CN105712716A - Zirconium oxide fiber ceramic plate and preparing method thereof - Google Patents
Zirconium oxide fiber ceramic plate and preparing method thereof Download PDFInfo
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
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Abstract
The invention relates to a method for preparing a zirconium oxide fiber ceramic plate through dry method formation. The method comprises the steps that zirconium oxide precursor fibers are prepared with a centrifugal thread throwing technology; in an environment with a protection atmosphere, the temperature is raised to 500 DEG C at a low speed, moisture and organic components in the precursor fibers are removed, and carbonized fibers are obtained; the carbonized fibers are loosened, evenly spread in a mold and sintered at the high temperature of 1200 DEG C, and then the zirconium oxide fiber plate is obtained. In the preparing process, the fibers are subjected to heat shrinkage, staggered and overlapped, and high strength is achieved on the condition that a binding agent does not need to be added; the influence of impurities on the high-temperature performance is avoided in the whole process which belongs to pure inorganic system preparation, and environment friendliness is achieved. The prepared zirconium oxide fiber plate can be used for a long time at 1500 DEG C and can be widely applied to the field of heat preservation and heat insulation.
Description
Technical field
The present invention relates to a kind of Zirconium oxide fibre ceramic wafer and preparation method thereof, 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 industries 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
The invention aims to solve the deficiency of above-mentioned existing technology of preparing, a kind of zirconia ceramic beaverboard is provided, its preparation technology is simple, need not add binding agent and reinforcing material, efficient pollution-free, will not reduce fibre board serviceability under the high temperature conditions.
Further object is that the preparation method that this zirconia ceramic beaverboard is provided.
For solving the problems referred to above, the technical solution adopted in the present invention is as follows:
A kind of Zirconium oxide fibre ceramic wafer, the thickness of this fibre board is 2～30mm, and density is 0.1～0.35g/cm3, described fibre board is made up of the Zirconium oxide fibre that fibre diameter is 1～12 μm.
The preparation method of above-mentioned Zirconium oxide fibre ceramic wafer, comprises the steps:
(1) adopt centrifugal tumbling machine, 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) by the fiber opening after carbonization, making fiber is loose unordered state.
(4) carbon fibre after shredding is spread layer by layer in lower mold, fiber after completing by lower mold pressure on the upper mold.
(5) whole mould is carried out high temperature sintering, then furnace cooling, open mould, 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 or 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), described shredding, is that by mini-bomb cotton machine, the fiber in certain sequence collected is carried out shredding separation, and making fiber is unordered dispersity, act in collusion between fiber, it is ensured that in the later stage more uniform contraction of sintering process fiber volume simultaneously.
In step (4), described mould is the density design according to required fibre board, certain size is left in the middle of upper/lower die, and this is sized larger than the size of fibre board, for the reserved size shunk, if simultaneously the density of fibre board is very big, one piece of ceramic wafer can be added at fibrous layer upper surface, the process of filament contraction gives certain pressure, makes fibre board more closely knit.
In step (5), the temperature of described high temperature sintering is 1000～1500 DEG C, temperature retention time is 0.5～10h, described sintering process is the most key step, and this process is burnt completely by carbide on the one hand, has been the transformation of zirconium oxide crystal formation on the other hand, whole process is the process of fibre board densification, form more, higher overlap joint between fiber simultaneously, make the three-dimensional net structure of fibre board be completely embedded, impart the mechanical strength that zirconia ceramic beaverboard goods are higher.
In step (5), the heating rate of described high temperature sintering is 5～15 DEG C/min, 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 mol 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 μm.
(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) fiber after the carbonization of preparation being carried out shredding to discongest, fiber is loose unordered dispersity.
(4) entering in lower mold by scattered carbon fibre uniform spreading, got togather by mold, whole mould is pushed in high temperature sintering furnace.
(5) fibre board of mould and internal carbonization is risen to 1000 DEG C with the speed of 5 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 0.15g/cm3, thickness is 26mm, 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 mol 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 μm..
(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) fiber after the carbonization of preparation being carried out shredding to discongest, fiber is loose unordered dispersity.
(4) entering in lower mold by scattered carbon fibre uniform spreading, got togather by mold, whole mould is pushed in high temperature sintering furnace.
(5) fibre board of mould and internal carbonization is risen to 1200 DEG C with the speed of 8 DEG C/min and carry out high temperature sintering, be incubated 8h, naturally cool to room temperature, open mould, namely obtain zirconium oxide fiber board.
The zirconium oxide fiber board density prepared is 0.2g/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 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 μm..
(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) fiber after the carbonization of preparation being carried out shredding to discongest, fiber is loose unordered dispersity.
(4) entering in lower mold by scattered carbon fibre uniform spreading, got togather by mold, whole mould is pushed in high temperature sintering furnace.
(5) 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 15h, 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 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 μm..
(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) fiber after the carbonization of preparation being carried out shredding to discongest, fiber is loose unordered dispersity.
(4) entering in lower mold by scattered carbon fibre uniform spreading, got togather by mold, whole mould is pushed in high temperature sintering furnace.
(5) 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 10h, 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 5
(1) by the oxide after burning till with mol ratio for ZrO2:Y2O3:SiO2:Al2O3: the zirconium oxide spinning liquid as precursor of Na2O:MgO=80:8:4.7:0.8:0.5:6 preparation, to get rid of silk by centrifugation and prepare zirconium oxide precursor fibre, the zirconium oxide precursor fibre average diameter of preparation is 11.4 μm..
(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) fiber after the carbonization of preparation being carried out shredding to discongest, fiber is loose unordered dispersity.
(4) entering in lower mold by scattered carbon fibre uniform spreading, got togather by mold, whole mould is pushed in high temperature sintering furnace.
(5) 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 8h, 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 10mm, places 30min under 1600 DEG C of high temperature, and fibre board keeps integrity, and efflorescence and shrinkage factor < 5% do not occur.
Claims (7)
1. a Zirconium oxide fibre ceramic wafer, 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 μm.
2. the preparation method of the Zirconium oxide fibre ceramic wafer described in claim 1, it is characterised in that comprise the steps:
(1) adopt centrifugal tumbling machine, 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) by the fiber opening after carbonization, making fiber is loose unordered state；
(4) carbon fibre after shredding is spread layer by layer in lower mold, fiber after completing by lower mold pressure on the upper mold；
(5) whole mould is carried out high temperature sintering, then furnace cooling, open mould, obtain zirconium oxide fiber board.
3. the preparation method of Zirconium oxide fibre ceramic wafer 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 Zirconium oxide fibre ceramic wafer 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 Zirconium oxide fibre ceramic wafer 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 Zirconium oxide fibre ceramic wafer as claimed in claim 2, it is characterised in that in step (5), the temperature of described high temperature sintering is 1000～1500 DEG C, and temperature retention time is 0.5～10h.
7. the preparation method of the Zirconium oxide fibre ceramic wafer as described in any one of claim 2 to 6, it is characterised in that in step (5), the heating rate of described high temperature sintering is 5～15 DEG C/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187254A (en) * | 2016-07-06 | 2016-12-07 | 南京理工宇龙新材料科技股份有限公司 | A kind of high strength fiberboard and preparation method thereof |
| CN112047745A (en) * | 2020-08-04 | 2020-12-08 | 山东金三河新材料科技有限公司 | Composite refractory fiber and preparation method thereof |
| CN112552061A (en) * | 2020-12-28 | 2021-03-26 | 海鹰空天材料研究院(苏州)有限责任公司 | Preparation method of ceramic fiber board |
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| 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 |
| CN103524140A (en) * | 2013-09-23 | 2014-01-22 | 天津大学 | Oxide ceramic fiber board |
| CN104193332A (en) * | 2014-08-24 | 2014-12-10 | 景德镇陶瓷学院 | Method for preparing zirconia fiber by using non-hydrolytic sol-gel process |
| KR101524728B1 (en) * | 2013-12-16 | 2015-06-01 | 부산대학교 산학협력단 | High heat -dissipating ceramic composite, manufacturing method therefor, and uses thereof |
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2016
- 2016-02-16 CN CN201610086237.5A patent/CN105712716A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103524140A (en) * | 2013-09-23 | 2014-01-22 | 天津大学 | Oxide ceramic fiber board |
| KR101524728B1 (en) * | 2013-12-16 | 2015-06-01 | 부산대학교 산학협력단 | High heat -dissipating ceramic composite, manufacturing method therefor, and uses thereof |
| CN104193332A (en) * | 2014-08-24 | 2014-12-10 | 景德镇陶瓷学院 | Method for preparing zirconia fiber by using non-hydrolytic sol-gel process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187254A (en) * | 2016-07-06 | 2016-12-07 | 南京理工宇龙新材料科技股份有限公司 | A kind of high strength fiberboard and preparation method thereof |
| CN112047745A (en) * | 2020-08-04 | 2020-12-08 | 山东金三河新材料科技有限公司 | Composite refractory fiber and preparation method thereof |
| CN112552061A (en) * | 2020-12-28 | 2021-03-26 | 海鹰空天材料研究院(苏州)有限责任公司 | Preparation method of ceramic fiber board |
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