CN105622095A - High-temperature-resistant zirconia fiber ceramic plate and preparation method thereof - Google Patents

High-temperature-resistant zirconia fiber ceramic plate and preparation method thereof Download PDF

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CN105622095A
CN105622095A CN201610087751.0A CN201610087751A CN105622095A CN 105622095 A CN105622095 A CN 105622095A CN 201610087751 A CN201610087751 A CN 201610087751A CN 105622095 A CN105622095 A CN 105622095A
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zirconium oxide
temperature
fibre
fiber
preparation
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张琦
张焱
祖群
赵骁儒
奚秋香
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Sinoma Science and Technology Co Ltd
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Abstract

The invention relates to a preparation method of a high-temperature-resistant zirconia fiber ceramic plate, comprising the steps: heating zirconia precursor fiber prepared with a centrifugal thread spinner in a protective atmosphere at a low temperature rise rate to 500 DEG C to remove water molecules and organic components in the precursor fiber to obtain carbonized fiber, defibering and pulping the carbonized fiber, and vacuum filtrating and drying to prepare a zirconia precursor fiber plate, and sintering at high temperature so that carbonized substance burns completely and a crystal transformation process is finished. The method is simple and easy to perform, the fiber is mutually staggered via heat shrinkage during preparation so that the obtained zirconia fiber plate is compact, there is no need to add an adhesive, thus avoiding introduction of impurities, ensuring zero harmful substance generated in usage of the fiber plate and ensuring greenness, and the prepared zirconia fiber plate is useful in a long term at 1500 DEG C and widely applicable to the field of thermal insulation and isolation.

Description

A kind of High-temperature-reszirconium zirconium oxide fiber ceramics plate and preparation method thereof
Technical field
The present invention relates to a kind of Zirconium oxide fibre ceramic wafer, can be widely applied to the field of employment of more than 1500 DEG C and equipment, belong to inorganic adiabator technical field.
Background technology
Along with the development of the rise of the NPD projects such as new work engine and aeronautical and space technology, increasingly exigence material can keep its working strength and modulus under high temperature oxidizing conditions. Zirconia ceramics fiber, owing to having the features such as high-melting-point, higher heat stability, corrosion resistance, thermal shock resistance, and becomes the high-temperature oxidation-resistant material of most research potential. Zirconia ceramics fiber and fiber board products thereof will be widely used in fields such as Aero-Space, guided missile and rocket engine interior trim, atomic reactor, Industrial Stoves, high temperature filtrations.
Restriction due to the current technology of preparing of domestic Zirconium oxide fibre own, the Zirconium oxide fibre intensity of preparation is relatively low, the technology of preparing directly preparing fibre board is more difficult, in published traditional method preparing zirconium oxide fiber board, need to add the materials such as binding agent, flocculant, fortifying fibre, not only complex process, but also introduce other components, reduce zirconium oxide fiber board applied at elevated temperature performance, especially the organic component added at high temperature carbonization, release harmful gas, causes environmental pollution, and personnel when to confined space produce harm. Therefore, seek a kind of simplicity, safety, green, free of contamination zirconia ceramic beaverboard preparation method particularly important.
Summary of the invention
It is an object of the invention to solve the deficiencies in the prior art, it is provided that a kind of zirconia ceramic beaverboard, its serviceability at high temperature is good.
Another object of the present invention also resides in the preparation method providing above-mentioned zirconia ceramic beaverboard, and preparation technology is simple, need not add binding agent and reinforcing material, efficient pollution-free.
For solving the problems referred to above, the technical solution adopted in the present invention is as follows:
A kind of High-temperature-reszirconium zirconium oxide fiber ceramics plate, the thickness of this Zirconium oxide fibre ceramic wafer is 2��30mm, and density is 0.1��0.35g/cm3, described Zirconium oxide fibre ceramic wafer is made up of the Zirconium oxide fibre that fibre diameter is 1��12 ��m.
The preparation method of above-mentioned High-temperature-reszirconium zirconium oxide fiber ceramics plate, comprises the steps:
(1) adopt centrifugal drying wire feed mechanism for zirconium oxide precursor fibre: to be added continuously to get rid of a head by zirconium oxide precursor solution, drive through high-speed electric expreess locomotive and throw away filamentation, collect and obtain zirconium oxide precursor fibre.
(2) zirconium oxide precursor fibre is carried out presintering, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after carbonization, obtain fibre stuff, fibre stuff is poured in molding pond, after stirring, draining successively, vacuum draw, roll-in, obtain the wet embryo of fibre board, namely obtain the fibre board of carbonization after drying.
(4) fibre board of carbonization is carried out high temperature sintering, as required cutting, namely obtain zirconium oxide fiber board.
In step (1), in described zirconium oxide precursor solution, the mol ratio of zirconium oxide, yittrium oxide, magnesium oxide, silicon oxide, sodium oxide, aluminium oxide and calcium oxide is: (80��96): (3��20): (0��10), (0��5): (0��5): (0��1): (0��1), the adjustment of ratio between each component, is the Zirconium oxide fibre in order to obtain Tetragonal or Emission in Cubic. Its preparation method can be synthesized by organic coordination method, it is also possible to is prepared by sol-gal process, and in order to obtain good fibroblast effect, both of which needs to add spin finish aid and is adjusted.
Such as, organic coordination method is adopted to prepare zirconium oxide precursor solution, mol ratio according to above-mentioned oxide calculates the quality of corresponding raw material, in advance yttrium salt, aluminium salt etc. are dissolved in the aqueous solution of spin finish aid, add suitable quantity of water and form uniform glue, again under intensively stirred condition, it is gradually added in the ethylene glycol monoethyl ether solution of solubilized depolymerization acetylacetone,2,4-pentanedione zirconium, forms zirconium oxide precursor solution.
In step (2), the temperature of described presintering is 500��800 DEG C, and temperature retention time is 0.5��2h. The organic component being primarily intended in removal zirconium oxide precursor fibre of described presintering, this process is along with the volume contraction of fiber, owing to whole sintering process also has formation and the transformation of zirconium oxide crystal formation, the same contraction along with fiber volume, sinters the impact on size after the contraction of presintering reduces fibre board molding.
In step (2), described sintering atmosphere is air, nitrogen or steam, and heating rate is 0.5��5 DEG C/min, and heating rate is unsuitable too fast, and speed is too fast, and organic volatile is also fast, and fibre damage is relatively big, and fiber very easily breaks up.
In step (3), the purpose discongesting slurrying is to make fiber rotate in water high speed, bundle fiber is dissociated into ultimate fibre, is only uniformly dispersed by fiber, by fibre cutting, will not will not damage fibre strength. The mass concentration of described fibre stuff is 0.5��2%, and the too small reduction production efficiency of concentration, concentration is excessive affects dispersion effect, causes product density uneven.
In step (3), described baking temperature is 90��110 DEG C.
In step (4), the temperature of described high temperature sintering is 1000��1500 DEG C, temperature retention time is 0.5��5h, described high-temperature sintering process is burnt completely by carbide on the one hand, being the transformation of zirconium oxide crystal formation on the other hand, whole process is the process of fibre board densification, forms more, higher overlap joint between fiber simultaneously, the three-dimensional net structure making fibre board is completely embedded, and imparts the mechanical strength that zirconia ceramic beaverboard goods are higher.
In step (4), it is 5��15 DEG C/min that the heating rate of described high temperature sintering controls, and heating rate is comparatively fast for inhibiting grain growth, it is achieved fiber densification.
The present invention compared with prior art, its remarkable advantage: the preparation method of the present invention be prone to molding, simple to operate flexibly, cost is low, safety non-pollution, the zirconia ceramic beaverboard of preparation has the heat-proof quality of excellence, uses temperature 1500 DEG C.
Detailed description of the invention
Further illustrate technical scheme by the examples below.
Embodiment 1
(1) by the oxide after burning till with mass ratio for ZrO2:Y2O3:Al2O3: the zirconium oxide spinning liquid as precursor of CaO=95.2:3.7:1:0.1 preparation, to get rid of silk by centrifugation and prepare zirconium oxide precursor fibre, the zirconium oxide precursor fibre average diameter of preparation is 2 ��m.
(2) by precursor fibre, at full N2Atmosphere sintering furnace in, with the ramp of 0.5 DEG C/min to 500 DEG C, be incubated 0.5h, naturally cool to room temperature, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after the carbonization of preparation, fibre stuff poured in molding pond, stir, draining, vacuum draw, roll-in, obtain the wet embryo of fibre board, 100 DEG C dry after obtain the fibre board of carbonization.
(4) with the speed of 10 DEG C/min, the fibre board of carbonization being risen to 1000 DEG C and carry out high temperature sintering, be incubated 0.5h, naturally cool to room temperature, namely cutting obtains a kind of tetragonal phase zirconium oxide fibre board as required.
The zirconium oxide fiber board density prepared is 0.1g/cm3, thickness is 30mm, places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.
Embodiment 2
(1) by the oxide after burning till with mass ratio for ZrO2:Y2O3:Al2O3: the zirconium oxide spinning liquid as precursor of MgO=82.8:15:0.5:1.7 preparation, to get rid of silk by centrifugation and prepare zirconium oxide precursor fibre, the zirconium oxide precursor fibre average diameter of preparation is 6 ��m.
(2) by precursor fibre, in sintering furnace, with the ramp of 0.5 DEG C/min to 600 DEG C, it is incubated 0.5h, naturally cools to room temperature, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after the carbonization of preparation, fibre stuff poured in molding pond, stir, draining, vacuum draw, roll-in, obtain the wet embryo of fibre board, 110 DEG C dry after obtain the fibre board of carbonization.
(4) with the speed of 5 DEG C/min, the fibre board of carbonization being risen to 1100 DEG C and carry out high temperature sintering, be incubated 0.5h, naturally cool to room temperature, namely cutting obtains a kind of cubic phase zircite fibre board as required.
The zirconium oxide fiber board density prepared is 0.15g/cm3, thickness is that 20mm places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.
Embodiment 3
(1) by the oxide after burning till with mol ratio for ZrO2:Y2O3:SiO2:Al2O3:Na2The zirconium oxide spinning liquid as precursor of O=82:15:1.5:0.5:1 preparation, gets rid of silk by centrifugation and prepares zirconium oxide precursor fibre, and the zirconium oxide precursor fibre average diameter of preparation is 3.8 ��m.
(2) by precursor fibre, in sintering furnace, with the ramp of 2 DEG C/min to 600 DEG C, it is incubated 1h, naturally cools to room temperature, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after the carbonization of preparation, fibre stuff poured in molding pond, stir, draining, vacuum draw, roll-in, obtain the wet embryo of fibre board, 100 DEG C dry after obtain the fibre board of carbonization.
(4) fibre board of mould and internal carbonization is risen to 1300 DEG C with the speed of 10 DEG C/min and carry out high temperature sintering, be incubated 5h, naturally cool to room temperature, open mould, namely obtain zirconium oxide fiber board.
The zirconium oxide fiber board density prepared is 0.35g/cm3, thickness is 2mm, places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.
Embodiment 4
(1) by the oxide after burning till with mol ratio for ZrO2:Y2O3:SiO2:Al2O3: the zirconium oxide spinning liquid as precursor of CaO=90.8:8:0.5:0.5:0.2 preparation, to get rid of silk by centrifugation and prepare zirconium oxide precursor fibre, the zirconium oxide precursor fibre average diameter of preparation is 9.2 ��m.
(2) by precursor fibre, in sintering furnace, with the ramp of 5 DEG C/min to 800 DEG C, it is incubated 2h, naturally cools to room temperature, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after the carbonization of preparation, fibre stuff poured in molding pond, stir, draining, vacuum draw, roll-in, obtain the wet embryo of fibre board, 100 DEG C dry after obtain the fibre board of carbonization.
(4) fibre board of mould and internal carbonization is risen to 1400 DEG C with the speed of 15 DEG C/min and carry out high temperature sintering, be incubated 3h, naturally cool to room temperature, open mould, namely obtain zirconium oxide fiber board.
The zirconium oxide fiber board density prepared is 0.25g/cm3, thickness is 15mm, places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.
Embodiment 5
(1) by the oxide after burning till with mol ratio for ZrO2:Y2O3:SiO2:Al2O3:Na2The zirconium oxide spinning liquid as precursor of O:MgO=80:8:4.7:0.8:0.5:6 preparation, gets rid of silk by centrifugation and prepares zirconium oxide precursor fibre, and the zirconium oxide precursor fibre average diameter of preparation is 11.4 ��m.
(2) by precursor fibre, in sintering furnace, with the ramp of 4 DEG C/min to 700 DEG C, it is incubated 1h, naturally cools to room temperature, obtain the fiber after carbonization.
(3) undertaken discongesting slurrying by the fiber after the carbonization of preparation, fibre stuff poured in molding pond, stir, draining, vacuum draw, roll-in, obtain the wet embryo of fibre board, 95 DEG C dry after obtain the fibre board of carbonization.
(4) fibre board of mould and internal carbonization is risen to 1500 DEG C with the speed of 10 DEG C/min and carry out high temperature sintering, be incubated 4h, naturally cool to room temperature, open mould, namely obtain zirconium oxide fiber board.
The zirconium oxide fiber board density prepared is 0.3g/cm3, thickness is 8mm, places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.

Claims (9)

1. a High-temperature-reszirconium zirconium oxide fiber ceramics plate, it is characterised in that the thickness of described Zirconium oxide fibre ceramic wafer is 2��30mm, density is 0.1��0.35g/cm3, described Zirconium oxide fibre ceramic wafer is made up of the Zirconium oxide fibre that fibre diameter is 1��12 ��m.
2. the preparation method of the High-temperature-reszirconium zirconium oxide fiber ceramics plate described in claim 1, it is characterised in that comprise the steps:
(1) adopt centrifugal drying wire feed mechanism for zirconium oxide precursor fibre: to be added continuously to get rid of a head by zirconium oxide precursor solution, drive through high-speed electric expreess locomotive and throw away filamentation, collect and obtain zirconium oxide precursor fibre;
(2) zirconium oxide precursor fibre is carried out presintering, obtain the fiber after carbonization;
(3) undertaken discongesting slurrying by the fiber after carbonization, obtain fibre stuff, fibre stuff is poured in molding pond, after stirring, draining successively, vacuum draw, roll-in, obtain the wet embryo of fibre board, namely obtain the fibre board of carbonization after drying;
(4) fibre board of carbonization is carried out high temperature sintering, as required cutting, namely obtain zirconium oxide fiber board.
3. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterized in that, in step (1), in described zirconium oxide precursor solution, the mol ratio of zirconium oxide, yittrium oxide, magnesium oxide, silicon oxide, sodium oxide, aluminium oxide and calcium oxide is: (80��96): (3��20): (0��10), (0��5): (0��5): (0��1): (0��1).
4. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterised in that in step (2), the temperature of described presintering is 500��800 DEG C, and temperature retention time is 0.5��2h.
5. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterised in that in step (2), described sintering atmosphere is air, nitrogen or steam, and heating rate is 0.5��5 DEG C/min.
6. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterised in that in step (3), the mass concentration of described fibre stuff is 0.5��2%.
7. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterised in that in step (3), described baking temperature is 90��110 DEG C.
8. the preparation method of High-temperature-reszirconium zirconium oxide fiber ceramics plate as claimed in claim 2, it is characterised in that in step (4), the temperature of described high temperature sintering is 1000��1500 DEG C, and temperature retention time is 0.5��5h.
9. the preparation method of the High-temperature-reszirconium zirconium oxide fiber ceramics plate as described in any one of claim 2 to 8, it is characterised in that in step (4), it is 5��15 DEG C/min that the heating rate of described high temperature sintering controls.
CN201610087751.0A 2016-02-16 2016-02-16 High-temperature-resistant zirconia fiber ceramic plate and preparation method thereof Pending CN105622095A (en)

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CN107698253A (en) * 2017-11-11 2018-02-16 郑州方铭高温陶瓷新材料有限公司 A kind of preparation method of thermal protection ceramic wafer applied to rocket launch platform
CN110557853A (en) * 2019-07-18 2019-12-10 武汉纺织大学 Method for manufacturing high-temperature sintered body capable of generating heat by electrifying, product and application method
CN110699849A (en) * 2019-10-30 2020-01-17 明光市铭垚凹凸棒产业科技有限公司 Attapulgite nanofiber membrane for water treatment and preparation method thereof
CN112250450A (en) * 2020-09-15 2021-01-22 航天特种材料及工艺技术研究所 Preparation method of heat insulation tile blank capable of resisting high temperature of 2000 DEG C
CN112661522A (en) * 2021-01-12 2021-04-16 南京理工大学 Method for improving filling power of ceramic fiber prepared by template method

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CN107698253A (en) * 2017-11-11 2018-02-16 郑州方铭高温陶瓷新材料有限公司 A kind of preparation method of thermal protection ceramic wafer applied to rocket launch platform
CN107698253B (en) * 2017-11-11 2020-03-27 郑州方铭高温陶瓷新材料有限公司 Preparation method of thermal protection ceramic plate applied to rocket launching platform
CN110557853A (en) * 2019-07-18 2019-12-10 武汉纺织大学 Method for manufacturing high-temperature sintered body capable of generating heat by electrifying, product and application method
CN110557853B (en) * 2019-07-18 2022-08-09 武汉纺织大学 Method for manufacturing high-temperature sintered body capable of generating heat by electrifying, product and application method
CN110699849A (en) * 2019-10-30 2020-01-17 明光市铭垚凹凸棒产业科技有限公司 Attapulgite nanofiber membrane for water treatment and preparation method thereof
CN112250450A (en) * 2020-09-15 2021-01-22 航天特种材料及工艺技术研究所 Preparation method of heat insulation tile blank capable of resisting high temperature of 2000 DEG C
CN112661522A (en) * 2021-01-12 2021-04-16 南京理工大学 Method for improving filling power of ceramic fiber prepared by template method

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