CN109320274A - A kind of improved zirconium oxide fiber board and preparation method thereof - Google Patents

A kind of improved zirconium oxide fiber board and preparation method thereof Download PDF

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Publication number
CN109320274A
CN109320274A CN201811070452.1A CN201811070452A CN109320274A CN 109320274 A CN109320274 A CN 109320274A CN 201811070452 A CN201811070452 A CN 201811070452A CN 109320274 A CN109320274 A CN 109320274A
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zirconium oxide
temperature
fiber board
oxide fiber
slurry
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戴生伢
张引
钱松根
黄振进
陈福金
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Nanjing Polytechnic Yulong New Materials Polytron Technologies Inc
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Nanjing Polytechnic Yulong New Materials Polytron Technologies Inc
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232Titanium oxides or titanates, e.g. rutile or anatase
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427Silicates other than clay, e.g. water glass
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/522Oxidic
    • C04B2235/5236Zirconia
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    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5276Whiskers, spindles, needles or pins
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    • C04B2235/9615Linear firing shrinkage

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Abstract

The invention discloses a kind of improved zirconium oxide fiber boards, characterized in that the zirconium oxide fiber board that compression strength is high, high-temperature heat conductivity is low is made by addition inorganic binder and infrared light screening agent on the basis of existing fiberboard preparation process.Wherein, inorganic binder is mainly alkaline silica sol, and infrared light screening agent is mainly rutile type titanium white or crystal whisker of hexa potassium titanate.Its density of zirconium oxide fiber board obtained is 0.6~0.8g/cm3, compressive strength at room temperature is 3.0~5.0MPa, and when sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is 270~300 DEG C, and 1200 DEG C of hot-face temperature, coldface temperature is 310~330 DEG C.

Description

A kind of improved zirconium oxide fiber board and preparation method thereof
Technical field
The invention belongs to heat preserving and insulating material fields, and in particular to a kind of improved Zirconium oxide fibre slab products.
Background technique
Zirconium oxide (ZrO2) fiber is a kind of lightweight polycrystalline fibre material that temperature-resistance thermal-insulation is had excellent performance, long-term use temperature Up to 2200 DEG C, maximum operation (service) temperature is thermally conductive in all metal-oxide fiber refractory materials up to 2300 DEG C in short-term Coefficient is minimum, and heat-proof quality is best, and has stable high-temperature performance, is non-volatile, is pollution-free, therefore ZrO2Fiber and its products are (such as Fiberboard, fiber cloth, fibrofelt etc.) it is had broad application prospects in industries such as aerospace, metallurgy, petrochemical industries.ZrO2 Fiber is mainly used for the reinforcement etc. of superhigh temperature thermal insulation layer, ceramic matric composite in space shuttle;ZrO2Fiberboard is mainly made For high-temperature electric resistance furnace burner hearth materials'use, such as it is used for crystal growing furnace, super high sintering temperature furnace.
Porous class heat-barrier material, generally refers to be formed or be sintered by mesoporous aeroge or microporous oxide powder and forms Heat-barrier material such as SiO2Aeroge, Alumina Foam Ceramics etc..Nanoporous heat-barrier material is to be less than gas using the aperture of material The characteristics of body molecule mean free path, it is suppressed that the mutual collision between gas molecule, to reduce gas thermal conductivity.In addition, The unique superfine nano particle connection structure of aeroge reduces contact heat conductien to reducing solid-state thermal conductivity, red by adding Outer opacifier can further decrease radiant heat conductanc.Therefore, the major advantage of porous heat insulation material is that thermal conductivity is smaller, matter Amount is a kind of high temperature insulating material of comparative maturity compared with light, craftsmanship is preferable.
The porous heat insulation material of relatively early stage is mainly by micropore SiO2Powder is pressed after adding infrared light screening agent and reinforcing fiber It makes, typical product has the tandem product of Belgian Microtherm company, can be processed into various shape, such material Material can achieve 1000 DEG C using temperature, density 0.32g/cm3, due to infrared light screening agent (TiO2Powder) additional amount it is larger, institute It is very low with high-temperature heat conductivity.But such material is SiO due to its matrix2, it can not be used above at 1000 DEG C, while the material Compression strength is low.Currently, porous heat insulation material research is mainly aerogel heat-barrier material and froth inorganic stock.Aeroge Heat-barrier material can be divided into SiO according to compositional classification again2、Al2O3、SiO2-Al2O3、ZrO2With Si-C-O etc., wherein about SiO2Gas The most study of gel heat-insulation material, has been realized in industrialization at present.But SiO2The long-term use temperature highest of aeroge It is 650 DEG C, in short-term using up to 800 DEG C.It common are silicon carbide, silica, aluminium oxide in inorganic foamed ceramic material Foamed ceramics etc..The common advantage of these foamed ceramicses is use intensity and temperature all with higher.According to microcosmic reason of conducting heat By the heat transfer of porous material is broadly divided into solid phase heat transfer, radiant heat transfer, gas heat-transfer and convective heat transfer.Though this kind of foamed ceramics The right porosity is high, but stomata average diameter is 100~200 μm, is much larger than air mean free path 70nm, therefore high-temperature heat conductivity It is higher.At present the zirconium oxide fiber board density that has prepared all >=1.0g/cm3, use zirconium colloidal sol as binder more, intensity is low, And picking is serious.And influence of the high-temperature infrared to its thermal conductivity is not all considered.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provide one kind have high compressive strength and The low lightweight zirconium oxide fiber board and preparation method thereof of thermal conductivity.
Technical solution: in order to solve the above technical problems, a kind of zirconium oxide fiber board prepared by the present invention, raw material by
Preferably, selected inorganic binder is alkaline silica sol, SiO2Content >=30wt.%, pH value are 9~10.
Preferably, selected infrared light screening agent is zircon, rutile type titanium white, and average grain diameter is 1 μm and six metatitanic acids Potassium whisker, the length is 50~200 μm.
The present invention provides a kind of preparation method of zirconium oxide fiber board, preparation step is as follows:
(1) slurry is prepared: by obtained zirconium oxide chopped strand and inorganic binder, infrared light screening agent and water according to one After certainty ratio mixing, slurry is obtained after electric blender is thoroughly mixed.
(2) wet forming: the slurry prepared is poured into mold, after mechanical pressurization and vacuum filtration are formed and demoulded Obtain the wet base of fiberboard.
(3) dry high temperature sintering: being put into drying in air dry oven for wet base, places into sintering in high temperature Muffle furnace and obtains Zirconium oxide fiber board.
Further, the zirconium oxide chopped strand diameter is 5~10 μm, the Zirconium oxide fibre length in obtained slurry For 0.3~2mm.
Further, the infrared light screening agent is zircon, rutile type titanium white, and average grain diameter is 1 μm and six metatitanic acids Potassium whisker, the length is 50~200 μm.Benefit is stable crystal form, and particle size and infrared wavelength are in the same order of magnitude, is scattered Sufficiently.
Further, its density of zirconium oxide fiber board obtained is 0.6~0.8g/cm3, compressive strength at room temperature be 3.0~ 5.0MPa, when sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is 270~300 DEG C, hot-face temperature 1200 DEG C, coldface temperature is 310~330 DEG C.
Further, in the step (4) by the wet base of fiberboard be placed on 90~100 DEG C of dryings 10 in air dry oven~ 15h is placed into and is warming up to 1200 DEG C in high-temperature electric resistance furnace with 3 DEG C/min and keeps the temperature 2h.
Using thin diameter zirconium oxide fiber and high-temperature agglomerant as primary raw material in the present invention, prepared using existing fiberboard Method prepares lightweight zirconium oxide fiber board, and fiber crossovers arrangement makes the hole in fiberboard be divided into smaller space, further Pore-size is reduced, while further decreasing its high-temperature heat conductivity by adding infrared light screening agent.
The utility model has the advantages that zirconium oxide fiber board prepared by the present invention is in terms of existing technologies,
(1) use diameter for 5~10 μm of Zirconium oxide fibre, fiber crossovers, which are arranged, is divided into the hole in fiberboard more Small space further decreases pore-size, total body density≤0.8g/cm3
(2) alkaline silica sol is used, obtains high strength fiberboard through high temperature sintering, and applied at elevated temperature will not dusting.
(2) infrared light screening agent is added, its high-temperature heat conductivity, while part opacifier meeting and alkaline silica sol are further decreased Reaction generates a small amount of low melting glass phase under high temperature, further increases the compression strength of fiberboard.
Detailed description of the invention
Fig. 1 is prepared zirconium oxide fiber board pictorial diagram.
Specific embodiment
The present invention will be further explained with reference to the accompanying drawing.
Embodiment one:
Chopped Zirconium oxide fibre, the alkaline silica sol (SiO being ready for2>=30wt.%), zircon, rutile type titanium White powder (average grain diameter is 1 μm) and crystal whisker of hexa potassium titanate (length is 50~200 μm).
140g Zirconium oxide fibre, 250g alkaline silica sol, 28g titanium dioxide and 250g water are weighed in container, through electric mixing The machine of mixing obtains slurry after dispersion is sufficiently stirred.Slurry is poured into mold through vacuum filtration and in surface-pressure 0.2MPa, demoulding After obtain the wet base of fiberboard.Wet base is put into 100 DEG C of dry 10h in air dry oven, place into high temperature Muffle furnace with 3 DEG C/ Min is warming up to 1300 DEG C, and keeps the temperature 2h, obtains zirconium oxide fiber board, as shown in Figure 1.
After tested, its compressive strength at room temperature of alumina fibre plate obtained is 3.1MPa, and density is about 0.63g/cm3, weight Burn linear shrinkage ratio≤1%.When sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is about 270 DEG C, heat 1200 DEG C of face temperature, coldface temperature is about 310 DEG C, no picking phenomenon.
Embodiment two:
140g Zirconium oxide fibre, 250g alkaline silica sol, 28g zircon powder and 250g water are weighed in container, through electronic Blender obtains slurry after dispersion is sufficiently stirred.Slurry is poured into mold through vacuum filtration and in surface-pressure 0.2MPa, is taken off The wet base of fiberboard is obtained after mould.Wet base is put into 100 DEG C of dry 10h in air dry oven, is placed into high temperature Muffle furnace with 3 DEG C/min is warming up to 1200 DEG C, and keeps the temperature 2h, obtain zirconium oxide fiber board.
After tested, its compressive strength at room temperature of alumina fibre plate obtained is 5.0MPa, and density is about 0.8g/cm3, reheating Linear shrinkage ratio≤1%.When sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is about 300 DEG C, hot face 1200 DEG C of temperature, coldface temperature is about 330 DEG C, no picking phenomenon.
Embodiment three:
120g Zirconium oxide fibre, 250g alkaline silica sol, 12g potassium hexatitanate and 250g water are weighed in container, through electronic Blender obtains slurry after dispersion is sufficiently stirred.Slurry is poured into mold through vacuum filtration and in surface-pressure 0.25MPa, is taken off The wet base of fiberboard is obtained after mould.Wet base is put into 95 DEG C of dry 12h in air dry oven, place into high temperature Muffle furnace with 3 DEG C/ Min is warming up to 1200 DEG C, and keeps the temperature 2h, obtains zirconium oxide fiber board.
After tested, its compressive strength at room temperature of alumina fibre plate obtained is about 4.3MPa, and density is about 0.75g/cm3, Reheating linear shrinkage ratio≤1%.When sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is about 290 DEG C, 1200 DEG C of hot-face temperature, coldface temperature is about 320 DEG C, no picking phenomenon.
Example IV:
140g Zirconium oxide fibre, 250g alkaline silica sol, 14g titanium dioxide, 7g potassium hexatitanate and 250g water are weighed in container In, slurry is obtained after dispersion is sufficiently stirred in electric blender.Slurry is poured into mold through vacuum filtration and in surface-pressure 0.25MPa obtains the wet base of fiberboard after demoulding.Wet base is put into 90 DEG C of dry 15h in air dry oven, places into high temperature Muffle 1200 DEG C are warming up to 3 DEG C/min in furnace, and keeps the temperature 2h, obtains zirconium oxide fiber board.
After tested, its compressive strength at room temperature of alumina fibre plate obtained is 3.5MPa, and density is about 0.67g/cm3, weight Burn linear shrinkage ratio≤1%.When sample is having a size of 1cm thickness, when stable state, 1000 DEG C of hot-face temperature, coldface temperature is about 280 DEG C, heat 1200 DEG C of face temperature, coldface temperature is about 315 DEG C, no picking phenomenon.It tests simultaneously and is not added with opacifier and on the market Several zirconium oxide fiber boards, 1200 DEG C of hot-face temperature, coldface temperature has been more than 350 DEG C, and fiberboard has picking phenomenon.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art For member, under the premise of not departing from present principles, several improvements and modifications can also be made, these improvements and modifications also should be regarded as Protection scope of the present invention.

Claims (8)

1. a kind of improved zirconium oxide fiber board, it is characterised in that: its prepare component include the following: by weight
2. zirconium oxide fiber board according to claim 1, it is characterised in that: the inorganic binder includes that alkaline silicon is molten Glue, (SiO2>=30wt.%), pH value is 9~10.
3. zirconium oxide fiber board according to claim 1, it is characterised in that: the infrared light screening agent is zircon, golden red Stone-type titanium dioxide and crystal whisker of hexa potassium titanate.
4. a kind of preparation method of zirconium oxide fiber board according to claim 1, it is characterised in that preparation step is as follows:
(1) slurry is prepared: by obtained zirconium oxide chopped strand and inorganic binder, infrared light screening agent and water according to certain ratio After example mixing, slurry is obtained after electric blender is thoroughly mixed.
(2) wet forming: the slurry prepared is poured into mold, is obtained after mechanical pressurization and vacuum filtration form and demould The wet base of fiberboard.
(3) dry high temperature sintering: being put into drying in air dry oven for wet base, places into sintering in high temperature Muffle furnace and is aoxidized Zirconium fiberboard.
5. zirconium oxide fiber board according to claim 4, it is characterised in that: the zirconium oxide chopped strand diameter be 5~ 10 μm, the Zirconium oxide fibre length in obtained slurry is 0.3~2mm.
6. zirconium oxide fiber board according to claim 4, it is characterised in that: the infrared light screening agent is zircon, golden red Stone-type titanium dioxide, average grain diameter are 1 μm and crystal whisker of hexa potassium titanate, and the length is 50~200 μm.Benefit is stable crystal form, partial size Size and infrared wavelength are in the same order of magnitude, and scattering is abundant.
7. alumina fibre plate according to claim 4, it is characterised in that: its density of zirconium oxide fiber board obtained is 0.6~0.8g/cm3, compressive strength at room temperature is 3.0~5.0MPa, when sample is having a size of 1cm thickness, when stable state, and hot-face temperature 1000 DEG C, coldface temperature is 270~300 DEG C, and 1200 DEG C of hot-face temperature, coldface temperature is 310~330 DEG C.
8. zirconium oxide fiber board according to claim 4, it is characterised in that: put the wet base of fiberboard in the step (4) 90~100 DEG C of dry 10~15h, place into and are warming up to 1200 DEG C in high-temperature electric resistance furnace with 3 DEG C/min and protect in air dry oven Warm 2h.
CN201811070452.1A 2018-09-13 2018-09-13 A kind of improved zirconium oxide fiber board and preparation method thereof Pending CN109320274A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111410544A (en) * 2020-04-29 2020-07-14 成都天道化工技术有限公司 Method for manufacturing non-flexible refractory fiber product
CN114133267A (en) * 2020-09-04 2022-03-04 南京理工大学 Method for preparing zirconia hollow fiber brick by using rice hull powder as binder
CN115700234A (en) * 2022-10-27 2023-02-07 广州世陶新材料有限公司 Fiber-reinforced low-density porous heat-insulating material and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
JP2005253500A (en) * 2004-03-09 2005-09-22 Nissan Chem Ind Ltd Aldehydes-deodorant composition
CN103524140A (en) * 2013-09-23 2014-01-22 天津大学 Oxide ceramic fiber board
CN104446222A (en) * 2014-12-15 2015-03-25 山东鲁阳股份有限公司 Ceramic fiber plate and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JP2005253500A (en) * 2004-03-09 2005-09-22 Nissan Chem Ind Ltd Aldehydes-deodorant composition
CN103524140A (en) * 2013-09-23 2014-01-22 天津大学 Oxide ceramic fiber board
CN104446222A (en) * 2014-12-15 2015-03-25 山东鲁阳股份有限公司 Ceramic fiber plate and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111410544A (en) * 2020-04-29 2020-07-14 成都天道化工技术有限公司 Method for manufacturing non-flexible refractory fiber product
CN114133267A (en) * 2020-09-04 2022-03-04 南京理工大学 Method for preparing zirconia hollow fiber brick by using rice hull powder as binder
CN115700234A (en) * 2022-10-27 2023-02-07 广州世陶新材料有限公司 Fiber-reinforced low-density porous heat-insulating material and preparation method thereof
CN115700234B (en) * 2022-10-27 2023-11-10 广州世陶新材料有限公司 Fiber-reinforced low-density porous heat insulation material and preparation method thereof

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