CN103757751B - A kind of preparation method of super high temperature zirconia ceramic fiber - Google Patents
A kind of preparation method of super high temperature zirconia ceramic fiber Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of super high temperature zirconia ceramic fiber, main employing following steps: with zirconium carbonate, yttrium nitrate and nitric acid for main raw material, take deionized water as retarder thinner, stir directly reaction at ambient temperature and generate the composite polymeric solution containing yttrium zirconium ion; Decompression distillation concentrated solution, finally obtains yttrium zirconium ion complex sol spinning solution, gets rid of silk obtain containing yttrium zirconium inorganic hydrate fiber through high speed centrifugation; The heat treatment of special atmosphere is carried out to yttrium zirconium inorganic hydrate fiber and superhigh temperature process can obtain yttrium zirconium mixed oxide ceramic fibre.Preparation process of the present invention is simple, and the crystal fibre composition of preparation is single, and purity is high, has stable high-temperature performance, and can use for a long time in the temperature range below 2250 DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of zirconia ceramics fiber, particularly a kind of preparation method of super high temperature zirconia ceramic fiber, belong to insulation, technical field of refractory materials.
Background technology
The physicochemical properties of the excellences such as zirconia has fusing point high (2715 DEG C), high-temperature steam forces down, corrosion-resistant, anti-oxidant, have a wide range of applications as heat insulating refractory material in high-temperature field more than 1700 DEG C, generally adopt the form of hollow ball brick to use at present.Hollow ball brick is compared with crystal fibre, and thermal conductivity factor is large, and thermal capacitance is high, and heat insulation effect is poor.But traditional mullite crystal fiber and the maximum operation (service) temperature of alpha-alumina crystals fiber only have 1400 DEG C and 1600 DEG C, cannot the hot environment more than 1700 DEG C use, and complete stable cubic phase zircite crystal fibre is just a kind of fibrous material that can meet the use of this type of hyperthermal environments.Although zirconia has above-mentioned numerous advantage, but because zirconia exists three kinds of crystalline phases, monoclinic phase, Tetragonal and Emission in Cubic, each other certain stable under can mutually transform, and with bulk effect (7%-9%), cause the Zirconium oxide fibre without stabilization processes to rupture, efflorescence, has a strong impact on its high-temperature resistance and service life.The transforming relationship of the various crystalline phase of zirconia is as follows:
Zirconia ceramics has to pass through stabilization processes could form the stable goods of geomery; Also appropriate stabilizing agent must be added in Zirconium oxide fibre and high performance goods could be obtained.Research finds: Y
3+add and can replace Zr
4+cATION forms substitution solid solution, thus stops crystal transfer, makes Emission in Cubic or Tetragonal at room temperature keep getting off, allows fiber be in stable state, to improve the stability in use of crystal fibre.The yittrium oxide adding more than 9% molar fraction in zirconia can obtain entirely stable Emission in Cubic, and the ceramic fibre of its correspondence has best high-temperature stability, and service life is also the longest.
At present, some common inorfils adopt fusion method as the suitability for industrialized production of alumina silicate fibre, quartz fibre, glass fibre etc., namely directly raw material is adopted resistance furnace or electric arc furnaces heating and melting, obtain staple fibre through centrifugal drying silk or air flow blowing, the fiber generally produced with fusion method all belongs to noncrystalline fiber.Because zirconia fusing point is too high, its fiber cannot adopt direct fusion method to prepare.Up to now, the preparation of zirconia crystal fiber mainly contains infusion process, mixing method and sol-gel process.
Infusion process: in the zirconium oxychloride that viscose (as hydrate cellulose) or whole fabric are immersed in 2M ~ 2.5M or zirconyl nitrate solution, soak 3h ~ 6h in 20-25 DEG C to take out, the material of such process is dry in atmosphere, then pyrolysis and calcining is carried out, volatilization organic component, obtains the Zirconium oxide fibre with certain TENSILE STRENGTH.Infusion process is more convenient, but the high uneven fibre structure of the obtained fiber porosity is loose, intensity is lower, poor-performing, and the production cycle is long.
Mixing method: be mixed with mixed solution with organic polymer (as polyvinyl alcohol) and the particle diameter additive Preparation of Fine Powders such as zirconates and yittrium oxide within the specific limits.The method (as centrifugal drying silk method, spinning head method, air flow blowing spinning etc.) that spinning is conventional, then sinters, is solidified into fiber.Mixing method technics comparing is complicated, simultaneously Y
3+be difficult to replace Zr uniformly etc. CATION
4+cATION forms substitution solid solution, is not easy to obtain complete stable cubic phase crystal fibre and consumes the energy greatly, generally not adopting in production.
Colloidal sol spin processes: by the colloidal sol of sol-gel process synthesis containing zirconium polymerization long-chain, utilize dry spinning, the fiber be spun into drying on spinning roller becomes gelatinous fibre, heat-treat (effect is removing volatile component), the fiber that then calcined oxide thing skeleton obtains has good mechanical performance.In the spinning presoma that this method obtains, zirconium content is high, spinning properties good, without the need to adding other auxiliary agent, there is not the defect remaining because auxiliary agent decomposes, just can obtain the zirconia crystal fiber with higher-strength through calcined crystallization in calcination process.Colloidal sol spin processes technique is simple and convenient, and obtained fibre composition is single, the good and even thickness of continuity.Unique shortcoming is that the fiber porosity is high, but colloidal sol spin processes is widely used at present.The method that this patent adopts is just sol-gel processing.
Calendar year 2001, the proper carat Ba Di of India, proper special lucky grade is being called (Zirconiafibrematspreparedbyasol-gelspinningtechniche in " sol-gel technique prepares Zirconium oxide fibre felt ", P.K.Chakrabarty, M.Chatterjee, etal, " JournalOftheEuropeanCeramicSociety ", 2001, (21), P355-361.) method utilizing sol-gel process to prepare Zirconium oxide fibre felt is reported: acetic acid peptization hydrous zirconium oxide(HZO) obtains colloidal sol, mix yttrium nitrate used as stabilizers, utilize multi-holed jet spinning, obtain cancellated gelatinous fibre felt, 150 DEG C of dry 1h, be heat-treated to 1300 DEG C again, obtain fibre diameter 10 μm, the round pie Zirconium oxide fibre felt that thickness is indefinite.But colloidal sol spinning solution poor stability prepared by the method, easy gelation and losing efficacy; Spun gelatinous fibre bonds mutually because water is wet, and can only obtain cancellated fibrofelt after calcining, range of application is narrow.
2004, the people such as Shandong University Xu Dong applied for a patent: Zirconium oxide fibre cotton (patent No. ZL200410024264.7) prepared by organic poly-zirconium precursor body spinning solution.Adopt methyl alcohol to make solvent in patent, utilize zirconium oxychloride, acetylacetone,2,4-pentanedione, triethylamine to generate containing zirconium organic polymer soln for raw material directly reacts under 0 DEG C ~ 50 DEG C and stirring condition; Evaporate to dryness methyl alcohol is that dissolution with solvents DDGS filters insoluble matter triethylamine hydrochloride with oxolane; Reclaim oxolane, the product obtained and yttrium salt (mixing the yttrium nitrate used as stabilizers being equivalent to zirconia yittrium oxide=92% ~ 99%:1% ~ 8% mol ratio) are dissolved in methyl alcohol preparation spinning solution, get rid of silk through high speed centrifugation and obtain containing zirconium organic polymer fiber.But prepared by this patent is the cellucotton of Tetragonal or Tetragonal, Emission in Cubic mixing, the easy efflorescence of high temperature, and service life is short, can only use by the environment below 1600 DEG C, the solvent that this patent uses simultaneously is methyl alcohol, and very large to the physical impairment of operator, the meaning of practical application is less.
2009, Shandong University applied for a patent: the preparation method (patent No. ZL200910013781.7) of complete stable cubic phase zircite crystal fibre.Adopt absolute ethyl alcohol to be retarder thinner in patent, utilize zirconium oxychloride, acetylacetone,2,4-pentanedione, triethylamine to generate containing zirconium organic polymer soln for raw material directly reacts under 0 DEG C ~ 50 DEG C and stirring condition; Evaporate to dryness ethanol, is dissolution with solvents DDGS with acetone, filters insoluble matter triethylamine hydrochloride; Reclaim acetone, the product obtained and yttrium salt (mixing the yttrium nitrate used as stabilizers being equivalent to zirconia yittrium oxide=80% ~ 91%:9% ~ 20% mol ratio) are dissolved in ethanol preparation spinning solution, get rid of silk through high speed centrifugation and obtain containing zirconium organic polymer fiber; , take the heat treatment of special atmosphere and superhigh temperature process to containing zirconium organic polymer fiber and get final product.The raw material Alternative that this patent adopts is complicated, causes the high cost of fiber.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of preparation method of super high temperature zirconia ceramic fiber, prepared zirconia ceramics fiber fineness is high, can use for a long time under hyperthermal environments.
The present invention is achieved by the following technical solutions:
(1) with zirconium carbonate, yttrium nitrate and nitric acid for main raw material, take water as retarder thinner, stir directly reaction at ambient temperature and generate and contain the composite polymeric solution of yttrium zirconium ion;
(2) decompression distillation concentrated solution, finally obtains yttrium zirconium complex sol spinning solution;
(3) get rid of silk through high speed centrifugation and obtain the inorganic hydrate fiber containing yttrium zirconium;
(4) heat treatment of special atmosphere is carried out to yttrium zirconium inorganic hydrate fiber and superhigh temperature process can obtain yttrium zirconium mixed oxide ceramic fibre.
Described special atmosphere is benzene vapour, nitrogen, argon gas, water vapour or their mixed-gas atmosphere.
Ceramic fibre composition prepared by the present invention is single, and purity is high, has stable high-temperature performance, and can use for a long time in the temperature range below 2250 DEG C.
The present invention compared with prior art has following excellent results:
(1) containing the synthesis technique simple (one-step synthesis) of yttrium zirconium ion composition polymer;
(2) complicated equipment (only needing reactor) is not needed; Environmentally safe;
(3) super high temperature zirconia ceramic fiber prepared, has stable high-temperature performance, free from admixture; Can use for a long time in temperature range below 2250 DEG C.
Accompanying drawing explanation
Fig. 1 is containing yttrium zirconium ion composite polymer fibers scanned photograph.
Fig. 2 is super high temperature zirconia ceramic fiber photo.
Fig. 3 is the stereoscan photograph of super high temperature zirconia ceramic fiber.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
embodiment 1
The preparation method of complete stable cubic phase zircite crystal fibre of the present invention is for adopting following steps:
(1) claim according to yittrium oxide: the ratio of zirconia mol ratio=10%:90% takes yttrium nitrate 40.85g and zirconium carbonate 100g is dissolved in deionized water, and the consumption of deionized water is 2 times of 329.2g of yttrium nitrate and zirconium carbonate gross mass; According to zirconium carbonate: nitric acid mol ratio=1:4 measures nitric acid 183ml(content 65%-68%), and under room temperature 30 DEG C and stirring condition, nitric acid is joined in the mixed solution of zirconium carbonate and yttrium nitrate, add rear continuation stirring 2 hours, obtain water white transparency reactant liquor, be the composite polymeric solution containing yttrium zirconium ion.
(2) the yttrium zirconium complex sol spinning fluid viscosity that obtains of reduced pressure concentration is within the scope of 2 ~ 10Pas;
(3) adopt centrifugal pan to get rid of a method spinning, be 90 DEG C in temperature, centrifuge speed is 7000r/min, centrifugal pan edge line speed 30m/s; Getting rid of wire tray aperture is 0.05 ~ 0.15mm, gets rid of filament diameter 350-380mm, being thrown away at a high speed by spinning solution, obtaining the polywater compound fiber containing yttrium zirconium ion compound of unordered accumulation from getting rid of wire tray edge;
(4) by being placed in the program control high temperature furnace of atmosphere heat treatment containing the polywater compound fiber of yttrium zirconium ion compound, under special atmosphere, with the programming rate of 1 DEG C/min, it is carried out to the heat treatment of room temperature ~ 1200 DEG C; Special atmosphere uses to 500 DEG C ~ 1200 DEG C, obtains complete stable cubic phase zircite crystal fibre;
(5) use gas to burn shuttle kiln, fuel is pure natural gas, maximum temperature 1700 DEG C in kiln; Temperature rise rate 1 DEG C/min; Temperature retention time 8 hours; Can obtain pure, the sufficient complete stable cubic phase zircite crystal fibre of grain development, diameter 5-15 micron, length 1-20 centimetre, purity more than 99.9% is Long-Time Service below 2250 degree.
embodiment 2
As described in Example 1, difference is namely changed to 658.4g by 329.2g by the consumption of deionized water being changed to 4 times by yttrium nitrate and zirconium carbonate gross mass 2 times in step (1); Zirconium carbonate; Nitric acid mol ratio becomes 1:4.5 from 1:4, and the consumption of nitric acid becomes 206ml from 183ml, and the concentration of dope of step (2) reduced pressure concentration is changed to 10-15Pas by 2-10Pas.
embodiment 3
As described in Example 1, difference be by step (1) by the consumption of deionized water by yttrium nitrate and zirconium carbonate gross mass 2 times this be 5 times and be namely changed to 823g by 329.2g; Zirconium carbonate: nitric acid mol ratio becomes 1:5 from 1:4, the consumption of nitric acid becomes 229ml from 183ml, changes the concentration of dope of step (2) reduced pressure concentration into 20-25Pas by 2-10Pas.
embodiment 4
As described in Example 1, difference is that temperature step (1) nitric acid being added yttrium nitrate and the zirconium carbonate aqueous solution changes 5 DEG C into by 30 DEG C, adding rear mixing time 2 hours, should be 10-15Pas by the concentration of dope of step (2) reduced pressure concentration by 2-10Pas
embodiment 5
As described in Example 1, difference is that temperature step (1) nitric acid being added yttrium nitrate and the zirconium carbonate aqueous solution changes 45 DEG C into by 30 DEG C, adding rear mixing time 1 hour, should be 20-25Pas by the concentration of dope of step (2) reduced pressure concentration by 2-10Pas
embodiment 6
As described in Example 1, difference is equivalent to zirconia by step (2) according to mol ratio: the ratio of yittrium oxide=85%:15%, mixes 64.6 yttrium nitrates, have complete stable cubic phase zircite crystal fibre to obtain in spinning solution.
embodiment 7
As described in Example 1, difference is equivalent to zirconia by step (2) according to mol ratio: the ratio of yittrium oxide=80%:20%, mixes 91.9g yttrium nitrate, have complete stable cubic phase zircite crystal fibre to obtain in spinning solution.
embodiment 8
As described in Example 1, difference is that the temperature of centrifugal drying silk in step (3) is become 105 DEG C from 90 DEG C, centrifuge speed changes 8000r/min into, getting rid of wire tray edge line speed is 35m/s, comparatively example 1 result is slightly little for the average diameter of the fiber obtained, but average length more routine l result is slightly short.
embodiment 9
As described in Example 1, difference is 80 DEG C by the temperature of centrifugal drying silk in step (3), and centrifuge speed changes 4700r/min into, and getting rid of wire tray edge line speed is 23.5m/s, the average diameter of the fiber obtained comparatively example 1 result is slightly large, but average length comparatively example 1 result is slightly long.
embodiment 10
As described in EXAMPLE l, difference changes 0.5 DEG C/min by step (4) into the heat treated programming rate carrying out room temperature ~ 1200 DEG C containing zirconium organic polymer fiber,
embodiment 11
As described in EXAMPLE l, difference changes 1.5 DEG C/min by step (4) into the heat treated programming rate carrying out room temperature ~ 1200 DEG C containing zirconium organic polymer fiber.
embodiment 12
As described in Example 1, difference changes 2 DEG C/min by step (4) into the heat treated programming rate carrying out room temperature ~ 1200 DEG C containing zirconium organic polymer fiber,
embodiment 13
As described in EXAMPLE l, difference changes 1750 DEG C by step (5) into the temperature that fiber carries out superhigh temperature process, and the kiln inside holding time became 4 hours from 8 hours.
embodiment 14
As described in EXAMPLE l, difference changes 1650 DEG C by step (5) into the temperature that fiber carries out superhigh temperature process, and the kiln inside holding time became 10 hours from 8 hours.
Claims (2)
1. a preparation method for super high temperature zirconia ceramic fiber, is characterized in that adopting following steps:
(1) with zirconium carbonate, yttrium nitrate and nitric acid for main raw material, take water as retarder thinner, stir directly reaction at ambient temperature and generate and contain the composite polymeric solution of yttrium zirconium ion;
The step generated containing the composite polymeric solution of yttrium zirconium ion is as follows: according to yittrium oxide: the ratio of zirconia mol ratio=9 ~ 20%:80 ~ 91% takes yttrium nitrate and zirconium carbonate is dissolved in deionized water, the consumption of deionized water is 2 ~ 5 times of yttrium nitrate and zirconium carbonate gross mass; According to zirconium carbonate: nitric acid mol ratio=1:4 ~ 5 measure nitric acid, and under room temperature 15 DEG C ~ 45 DEG C and stirring condition, nitric acid is joined in the mixed solution of zirconium carbonate and yttrium nitrate, add rear continuation stirring 1 ~ 2 hour, obtain water white transparency reactant liquor, be the composite polymeric solution containing yttrium zirconium ion;
(2) decompression distillation concentrated solution, finally obtains yttrium zirconium complex sol spinning solution; The yttrium zirconium complex sol spinning fluid viscosity that reduced pressure concentration obtains is within the scope of 2 ~ 25Pas;
(3) get rid of silk through high speed centrifugation and obtain the inorganic hydrate fiber containing yttrium zirconium; Described centrifugal drying silk method is that centrifugal pan gets rid of a method spinning, and be 70 DEG C ~ 120 DEG C in temperature, centrifuge speed is 4700r/min ~ 8000r/min; Getting rid of wire tray aperture is 0.05 ~ 0.15mm, under getting rid of the condition of filament diameter 250 ~ 400mm, being thrown away at a high speed by spinning solution, obtaining the polywater compound fiber containing yttrium zirconium ion compound of unordered accumulation from getting rid of wire tray edge;
(4) heat treatment of special atmosphere is carried out to yttrium zirconium inorganic hydrate fiber and superhigh temperature process can obtain yttrium zirconium mixed oxide ceramic fibre;
The heat treatment step of described special atmosphere is: by being placed in the program control high temperature furnace of atmosphere heat treatment containing the polywater compound fiber of yttrium zirconium ion compound, under special atmosphere, with the programming rate of 1 DEG C/min ~ 5 DEG C/min, it is carried out to the heat treatment of room temperature ~ 1200 DEG C; Special atmosphere uses to 500 DEG C ~ 1200 DEG C;
Described superhigh temperature is more than 1700 DEG C;
Described special atmosphere is benzene vapour, nitrogen, argon gas, water vapour or their mixed-gas atmosphere.
2. the preparation method of a kind of super high temperature zirconia ceramic fiber according to claim 1, is characterized in that
Described superhigh temperature treatment step is: use gas to burn shuttle kiln, fuel is pure natural gas, maximum temperature 1600 DEG C ~ 1800 DEG C in kiln; Temperature rise rate 0.1 DEG C/min ~ 3 DEG C/min; Temperature retention time 4 ~ 8 hours.
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| CN105369393A (en) * | 2014-08-12 | 2016-03-02 | 山东宏瑞超高温纤维科技有限公司 | Zirconium oxide ceramic fiber preparation method |
| CN111774402B (en) * | 2020-06-24 | 2021-12-28 | 天津市丽碧朗环保科技有限公司 | Industrial organic solid waste treatment method |
Citations (4)
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| CN1459418A (en) * | 2003-06-10 | 2003-12-03 | 山东大学 | Method and equipment of preparing high performance zirconium oxide continuous fiber |
| CN102181962A (en) * | 2010-09-30 | 2011-09-14 | 南京理工大学 | Method for preparing thin-diameter zirconium oxide fibers and fiber board thereof |
| CN102775143A (en) * | 2012-08-22 | 2012-11-14 | 安徽同和晶体新材料股份有限公司 | Method for preparing fully-stabilized tetragonal-phase zirconia crystal fibers |
| CN103193480A (en) * | 2013-03-11 | 2013-07-10 | 绍兴市圣诺超高温晶体纤维材料有限公司 | Preparation method of high-performance zirconia ceramic fibers |
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| JPH04100921A (en) * | 1990-08-17 | 1992-04-02 | Nippon Shokubai Co Ltd | Production of zirconia-based fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1459418A (en) * | 2003-06-10 | 2003-12-03 | 山东大学 | Method and equipment of preparing high performance zirconium oxide continuous fiber |
| CN102181962A (en) * | 2010-09-30 | 2011-09-14 | 南京理工大学 | Method for preparing thin-diameter zirconium oxide fibers and fiber board thereof |
| CN102775143A (en) * | 2012-08-22 | 2012-11-14 | 安徽同和晶体新材料股份有限公司 | Method for preparing fully-stabilized tetragonal-phase zirconia crystal fibers |
| CN103193480A (en) * | 2013-03-11 | 2013-07-10 | 绍兴市圣诺超高温晶体纤维材料有限公司 | Preparation method of high-performance zirconia ceramic fibers |
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