CN101462876B - Preparation of zirconia ceramic beaverboard - Google Patents
Preparation of zirconia ceramic beaverboard Download PDFInfo
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- CN101462876B CN101462876B CN2009100137821A CN200910013782A CN101462876B CN 101462876 B CN101462876 B CN 101462876B CN 2009100137821 A CN2009100137821 A CN 2009100137821A CN 200910013782 A CN200910013782 A CN 200910013782A CN 101462876 B CN101462876 B CN 101462876B
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- zirconium
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- yttrium
- ethanol
- fiber
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000919 ceramic Substances 0.000 title claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 42
- 239000011094 fiberboard Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 24
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 24
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 13
- 239000012298 atmosphere Substances 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- 229910052726 zirconium Inorganic materials 0.000 claims description 13
- 229920000620 organic polymer Polymers 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 150000003746 yttrium Chemical class 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000009987 spinning Methods 0.000 claims description 5
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- ZTEQFJRPFFHAOW-UHFFFAOYSA-N pentane-2,3-dione yttrium Chemical compound [Y].C(C)C(=O)C(=O)C ZTEQFJRPFFHAOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000000567 combustion gas Substances 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- NREVZTYRXVBFAQ-UHFFFAOYSA-N propan-2-ol;yttrium Chemical compound [Y].CC(C)O.CC(C)O.CC(C)O NREVZTYRXVBFAQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000007669 thermal treatment Methods 0.000 claims description 3
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims description 3
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 3
- JQLZABHNCZQFNR-UHFFFAOYSA-J O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] Chemical compound O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] JQLZABHNCZQFNR-UHFFFAOYSA-J 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 239000003034 coal gas Substances 0.000 claims description 2
- 235000009508 confectionery Nutrition 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 229910002078 fully stabilized zirconia Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 239000003345 natural gas Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 230000035924 thermogenesis Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 239000011819 refractory material Substances 0.000 abstract 1
- 238000003828 vacuum filtration Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011449 brick Substances 0.000 description 2
- 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 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
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Images
Abstract
The invention belongs to the inorganic refractory material field, and relates to a preparation method of a refractory and heat-insulating fiber board based on zirconia fiber. The preparation method mainly comprises the following steps: stable cubic phase zirconia fiber is taken as a base phase, fine zirconia powder is taken as a filler, an organic binding agent is added to prepare slurry, and the slurry is formed by vacuum filtration, dried and sintered at a high temperature to prepare the ceramic zirconia fiber board. The preparation process is simple; the prepared fiber board has the advantages of even and single component and high-temperature resistance, and the fiber board can be used in an environment of 1700 DEG C-2160 DEG C for a long time.
Description
Technical field
The present invention relates to a kind of is the preparation method of the refractory heat-insulating fiberboard on basis with the Zirconium oxide fibre, belongs to the inorganic fire proof material field.
Background technology
Along with China's industrial expansion, the energy expenditure total amount is increasingly high.Selecting the heat-insulating material with the utilisation technology excellent property, can reduce the kiln radiation heat loss, improve furnace heat efficiency, is the effective technical means of realization industrial thermal equipment good quality and high output, low consumption and energy-saving and emission-reduction.At present the good material of heat-insulating properties such as mullite fiber and sapphire whisker is applied in industries such as the metallurgy of China, electric power, building materials, petrochemical compleies on a large scale, and has obtained good effect.But the maximum operation (service) temperature of mullite crystal fiber and alpha-alumina crystals fiber has only 1400 ℃ and 1600 ℃.In the hot environment more than 1700 ℃, generally use zirconium white hollow ball brick as heat-resistant insulation material at present, but compare with the crystal of zirconium oxide fiber, hollow ball brick thermal conductivity is big, and thermal capacitance is high, and heat insulation effect is poor.And zirconium white (ZrO
2) fiber is a kind of docrystalline oxide compound refractory fibrous material of life-time service under the ultrahigh-temperature oxidizing atmosphere that can satisfy more than 1600 ℃; Have than existing refractory fibre kind is higher on the home market use temperature and better heat-proof quality, and pyrochemistry stable in properties, corrosion-resistant, anti-oxidant, anti-thermal shock, non-volatile, pollution-free.ZrO2 has monocline, four directions and cube three kinds of crystalline phases.Through to ZrO
2Middle admixture stablizer Y
2O
3, can be with four directions or cube phase ZrO
2Settle out, avoided ZrO
2Fiber undergoes phase transition in heating and cooling process.Yet, because the difficulty of the technology of preparing of Zirconium oxide fibre own makes the preparation method of zirconium oxide fiber board have very big blank.
Summary of the invention
The present invention provides a kind of preparation method of zirconia ceramic beaverboard in order to remedy the deficiency of prior art, and the wad composition of preparation is evenly single, high temperature resistant, can under 1700 ℃～2160 ℃ environment, use for a long time.
The present invention realizes through following technical scheme:
The preparation method of zirconia ceramic beaverboard of the present invention may further comprise the steps:
(1) chopping: the Zirconium oxide fibre weak point is cut to 1mm-3mm.
(2) slurrying: short fiber and the fully stabilized zirconia fine powder that cuts placed kiln basin in mass ratio 1: 0～0.5 ratio; Adding massfraction then is the combination agent solution of 0.1-1%; Be mixed with Zirconium oxide fibre slurry and stirring, churning time was not less than 3 minutes; Alr mode can use mechanical type to stir, and also can stir by using gas.The homogeneity of slurry is an important factor that influences the wad quality.The unit weight of wad can be controlled through the adding proportion of powdered zirconium oxide, and along with the increase of powdered zirconium oxide adding proportion, the unit weight of wad increases, and intensity increases, but heat insulation effect reduces.The wad of zirconia free fine powder, unit weight is minimum, and heat insulation effect is best.
Described powdered zirconium oxide be x greater than the stable zirconium white of the yttrium salt of 8%-15%, normal temperature is down cube crystalline phase.Described yttrium salt is one or more in Yttrium trinitrate, methyl ethyl diketone yttrium, yttrium isopropoxide and the Yttrium trichloride.
Described organic bond is Z 150PH, SEPIGEL 305 or both mixtures.
For preventing that other crystalline phase fibers from high temperature producing phase transformation, and, cause the wad efflorescence with volume effect, no intensity, described Zirconium oxide fibre is a complete stable cubic phase fiber.
Described Zirconium oxide fibre adopts the following steps preparation:
(1) according to zirconium oxychloride: the ratio of ethanol=100g: 800～1000ml is dissolved in zirconium oxychloride in the ethanol; According to mol ratio is zirconium oxychloride: methyl ethyl diketone: the ratio of triethylamine=1: 1.8～2.0: 2.5 is measured methyl ethyl diketone and triethylamine; Be dissolved in jointly in another part ethanol with the ethanol equivalent of dissolved oxygen zirconium chloride; 0 ℃～50 ℃ with agitation condition under; The alcohol dilution liquid atomizing of methyl ethyl diketone and triethylamine is joined in the zirconium oxychloride alcohol dilution liquid, add the continued stirring and obtain the golden transparent reaction solution;
(2) evaporate to dryness ethanol is the dissolution with solvents solvend with acetone, removes by filter the insolubles Triethylammonium chloride, reclaims acetone, must contain the zirconium organic polymer;
(3) according to the ratio of reactant zirconium oxychloride: ethanol=100g: 10～50ml; Product is contained the zirconium organic polymer dissolve in the ethanol, and be zirconium white: yttrium oxide=80%～91% according to mol ratio: 20%～9% ratio, mix yttrium salt; Sealing and standing obtains spinning solution;
(4) adopt centrifugal pan to get rid of a method and obtain to contain the zirconium organic polymer fiber, under special atmosphere, heat-treat, obtain cubic phase zircite crystal fibre; Said special atmosphere is organic steam, nitrogen, water vapor or their mixed-gas atmosphere, and organic steam is to contain the steam that the zirconium organic polymer soln adds thermogenesis.
For improving the high-temperature resistance of fiber, described cubic phase zircite crystal fibre can carry out uht treatment.
Described uht treatment step is: be used for the fiber winding-up after to thermal treatment of gas flame that diameter 8-12 centimetre burner produces; 1800 ℃-2200 ℃ of flame temperatures; The winding-up time is 5min-1h, and gas flame is one or more in hydrogen, acetylene, propane, Sweet natural gas, coal gas and the coal mine gas flame.Described High Temperature Furnaces Heating Apparatus is a kind of in air atmosphere electric furnace, nitrogen nitrogen atmosphere electric furnace, vacuum test electric furnace and the industrial combustion gas stove.
(3) filtering molding: mould is placed kiln basin, open vacuum pump,, obtain the wet base of wad of moulding through vacuum suction filter.
(4) drying: the wet base of wad is carried out drying in 50-120 ℃ of scope, the time is 20-30 hour; To regularly stir when dry, prevent the partial drying excessive velocities, cause the phenomenon of wad distortion wad.
(5) high temperature sintering: the wad that drying is good, be positioned over sintering in the High Temperature Furnaces Heating Apparatus, sintering temperature is 1600 ℃-1750 ℃, time 5-8 hour, obtains zirconium oxide fiber board.During high temperature sintering, wad will keep flat to load bearing board, prevents in sintering process, and wad deforms because of the gravity of self.
The present invention compared with prior art has following beneficial effect:
(1) wad of the present invention preparation is the complete stable cubic phase zircite wad, can in 1700 ℃ of-2160 ℃ of scopes, use for a long time, has filled up the blank that this TR does not have heat-insulating fiberboard.
(2) adopt the filtering molding method, prepared fibreboard fibres is evenly distributed in order, and high temperature is parallel to the contraction of exposure directional ray when using little, helps improving body of heater long term high temperature work-ing life.
(3) the prepared wad of the present invention, the single inclusion-free of composition is a kind of purified high-temperature flame-proof lagging material, not only can be in the medium-term and long-term use of 1700 ℃～2160 ℃ pyritous environment, the atmosphere requirement of harshness in the time of can also satisfying crystal growth.
(4) preparation technology is simple, need not to prepare in advance inorganic zirconium glue bond agent.
Description of drawings
Fig. 1 is the digital photograph of zirconia ceramic beaverboard of the present invention.
Embodiment
Embodiment 1
The preparation method of zirconia ceramic beaverboard of the present invention is for adopting following steps:
(1) preparation complete stable cubic phase zircite fiber:
A takes by weighing zirconium oxychloride (ZrOCl
28H
2O) 100g is dissolved in the 800ml ethanol, is zirconium oxychloride according to mol ratio: methyl ethyl diketone: the ratio of triethylamine=1: 1.8: 2.5; Measure 60ml methyl ethyl diketone and 110ml triethylamine, be dissolved in jointly in 800 milliliters of ethanol, 5 ℃ with agitation condition under; The alcohol dilution liquid atomizing of methyl ethyl diketone and triethylamine is joined in the zirconium oxychloride alcohol dilution liquid, add continued and stirred 3 hours, obtain the golden transparent reaction solution; 40 ℃ of rotary evaporations are removed etoh solvent, do until near, obtain flaxen dung; Ratio according to zirconium oxychloride: acetone=100g: 500ml adds 500ml acetone, stirs to make the solvend dissolving, and insoluble Triethylammonium chloride white precipitate is removed in press filtration; Acquisition golden transparent filtrating; 50 ℃ of rotary evaporations are removed solvent acetone, until obtaining dry and hard faint yellow solid substance 70g, are product and contain the zirconium organic polymer;
B contains zirconium organic polymer 70g with products therefrom and dissolves in the 20ml ethanol, and be equivalent to zirconium white according to mol ratio according to the ratio of reactant zirconium oxychloride: ethanol=100g: 20ml: the ratio of yttrium oxide=90%: 10%, mix 22.3g Yttrium trinitrate (Y (NO
3)
36H
2O), sealing and standing obtains the spinning solution of golden yellow homogeneous transparent;
C adopts centrifugal pan to get rid of a method spinning, is 10 ℃ in temperature, and relative humidity is 20%, and centrifuge speed is 15000r/min, and getting rid of a plate edge LV is under the condition of 30m/s, and spinning solution is thrown away at a high speed, and what obtain unordered accumulation contains the zirconium organic polymer fiber;
D will contain the zirconium organic polymer fiber and place in the program control stove of atmosphere, under organic steam atmosphere, with the heat-up rate of 1 ℃/min, in the TR of room temperature～1200 ℃, heat-treat, and obtain complete stable cubic phase zircite crystal fibre;
It is the fiber winding-up of the acetylene gas flame that produces of 12 centimetres burner after to thermal treatment that E uses diameter; 1800 ℃ of flame temperatures, winding-up time 5min can obtain purified, crystal grain and grow sufficient complete stable cubic phase zircite crystal fibre; Diameter 8-15 micron, length 1-50 centimetre.
(2) with complete stable cubic phase zircite fiber 100 gram, use the filament cutter weak point to cut to 3-5mm, place kiln basin, add massfraction again and be 0.1% polyvinyl alcohol solution; In kiln basin, stirred 3 minutes, mould is placed kiln basin, open vacuum pump, use vacuum filtering shape process, with the wet base of wad under 100 ℃ temperature dry 24 hours; Place the air atmosphere electric furnace then, 1650 ℃ of sintering 5 hours.Gained zirconium oxide fiber board performance is following: unit weight 250kg/m
3, making temperature for a long time is 2100 ℃, and thermal conductivity is 0.18W/mK, and shrinking percentage is being to be 2% under 0.9%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 2
Said with embodiment 1, difference is to use the filament cutter weak point to cut to 1mm complete stable cubic phase zircite fiber 100 grams; Place kiln basin then; Add 20 gram normal temperature and be that down it is that 9% Yttrium trinitrate is stablized the made ZrO that contains that the powdered zirconium oxide of cube crystalline phase, zirconium white mix x
2Fibreboard performance is following: unit weight 300kg/m
3, thermal conductivity is 0.25W/mK, shrinking percentage is being to be 1.5% under 0.7%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 3
Said with embodiment 1; Difference is complete stable cubic phase zircite fiber 100 grams; Use the filament cutter weak point to cut to 2mm, place kiln basin then, adding 50 grams, to mix x be that 10% the stable normal temperature of methyl ethyl diketone yttrium is the powdered zirconium oxide of cube crystalline phase down.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.4% under 0.65%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 4
Said with embodiment 1, difference is 1750 ℃ of sintering 5 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 250kg/m
3, making temperature for a long time is 2100 ℃, and thermal conductivity is 0.18W/mK, and shrinking percentage is being to be 1.8% under 0.5%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 5
Said with embodiment 2, difference is to add massfraction and is respectively in 1% and 0.1% the Z 150PH and polyacrylamide solution, and in the vacuum test electric furnace 1700 ℃ of sintering 6 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.2% under 0.3%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 6
Said with embodiment 2, it is in 0.8% the polyacrylamide solution that difference is to add massfraction, and in the industrial combustion gas stove 1600 ℃ of sintering 8 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.2% under 0.3%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 7
Said with embodiment 2, difference is to add massfraction and is respectively in 0.4% and 0.6% the Z 150PH and polyacrylamide solution, and in nitrogen nitrogen atmosphere electric furnace 1750 ℃ of sintering 5 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.2% under 0.3%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 8
Said with embodiment 2, difference is to add 10 grams, and to mix x be 10% the stable powdered zirconium oxide of methyl ethyl diketone yttrium, Yttrium trinitrate and yttrium isopropoxide; With the wet base of wad under 50 ℃ temperature dry 20 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.4% under 0.65%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 9
Said with embodiment 2, difference is to add 30 grams, and to mix x be 9% the stable powdered zirconium oxide of Yttrium trichloride; With the wet base of wad under 80 ℃ temperature dry 30 hours.The made ZrO that contains
2Fibreboard performance is following: unit weight 400kg/m
3, thermal conductivity is 0.28W/mK, shrinking percentage is being to be 1.4% under 0.65%, the 2100 ℃ * 1h condition under the 1650 ℃ * 24h condition.
Embodiment 10
Said with embodiment 3, difference is the wet base of wad under 120 ℃ temperature dry 25 hours.
Claims (6)
1. the preparation method of a zirconia ceramic beaverboard may further comprise the steps:
(1) chopping: the Zirconium oxide fibre weak point is cut to 1mm-3mm;
(2) slurrying: short fiber and the fully stabilized zirconia fine powder that cuts placed kiln basin in mass ratio 1: 0～0.5 ratio; Adding massfraction then is the combination agent solution of 0.1-1%; Be mixed with Zirconium oxide fibre slurry and stirring, churning time was not less than 3 minutes;
(3) filtering molding: mould is placed kiln basin, open vacuum pump,, obtain the wet base of wad of moulding through vacuum suction filter;
(4) drying: the wet base of wad is carried out drying in 50-120 ℃ of scope, the time is 20-30 hour;
(5) high temperature sintering: the wad that drying is good, be positioned over sintering in the High Temperature Furnaces Heating Apparatus, sintering temperature is 1600 ℃-1750 ℃, time 5-8 hour, obtains zirconium oxide fiber board;
Described Zirconium oxide fibre is a complete stable cubic phase fiber, and diameter is the 8-15 micron;
Described Zirconium oxide fibre is to adopt the following steps preparation:
1) according to zirconium oxychloride: the ratio of ethanol=100g: 800～1000ml is dissolved in zirconium oxychloride in the ethanol; According to mol ratio is zirconium oxychloride: methyl ethyl diketone: the ratio of triethylamine=1: 1.8～2.0: 2.5 is measured methyl ethyl diketone and triethylamine; Be dissolved in jointly in another part ethanol with the ethanol equivalent of dissolved oxygen zirconium chloride; 0 ℃～50 ℃ with agitation condition under; The alcohol dilution liquid atomizing of methyl ethyl diketone and triethylamine is joined in the zirconium oxychloride alcohol dilution liquid, add the continued stirring and obtain the golden transparent reaction solution;
2) evaporate to dryness ethanol is the dissolution with solvents solvend with acetone, removes by filter the insolubles Triethylammonium chloride, reclaims acetone, must contain the zirconium organic polymer;
3) according to the ratio of reactant zirconium oxychloride: ethanol=100g: 10～50ml; Product is contained the zirconium organic polymer dissolve in the ethanol, and be zirconium white: yttrium oxide=80%～91% according to mol ratio: 20%～9% ratio, mix yttrium salt; Sealing and standing obtains spinning solution;
4) adopt centrifugal pan to get rid of a method and obtain to contain the zirconium organic polymer fiber, under special atmosphere, heat-treat, obtain cubic phase zircite crystal fibre; Said special atmosphere is organic steam, nitrogen, water vapor or their mixed-gas atmosphere, and organic steam is to contain the steam that the zirconium organic polymer soln adds thermogenesis.
2. the preparation method of zirconia ceramic beaverboard according to claim 1; It is characterized in that; Described Zirconium oxide fibre is through uht treatment, and described uht treatment step is: the fiber after using gas flame that diameter produces as 8-12 centimetre burner to thermal treatment is jetted 1800 ℃-2200 ℃ of flame temperatures; The winding-up time is 5min-1h, and gas flame is more than one in hydrogen, acetylene, propane, Sweet natural gas, coal gas or the coal mine gas flame.
3. the preparation method of zirconia ceramic beaverboard according to claim 1, it is characterized in that: described powdered zirconium oxide is that x is the stable zirconium white of yttrium salt of 8%-15%, normal temperature is cube crystalline phase down.
4. the preparation method of zirconia ceramic beaverboard according to claim 3, it is characterized in that: described yttrium salt is more than one in Yttrium trinitrate, methyl ethyl diketone yttrium, yttrium isopropoxide or the Yttrium trichloride.
5. the preparation method of zirconia ceramic beaverboard according to claim 1, it is characterized in that: described organic bond is Z 150PH, SEPIGEL 305 or both mixtures.
6. the preparation method of zirconia ceramic beaverboard according to claim 1 is characterized in that: described High Temperature Furnaces Heating Apparatus is a kind of in air atmosphere electric furnace, nitrogen nitrogen atmosphere electric furnace, vacuum test electric furnace or the industrial combustion gas stove.
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| CN106396701A (en) * | 2016-08-30 | 2017-02-15 | 山东磊宝锆业科技股份有限公司 | Production method of high-purity zirconium oxide plates |
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| CN108301071A (en) * | 2018-01-17 | 2018-07-20 | 太原理工大学 | A kind of preparation method of zirconium carbide crystal fibre and its zirconium carbide crystal fibre of preparation |
| CN108585842B (en) * | 2018-05-24 | 2020-09-22 | 宁波海纳机械有限公司 | High-performance engine heat shield and preparation method thereof |
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