CN103524140A - Oxide ceramic fiber board - Google Patents
Oxide ceramic fiber board Download PDFInfo
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- CN103524140A CN103524140A CN201310437109.7A CN201310437109A CN103524140A CN 103524140 A CN103524140 A CN 103524140A CN 201310437109 A CN201310437109 A CN 201310437109A CN 103524140 A CN103524140 A CN 103524140A
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- oxide ceramic
- ceramic fiber
- silicon sol
- fiber board
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Abstract
The invention discloses an oxide ceramic fiber board. The oxide ceramic fiber board comprises raw material components including silica sol, chopped fibers and a surfactant in a mass ratio of 1000:(100-200):(1-10), wherein the silica sol is prepared by mixing tetraethyl orthosilicate, ethanol and water in a mass ratio of (2-10):(1-9):(1-9), performing vacuum filtration to mold a wet blank, and after the gel is dried, and calcining the gel at 1200-1400 DEG C for 0.5-4 hours. According to the invention, the volume density (0.3g/cm<3>-0.7g/cm<3>) of the ceramic fiber board can be adjusted by changing the concentration (5-20wt%) of the silica sol, and the normal temperature heat conductivity of the oxide ceramic fiber board is 0.07-0.2W/m.K and is adjustable. The oxide ceramic fiber board disclosed by the invention is simple in process and environment-friendly, and can be prepared into any size and shape, and the long-term use temperature of the oxide ceramic fiber board can reach 1600 DEG C.
Description
Technical field
The present invention relates to a kind of rigidity high-temperature structural material, relate in particular to a kind of oxide ceramic fibre plate and preparation method thereof.
Background technology
Oxide ceramic fibre plate, as a kind of novel rigidity high-temperature structural material, is widely used in tunnel furnace, retort furnace as furnace lining; Ladle, coke-oven plant's pipeline are as thermofin etc.Ceramic beaverboard is one of deep processed product of ceramic fiber, than cloth, tapetum fibrosum, fibrefelt etc., has following advantage: high porosity, high physical strength, high temperature tolerance, lower thermal conductivity have certain toughness simultaneously.
Selecting a kind of suitable high-temperature fibre and high-temperature agglomerant is that the prerequisite of preparing ceramic beaverboard is also core main points.From chemical constitution and weave construction, oxide ceramic fibre can be divided into: Zirconium oxide fibre, sapphire whisker (80,95), mullite fiber (72), aluminum silicate fiber, silica fiber, high silica fiber.Hundreds of micron to tens centimetre), whisker (length: below hundreds of micron) from Fibre diameter and length-to-diameter ratio, oxide fibre can be divided into: macrofiber (length: tens centimetres to hundreds of rice), staple fibre (length:.
The difference of ceramic fiber the Nomenclature Composition and Structure of Complexes has directly determined high low temperature intensity, creep resistance, Young's modulus of fiber etc.; The length of fiber has determined the final form of fibre product: some fibre spinnable cloth, can blanket processed, can papermaking, some fiber is just not all right, final decision different fibre products proprietary Application Areass separately.
High-temperature agglomerant is divided into (1) reaction bonded type binding agent from bonding mechanism: norbide, silicon carbide, during high temperature, sintering aid autoxidation is high-viscosity melt or the nanometer high activity oxide anchoring fiber node that bonds.(2) high-temperature stream ejector half binding agent: highly reactive form of oxygen SiClx, boron oxide, aluminum oxide.From states of matter, be divided into (1) solid-state adhesion agent and (2) colloidal binder: silicon sol, aluminium colloidal sol, zirconium colloidal sol, water glass etc., application solgel reaction anchoring fiber node, obtains high strength base substrate, and high temperature sintering makes goods.
The characteristics such as the ultimate compression strength of How to choose high-temperature agglomerant meeting remarkably influenced fibrous matrix, compression resilience, void content, thermal conductivity.While adopting solid-state adhesion agent, add-on is difficult for being evenly distributed at least in fibrous matrix, stress concentration and affect the mechanical property of fibre product; Fibre product volume density is large at most for add-on, and then thermal conductivity increase (fibre product normal temperature thermal conductivity and volume density are linear), and void content reduces.In a lot of situations, colloidal state and solid-state high-temperature agglomerant can be used in conjunction with.
The basal component of silicon sol is hydration SiO
2(amorphous Si O
2), SiO
2with micelle form, be dispersed in water or in ethanol, outward appearance is creamy white or clear, has hydrophilic increasing oiliness, and available distilled water diluting is to any concentration, and dilution rear stability strengthens.There is polymolecularity, preferably wear resistance, good light transmission.The character more complicated of silicon sol, SiO
2dispersity, temperature, amount of cure and the system of concentration, size of particles, specific surface area, system in the factors such as character of minor component all can affect the performance of silicon sol.
Alkaline silica sol is by take water glass as raw material, making by ion exchange method, obtains the poly-silicate solution of less stable after cation and anion exchange, and solution is slightly acidic, with NaOH or other reagent, makees stablizer, by the stable range of pH modulation 8.5～9.5.SiO
2content 15%～40%, Na2O content 0.1%～0.5%, owing to containing a certain amount of Na in alkaline silica sol
2o, refractoriness is lower than acidic silicasol.
Filler: 1, filler can be hollow glass ball, hollow ball is in fibrous matrix network gap, and the one, increase matrix strength, the 2nd, reduce heat conduction.2, filler can be also silicon gel: first prepare fibre network matrix, after vacuum impregnation silicon sol, through supercritical drying, make silicon gel-filled in fibre network gap, this structure can largely reduce the thermal conductivity of goods.
Sintering: mainly consider two factors: sintering temperature must be lower than the intensity of fiber impaired temperature, higher than high-temperature agglomerant, produce the temperature of cohesive strength simultaneously, from this point, say, a kind of ceramic fiber of rational Match and high-temperature agglomerant are the core places that success is prepared ceramic beaverboard!
Generally speaking, the forming method of ceramic beaverboard is all colloidal formation: as gel injection, can realize complicated shape moulding, still, monomer is poisonous, and slurry and gelation process are controlled more complicated; Vacuum filtration moulding is relatively simple, has more general applicability, is more suitable for heavy industrialization application.
Summary of the invention
The present invention is directed to the deficiency of existing oxide ceramic fibre plate technology of preparing, provide the method for a kind of employing " acidic silicasol high-temperature agglomerant adds vacuum filtration moulding " to prepare oxide ceramic fibre plate; The long-time use temperature of ceramic beaverboard prepared by the method reaches 1600 ℃ (using Zirconium oxide fibre as matrix), and the volume density of ceramic beaverboard can regulate arbitrarily within the specific limits according to the concentration of silicon sol.
The present invention realizes above-mentioned purpose by following technical solution, and concrete steps are as follows:
A plate, its raw material consists of silicon sol, chopped strand and tensio-active agent, and its mass ratio is 1000:100～200:1～10;
This oxide ceramic fibre plate preparation method, has the following step:
(1) prepare silicon sol
Tetraethoxy, second alcohol and water are mixed according to the mass ratio of 2～10:1～9:1～9, with inorganic or organic acid, pH is transferred to 1～3, magnetic agitation 2 hours, the silicon sol that acquisition concentration is 5wt%～20wt% is high-temperature agglomerant;
(2) prepare fibre stuff and vacuum filtration moulding
Select one or more mixtures in aluminum silicate fiber, mullite fiber, sapphire whisker, Zirconium oxide fibre, silica fiber, high silica fiber, with hollander, smash, obtain length-to-diameter ratio and be 50～500 chopped strand; The tensio-active agent of chopped strand and step (1) is joined in silicon sol and prepares fibre stuff, and its composition and ratio is: silicon sol: chopped strand: the mass ratio of tensio-active agent is 1000:100～200:1～10; Fibre stuff quick oscillation is stirred 30 minutes again, then fibre stuff is injected to mould, vacuum filtration moulding, obtains wet base after gel;
(3) dry and calcining
The wet base of step (2), after dry 48 hours, in 1200 ℃～1400 ℃ calcinings 0.5～4 hour, is made to oxide ceramic fibre plate.
Inorganic or the organic acid of described step (1) is a kind of in sulfuric acid, hydrochloric acid, nitric acid or acetic acid.
The tensio-active agent of described step (2) is a kind of in sodium alkyl benzene sulfonate, sodium alkyl sulfate, sodium soap or alkyl sodium sulfonate, and its concentration is 0.2～0.5wt%.
The shape of cross section of the forming mould of described step (2) is arbitrary shape, and mold bottom has some through holes for draining.
The high-temperature calcination of described step (3) can, for Resistant heating, globars heating or Si-Mo rod heating, be preferably microwave heating.
Tool of the present invention has the following advantages and positively effect:
(1) use temperature of oxide ceramic fibre plate of the present invention can be according to different change (1000 ℃～1600 ℃) of ceramic fiber; By changing the concentration of high-temperature agglomerant, can regulate the volume density (0.3g/cm of ceramic beaverboard
3～0.7g/cm
3); Meanwhile, the normal temperature thermal conductivity of oxide ceramic fibre plate is that 0.07W/mK～0.2W/mK is adjustable.
(2) the present invention adopts microwave heating can significantly shorten ceramic beaverboard required time in calcination process, energy-saving and emission-reduction.
(3) the present invention adopts acidic silicasol as high-temperature agglomerant, and the component of acidic silicasol is 100% pure SiO
2, do not use any organic binder bond, improved the use temperature of fiberboard.
Accompanying drawing explanation
Scanning electronic microscope (SEM) picture of Fig. 1 embodiment of the present invention 1 mullite fiber plate.
Embodiment
Below in conjunction with embodiment, be that the present invention is further explained and is illustrated, but the present invention is not constituted any limitation.The raw material using in following examples is commercially available analytical pure raw material.
Embodiment 1
By tetraethoxy, second alcohol and water in mass ratio 10:9:9 mix, with nitric acid, adjust pH to 1, magnetic agitation 2 hours, obtains silicon sol high-temperature agglomerant.It is 300 chopped strand that mullite loose wool chopping is obtained to length-to-diameter ratio, 100g fiber is joined in 1000mL silicon sol, then adding successively 10mL concentration is the Sodium dodecylbenzene sulfonate solution of 0.2wt%, stir after 30 minutes, again fibre stuff is injected to mould, vacuum filtration moulding, obtains wet base after gel.To wet base at air drying 24 as a child, 1300 ℃ of calcinings, within 2 hours, made oxide ceramic fibre slab products.Product volume density is 0.3g/cm
3～0.4g/cm
3, normal temperature thermal conductivity is 0.07W/mK～0.1W/mK, its long-time use temperature is 1400 ℃.As shown in Figure 1, mullite fiber overlaps mutually the microscopic appearance of goods, intert and form network matrix, and high-temperature agglomerant adheres to fiber node, the hole that exists a lot of three-dimensionals to run through in the surrounding of fiber.
Embodiment 2
By tetraethoxy, second alcohol and water in mass ratio 2:1:1 mix, with hydrochloric acid, adjust pH to 2, magnetic agitation 2 hours, obtains silicon sol high-temperature agglomerant.It is 200 chopped strand that aluminum oxide loose wool chopping is obtained to length-to-diameter ratio, 150g fiber is joined in 1000mL silicon sol, then adding successively 10mL concentration is the Sodium dodecylbenzene sulfonate solution of 0.3wt%, stir after 30 minutes, again fibre stuff is injected to mould, vacuum filtration moulding, obtains wet base after gel.To wet base at air drying 24 as a child, 1350 ℃ of calcinings, within 3 hours, made oxide ceramic fibre slab products.Product volume density is 0.4g/cm
3～0.5g/cm
3, normal temperature thermal conductivity is 0.1W/mK～0.14W/mK, its long-time use temperature is 1500 ℃.
Embodiment 3
By tetraethoxy, second alcohol and water in mass ratio 4:1:1 mix, with sulfuric acid, adjust pH to 1, magnetic agitation 2 hours, obtains silicon sol high-temperature agglomerant.It is 100 chopped strand that zirconium white loose wool chopping is obtained to length-to-diameter ratio, 100g fiber is joined in 1000mL silicon sol, then adding successively 10mL concentration is the Sodium dodecylbenzene sulfonate solution of 0.4wt%, stir after 30 minutes, again fibre stuff is injected to mould, vacuum filtration moulding, obtains wet base after gel.To wet base at air drying 24 as a child, with microwave Muffle furnace, 1400 ℃ of calcinings, within 1 hour, made oxide ceramic fibre slab products.Product volume density is 0.6g/cm
3～0.7g/cm
3, normal temperature thermal conductivity is 0.17W/mK～0.2W/mK, its long-time use temperature is 1600 ℃.
The various raw materials that the present invention is cited and the span of various processing parameters can realize the present invention, then this is illustrated no longer one by one.
Claims (5)
1. an oxide ceramic fibre plate, its raw material consists of silicon sol, chopped strand and tensio-active agent, and its mass ratio is 1000:100～200:1～10;
This oxide ceramic fibre plate preparation method, has the following step:
(1) prepare silicon sol
Tetraethoxy, second alcohol and water are mixed according to the mass ratio of 2～10:1～9:1～9, with inorganic or organic acid, pH is transferred to 1～3, magnetic agitation 2 hours, the silicon sol that acquisition concentration is 5wt%～20wt% is high-temperature agglomerant;
(2) prepare fibre stuff and vacuum filtration moulding
Select one or more mixtures in aluminum silicate fiber, mullite fiber, sapphire whisker, Zirconium oxide fibre, silica fiber, high silica fiber, with hollander, smash, obtain length-to-diameter ratio and be 50～500 chopped strand; The tensio-active agent of chopped strand and step (1) is joined in silicon sol and prepares fibre stuff, and its composition and ratio is: silicon sol: chopped strand: the mass ratio of tensio-active agent is 1000:100～200:1～10; Fibre stuff quick oscillation is stirred 30 minutes again, then fibre stuff is injected to mould, vacuum filtration moulding, obtains wet base after gel;
(3) dry and calcining
The wet base of step (2), after dry 48 hours, in 1200 ℃～1400 ℃ calcinings 0.5～4 hour, is made to oxide ceramic fibre plate.
2. according to the oxide ceramic fibre plate of claim 1, it is characterized in that, the inorganic or organic acid of described step (1) is a kind of in sulfuric acid, hydrochloric acid, nitric acid or acetic acid.
3. according to the oxide ceramic fibre plate of claim 1, it is characterized in that, the tensio-active agent of described step (2) is a kind of in sodium alkyl benzene sulfonate, sodium alkyl sulfate, sodium soap or alkyl sodium sulfonate, and its concentration is 0.2～0.5wt%.
4. according to the oxide ceramic fibre plate of claim 1, it is characterized in that, the shape of cross section of the forming mould of described step (2) is arbitrary shape, and mold bottom has some through holes for draining.
5. according to the oxide ceramic fibre plate of claim 1, it is characterized in that, the high-temperature calcination of described step (3) can, for Resistant heating, globars heating or Si-Mo rod heating, be preferably microwave heating.
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|---|---|---|---|
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| CN103524140B CN103524140B (en) | 2015-05-13 |
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| CN105272322A (en) * | 2015-09-30 | 2016-01-27 | 航天特种材料及工艺技术研究所 | Light-weight, high temperature-resistance and heat-insulation ceramic fiber tile and making method thereof |
| CN105545013A (en) * | 2016-01-26 | 2016-05-04 | 柳州市力万科技有限公司 | Thermal-insulating removable house |
| CN105712716A (en) * | 2016-02-16 | 2016-06-29 | 中材科技股份有限公司 | Zirconium oxide fiber ceramic plate and preparing method thereof |
| CN106145970A (en) * | 2016-07-06 | 2016-11-23 | 南京理工宇龙新材料科技股份有限公司 | A kind of fibre board and preparation method thereof |
| CN106187252A (en) * | 2016-07-06 | 2016-12-07 | 南京理工宇龙新材料科技股份有限公司 | A kind of anti-corrosive properties fibre board and preparation method thereof |
| CN106587901A (en) * | 2016-11-30 | 2017-04-26 | 山东工业陶瓷研究设计院有限公司 | Preparation method of high-temperature-resistant, high-strength and rigid thermal insulation material |
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| CN108033756A (en) * | 2017-12-12 | 2018-05-15 | 山东鲁阳节能材料股份有限公司 | A kind of high density ceramic fiberboard and preparation method thereof |
| CN108517714A (en) * | 2018-04-04 | 2018-09-11 | 黄智慧 | A kind of preparation method of high tenacity inorganic refractory paper material |
| CN109320273A (en) * | 2018-09-13 | 2019-02-12 | 南京鑫达晶体材料科技有限公司 | A kind of improved alumina fibre plate and preparation method thereof |
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| CN112142485A (en) * | 2020-08-25 | 2020-12-29 | 阿尔赛(苏州)无机材料有限公司 | Ceramic fiber material and preparation method thereof |
| CN114057475B (en) * | 2020-11-23 | 2022-11-11 | 航天特种材料及工艺技术研究所 | Silicon dioxide ceramic matrix composite material and preparation method thereof |
| CN114057475A (en) * | 2020-11-23 | 2022-02-18 | 航天特种材料及工艺技术研究所 | Silicon dioxide ceramic matrix composite material and preparation method thereof |
| CN116406436A (en) * | 2020-11-27 | 2023-07-07 | 霓佳斯株式会社 | Molded body |
| CN112645677B (en) * | 2020-12-24 | 2022-11-01 | 山东鲁阳节能材料股份有限公司 | High-low temperature composite high-density ceramic fiber board and preparation method thereof |
| CN112645677A (en) * | 2020-12-24 | 2021-04-13 | 山东鲁阳节能材料股份有限公司 | High-low temperature composite high-density ceramic fiber board and preparation method thereof |
| CN113387718A (en) * | 2021-07-13 | 2021-09-14 | 衢州市智能制造技术与装备研究院 | Method for preparing reticular ceramic film |
| CN117902896A (en) * | 2024-03-19 | 2024-04-19 | 上海南极星高科技股份有限公司 | Preparation method of lightweight heat-insulating zirconia fiber-based porous ceramic |
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