxalic acid, citric acid or malic acid.
  4. A kind of 4. preparation method of In-situ Mullite Whisker ceramic material according to claim 2, it is characterised in that The step（2）Middle wet ball grinding is to powder particle size in 0.045-0.075mm.
  5. A kind of 5. preparation method of In-situ Mullite Whisker ceramic material according to claim 2, it is characterised in that The step（5）Middle two-part sintering concrete technology is as follows：When insulation 2-3 is small at a temperature of 1270-1340 DEG C, 1430-1560 When insulation 3-5 is small at a temperature of DEG C.
CN201711172952.1A 2017-11-22 2017-11-22 A kind of preparation method of In-situ Mullite Whisker ceramic material Pending CN108017405A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN111423221A (en) * 2020-03-16 2020-07-17 宝武装备智能科技有限公司 Castable for rotary hearth furnace working layer and preparation method thereof
CN113105224A (en) * 2021-04-14 2021-07-13 武汉理工大学 Mullite ceramic with high strength and low shrinkage performance and preparation method thereof
CN113248263A (en) * 2021-05-25 2021-08-13 西北工业大学 Si3N4wSi preform and preparation of Si using the same3N4w/Si3N4Method for compounding materials
CN115724689A (en) * 2022-11-21 2023-03-03 景德镇陶瓷大学 Low-temperature in-situ synthesis method of silicon carbide whisker coating surface modified cordierite honeycomb ceramic and product prepared by same
CN115724680A (en) * 2022-11-21 2023-03-03 景德镇陶瓷大学 Low-temperature in-situ preparation method of SiC nanowire coating surface modified alumina-based honeycomb ceramic and product prepared by same
CN115745650A (en) * 2022-11-21 2023-03-07 景德镇陶瓷大学 Low-temperature in-situ synthesis method of nitride whisker coating surface modified cordierite honeycomb ceramic and product prepared by same
CN115974523A (en) * 2022-12-09 2023-04-18 湖北飞龙摩擦密封材料股份有限公司 Porous mullite for friction material and preparation method and application thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111423221A (en) * 2020-03-16 2020-07-17 宝武装备智能科技有限公司 Castable for rotary hearth furnace working layer and preparation method thereof
CN111423221B (en) * 2020-03-16 2022-10-21 宝武装备智能科技有限公司 Castable for rotary hearth furnace working layer and preparation method thereof
CN113105224A (en) * 2021-04-14 2021-07-13 武汉理工大学 Mullite ceramic with high strength and low shrinkage performance and preparation method thereof
CN113248263A (en) * 2021-05-25 2021-08-13 西北工业大学 Si3N4wSi preform and preparation of Si using the same3N4w/Si3N4Method for compounding materials
CN115724689A (en) * 2022-11-21 2023-03-03 景德镇陶瓷大学 Low-temperature in-situ synthesis method of silicon carbide whisker coating surface modified cordierite honeycomb ceramic and product prepared by same
CN115724680A (en) * 2022-11-21 2023-03-03 景德镇陶瓷大学 Low-temperature in-situ preparation method of SiC nanowire coating surface modified alumina-based honeycomb ceramic and product prepared by same
CN115745650A (en) * 2022-11-21 2023-03-07 景德镇陶瓷大学 Low-temperature in-situ synthesis method of nitride whisker coating surface modified cordierite honeycomb ceramic and product prepared by same
CN115724680B (en) * 2022-11-21 2023-05-26 景德镇陶瓷大学 Low-temperature in-situ preparation method of SiC nanowire coating surface modified alumina-based honeycomb ceramic and product prepared by same
CN115724689B (en) * 2022-11-21 2023-05-26 景德镇陶瓷大学 Low-temperature in-situ synthesis method of silicon carbide whisker coated surface modified cordierite honeycomb ceramic and product prepared by same
CN115745650B (en) * 2022-11-21 2023-05-26 景德镇陶瓷大学 Low-temperature in-situ synthesis method of nitride whisker coated surface modified cordierite honeycomb ceramic and product prepared by same
CN115974523A (en) * 2022-12-09 2023-04-18 湖北飞龙摩擦密封材料股份有限公司 Porous mullite for friction material and preparation method and application thereof
CN115974523B (en) * 2022-12-09 2024-02-20 湖北飞龙摩擦密封材料股份有限公司 Porous mullite for friction material and preparation method and application thereof

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Application publication date: 20180511