CN117902896A - Preparation method of lightweight heat-insulating zirconia fiber-based porous ceramic - Google Patents

Preparation method of lightweight heat-insulating zirconia fiber-based porous ceramic Download PDF

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CN117902896A
CN117902896A CN202410309469.7A CN202410309469A CN117902896A CN 117902896 A CN117902896 A CN 117902896A CN 202410309469 A CN202410309469 A CN 202410309469A CN 117902896 A CN117902896 A CN 117902896A
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fiber
zirconia
based porous
porous ceramic
mould
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刘礼龙
刘津
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Shanghai Nanjixing High Tech Co ltd
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Shanghai Nanjixing High Tech Co ltd
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Abstract

The invention belongs to the field of zirconia fiber-based porous ceramics, and discloses a preparation method of light heat-insulating zirconia fiber-based porous ceramics, which comprises the steps of uniformly mixing zirconia fibers and silica fibers, adding a certain amount of dispersing agent and starch after uniformly stirring, continuously stirring to obtain mixed fiber slurry, transferring the mixed fiber slurry into a mould, coating the mould by a polyvinyl chloride film, transferring the mould into a blast drying oven, preserving heat, taking out the mould, and demoulding to obtain a zirconia-silica fiber composite blank; and (3) placing the obtained zirconia-silica fiber composite blank body into a box-type furnace, and calcining to obtain the light heat-insulating zirconia fiber-based porous ceramic. The invention adopts the silicon oxide fiber as the high-temperature binder, and can not block the holes overlapped by the zirconium oxide fiber, thereby ensuring that the porous ceramic based on the zirconium oxide fiber has high porosity and low thermal conductivity.

Description

Preparation method of lightweight heat-insulating zirconia fiber-based porous ceramic
Technical Field
The invention belongs to the field of zirconia fiber-based porous ceramics, and particularly relates to a preparation method of light heat-insulating zirconia fiber-based porous ceramics.
Background
The porous zirconia (ZrO 2) ceramic not only has the characteristics of low density and low thermal conductivity, but also has the characteristics of lower thermal expansion coefficient, good chemical stability and thermal shock resistance, and has been widely applied in the fields of high-temperature thermal protection materials and functional materials. The zirconia fiber is an ideal heat insulation material in the ultra-high temperature environment with the temperature of more than 1600 ℃. Fiber morphology is maintained up to 2400 c, which is not achieved with other ceramic fibers. The zirconia fiber has a wide application range, and can be used in an oxidizing atmosphere, a reducing atmosphere and vacuum. Zirconia fiber can be used for processing or manufacturing various products, and zirconia fiber-based porous ceramics with zirconia fiber as a main matrix are one of the most important porous ceramics in the field of high-temperature heat insulation in recent years. The zirconia fiber-based porous ceramic can be used as a furnace lining of a high-temperature furnace and the like, an ultrahigh-temperature heat insulation layer in a space shuttle and other materials to prepare a high-temperature resistant composite material.
The zirconia fiber-based porous ceramic is mainly composed of zirconia fibers and a binder between the fibers. The most common binder at present is silica sol, which at high temperatures is converted to silica, thereby reacting with adjacent fibers to form zirconium silicate, which in turn binds the adjacent zirconia fibers together. However, such high temperature adhesives have serious drawbacks: the added silica sol is accumulated at the nodes of the fibers and is adsorbed on the surfaces of the fibers, so that the formed silica can fill the internal holes of the zirconia fiber-based porous ceramic, and the porosity of the porous ceramic is reduced. Therefore, there is an urgent need to develop a method for preparing zirconia porous ceramics with high porosity and low thermal conductivity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a lightweight heat-insulating zirconia fiber-based porous ceramic, which takes zirconia fiber as a matrix, silica fiber as a high-temperature binder, and bonds adjacent zirconia fiber by in-situ melting of the silica fiber, so that the zirconia fiber-based porous ceramic is ensured to have high porosity and low thermal conductivity.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a lightweight heat-insulating zirconia fiber-based porous ceramic, which comprises the following steps:
(1) Weighing zirconia fiber and silica fiber according to the mass ratio of 4-6:1, and uniformly mixing to obtain mixed fiber;
(2) Adding the mixed fiber into water, uniformly stirring, adding a dispersing agent and starch, and continuously uniformly stirring to obtain mixed fiber slurry;
(3) Transferring the mixed fiber slurry into a mould, coating the mould by using a polyvinyl chloride film, transferring the mould into a blast drying oven, taking out the mould after heat preservation, and demoulding to obtain a zirconia-silica fiber composite blank;
(4) And (3) placing the zirconia-silica fiber composite blank body into a box-type furnace, and calcining to obtain the light heat-insulating zirconia fiber-based porous ceramic.
Aiming at the problem that the porosity of the zirconia fiber-based porous ceramic is too low at present, the application provides the zirconia fiber-based porous ceramic with high porosity and low thermal conductivity, which is prepared by taking zirconia fibers as a matrix and silica fibers as a high-temperature binder. The high temperature binder used in the current common zirconia fiber-based porous ceramics is silica sol. However, during the molding process, silica sol adheres to the surface of zirconia due to the surface tension of the liquid, and a large area of liquid film is formed at the fiber nodes. After high temperature sintering, the silica formed can clog the pores between the fibers, resulting in too low porosity of the zirconia fiber-based porous ceramic.
In view of this problem, the present application proposes to use silica fibers as a high temperature binder. Firstly, uniformly mixing silicon oxide fibers and zirconium oxide, and then, in-situ curing by starch to form a zirconium oxide-silicon oxide fiber composite blank. After high temperature sintering, the silica fibers melt and react with adjacent zirconia fibers to bind the zirconia fibers together. In this process, the incorporated silica fibers do not clog the pores formed by the zirconia fibers. In addition, the disappearance of the melting of the silica fibers provides a large number of voids to some extent.
In the whole system, the zirconia fiber plays a role of a three-dimensional framework, and the silica fiber plays a role of a binder. If the zirconia fiber is too much, the silica fiber as a binder is too little, and the sample strength after high-temperature sintering is too low, so that pulverization is liable to occur. If the zirconia fiber is too small, a stable three-dimensional network structure cannot be formed inside the sample, and the sample can collapse and deform.
Further, the starch is one or more of corn starch, potato starch and tapioca starch.
Further, the dispersing agent is one or more of sodium hexametaphosphate, hydroxypropyl methylcellulose and polyacrylamide.
Further, in the mixed fiber slurry in the step (2), the mass fraction of the mixed fibers is 5-20wt%, if the mass fraction of the mixed fibers is lower than 5wt%, the mixed fibers are too small, and cannot be lapped into a three-dimensional skeleton structure in a blank stage, and if the mass fraction of the mixed fibers is higher than 20wt%, the viscosity of the whole slurry is too large, and aggregation is easy to occur among the mixed fibers; the mass fraction of the dispersing agent is 1-5wt%; the mass fraction of the starch is 3-15 wt%, if the starch content is lower than 3wt%, the effect of the starch serving as a room temperature binder is not obvious, the green body collapses after being dried, and if the starch content is higher than 15wt%, the viscosity of the solution is obviously increased, so that the added mixed fiber cannot be uniformly dispersed. Preferably, the mass fraction of the mixed fiber is 5-15 wt%, the mass fraction of the dispersing agent is 1-3 wt%, and the mass fraction of the starch is 5-10 wt%.
Further, the temperature of the blast drying box is 70-90 ℃, and the heat preservation time is 6-10 hours.
Further, the calcination temperature is 1400-1600 ℃, when the calcination temperature is lower than 1400 ℃, the silicon oxide fiber is not melted, the bonding effect can not be achieved, and the sample is easy to pulverize. If the calcination temperature is higher than 1600 ℃, the temperature resistance limit of the zirconia is also reached, the zirconia fiber can be damaged, and the mechanical property is reduced. The temperature rising rate is 2-10 ℃/min, and the heat preservation time is 1-3 h.
The invention has the advantages and positive effects that:
the invention provides a lightweight heat-insulating zirconia fiber-based porous ceramic, which is prepared by adopting silica fibers as a high-temperature binder, and improving the bonding property between zirconia fibers through the melting of the silica fibers at high temperature and the reaction of the silica fibers with the zirconia fibers.
Drawings
FIG. 1 is an SEM image at 500 times magnification of a zirconia fiber-based porous ceramic prepared in example 1;
FIG. 2 is an SEM image at 500 times magnification of a zirconia fiber-based porous ceramic prepared in example 2;
fig. 3 is an SEM image of the zirconia fiber-based porous ceramic prepared in comparative example 1 at 500 x magnification.
Detailed Description
For a better understanding of the present invention, the present invention will be described in further detail below with reference to the accompanying drawings. The features in the cases can be combined with each other without conflict. The starting materials used in the examples below were all commercially available analytically pure starting materials.
Example 1
The preparation method of the lightweight heat-insulating zirconia fiber-based porous ceramic comprises the following steps:
(1) Respectively weighing 8g of zirconia fiber and 2g of silica fiber, and uniformly mixing to obtain mixed fiber;
(2) Adding the mixed fiber into 83g of water, uniformly stirring, adding 1g of sodium hexametaphosphate and 6g of corn starch, and continuously uniformly stirring to obtain mixed fiber slurry;
(3) Transferring the mixed fiber slurry into a metal mold, coating the metal mold by using a polyvinyl chloride film, transferring the metal mold into a blast drying oven at 80 ℃, insulating for 8 hours, taking out the mold, and demolding to obtain a zirconia-silica fiber composite blank;
(4) And (3) heating the obtained zirconia-silica fiber composite blank to 1500 ℃ at a speed of 2 ℃/min, calcining at a high temperature, and preserving heat for 2 hours to obtain the zirconia fiber-based porous ceramic.
A scanning electron microscope image of the zirconia fiber-based porous ceramic prepared in example 1 is shown in FIG. 1.
Example 2
The preparation method of the lightweight heat-insulating zirconia fiber-based porous ceramic comprises the following steps:
(1) Respectively weighing 10g of zirconia fiber and 2g of silica fiber, and uniformly mixing to obtain mixed fiber;
(2) Adding the mixed fiber into 76g of water, uniformly stirring, adding 2g of hydroxypropyl methylcellulose and 10g of potato starch, and continuously uniformly stirring to obtain mixed fiber slurry;
(3) Transferring the mixed fiber slurry into a metal mold, coating the metal mold by using a polyvinyl chloride film, transferring the metal mold into a blast drying oven at 85 ℃, insulating for 10 hours, taking out the mold, and demolding to obtain a zirconia-silica fiber composite blank;
(4) And heating the obtained zirconia-silica fiber composite blank to 1400 ℃ at a speed of 5 ℃/min, calcining at a high temperature, and preserving heat for 3 hours to obtain the zirconia fiber-based porous ceramic.
A scanning electron microscope image of the zirconia fiber-based porous ceramic prepared in example 1 is shown in FIG. 2.
Comparative example 1
A method for preparing lightweight heat-insulating zirconia fiber-based porous ceramics, which is the same as that of example 1, is different from the method in the step (1) only in that no silica fiber is used, and silica sol having the same silica content as 2g of silica fiber is weighed.
A scanning electron microscope image of the zirconia fiber-based porous ceramic prepared in comparative example 1 is shown in FIG. 3.
Comparative example 2
A preparation method of a lightweight heat-insulating zirconia fiber-based porous ceramic is the same as that of example 1, except that in step (1), 2g of zirconia fiber and 8g of silica fiber are weighed respectively and mixed uniformly.
Comparative example 3
A preparation method of a lightweight heat-insulating zirconia fiber-based porous ceramic is the same as that of example 1, except that in step (1), 9.5g of zirconia fiber and 0.5g of silica fiber are weighed respectively and mixed uniformly.
Evaluation and characterization
Fig. 1 is an SEM image of the zirconia fiber-based porous ceramic prepared in example 1 at 500 x magnification, and fig. 2 is an SEM image of the zirconia fiber-based porous ceramic prepared in example 2 at 500 x magnification. Through tests, the zirconia fiber-based porous ceramic prepared in example 1 has a porosity of 90%, a compressive strength of 1.2MPa and a thermal conductivity of 0.082W.m -1·K-1; the zirconia fiber-based porous ceramic prepared in example 2 had a porosity of 87%, a compressive strength of 1.4MPa, and a thermal conductivity of 0.092W ·m -1·K-1. As can be seen from the SEM images, the zirconia fibers are lapped into a three-dimensional network structure, and no obvious binder is present inside the sample. The unique three-dimensional network structure endows the zirconia fiber-based porous ceramic material with the characteristics of light weight and heat insulation.
Fig. 3 is an SEM image of the zirconia fiber-based porous ceramic prepared in comparative example 1 at 500 x magnification. The test shows that the porosity of the prepared zirconia fiber-based porous ceramic is 72%, the compression strength is 3.4MPa, and the thermal conductivity is 0.193W m -1·K-1. As can be seen from SEM images, in the zirconia-fiber-based porous ceramic, many pores are filled with high-temperature binder silica, so that the porosity of the prepared zirconia-fiber-based porous ceramic is too low and the thermal conductivity is too high.
In comparative example 2, since zirconia fiber was excessively added, zirconia fiber as a skeleton could not form a stable three-dimensional network structure after sintering at high temperature, and dishing and cracking occurred in the sample. In comparative example 3, since the silica fibers were excessively added, there was insufficient adhesive between the zirconia fibers as a skeleton after sintering at high temperature, and the sample underwent pulverization.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that variations and modifications can be made without departing from the scope of the invention.

Claims (6)

1. The preparation method of the lightweight heat-insulating zirconia fiber-based porous ceramic is characterized by comprising the following steps of:
(1) Weighing zirconia fiber and silica fiber according to the mass ratio of 4-6:1, and uniformly mixing to obtain mixed fiber;
(2) Adding mixed fibers into water, uniformly stirring, adding a dispersing agent and starch, and continuously uniformly stirring to obtain mixed fiber slurry, wherein the mass fraction of the mixed fibers in the mixed fiber slurry is 5-20wt%, the mass fraction of the dispersing agent is 1-5wt%, and the mass fraction of the starch is 3-15wt%;
(3) Transferring the mixed fiber slurry into a mould, coating the mould by using a polyvinyl chloride film, transferring the mould into a blast drying oven, taking out the mould after heat preservation, and demoulding to obtain a zirconia-silica fiber composite blank;
(4) And (3) placing the zirconia-silica fiber composite blank body into a box-type furnace, and calcining to obtain the light heat-insulating zirconia fiber-based porous ceramic.
2. The method according to claim 1, wherein the starch is one or more of corn starch, potato starch, tapioca starch.
3. The preparation method according to claim 1, wherein the dispersing agent is one or more of sodium hexametaphosphate, hydroxypropyl methylcellulose and polyacrylamide.
4. The preparation method of the composite fiber slurry according to claim 1, wherein in the composite fiber slurry in the step (2), the mass fraction of the composite fiber is 5-15 wt%, the mass fraction of the dispersant is 1-3 wt%, and the mass fraction of the starch is 5-10 wt%.
5. The preparation method of claim 1, wherein the temperature of the forced air drying oven is 70-90 ℃ and the heat preservation time is 6-10 h.
6. The preparation method of claim 1, wherein the calcination temperature is 1400-1600 ℃, the heating rate is 2-10 ℃/min, and the heat preservation time is 1-3 h.
CN202410309469.7A 2024-03-19 2024-03-19 Preparation method of lightweight heat-insulating zirconia fiber-based porous ceramic Pending CN117902896A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2412134C1 (en) * 2009-09-23 2011-02-20 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Method of producing ceramic composite article
CN103524140A (en) * 2013-09-23 2014-01-22 天津大学 Oxide ceramic fiber board
CN105565845A (en) * 2015-12-14 2016-05-11 天津大学 Preparation method for porous ceramic fiber heat-insulation tile
CN108178647A (en) * 2017-12-28 2018-06-19 天津大学 A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light
CN112624776A (en) * 2020-12-24 2021-04-09 山东鲁阳浩特高技术纤维有限公司 Zirconia-alumina fiber composite wet module and preparation method thereof
CN116496069A (en) * 2023-04-26 2023-07-28 深圳市吉迩科技有限公司 Preparation method of fiber porous ceramic and fiber porous ceramic
CN116693324A (en) * 2023-08-07 2023-09-05 天津南极星隔热材料有限公司 Preparation method of lightweight heat-insulating aluminum titanate porous ceramic with multistage pore structure
CN117303927A (en) * 2023-11-28 2023-12-29 上海南极星高科技股份有限公司 Preparation method of high-strength heat-insulating composite alumina fiber-based porous ceramic

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2412134C1 (en) * 2009-09-23 2011-02-20 Российская Федерация, от имени которой выступает Министерство промышленности и торговли Российской Федерации (Минпромторг России) Method of producing ceramic composite article
CN103524140A (en) * 2013-09-23 2014-01-22 天津大学 Oxide ceramic fiber board
CN105565845A (en) * 2015-12-14 2016-05-11 天津大学 Preparation method for porous ceramic fiber heat-insulation tile
CN108178647A (en) * 2017-12-28 2018-06-19 天津大学 A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light
CN112624776A (en) * 2020-12-24 2021-04-09 山东鲁阳浩特高技术纤维有限公司 Zirconia-alumina fiber composite wet module and preparation method thereof
CN116496069A (en) * 2023-04-26 2023-07-28 深圳市吉迩科技有限公司 Preparation method of fiber porous ceramic and fiber porous ceramic
CN116693324A (en) * 2023-08-07 2023-09-05 天津南极星隔热材料有限公司 Preparation method of lightweight heat-insulating aluminum titanate porous ceramic with multistage pore structure
CN117303927A (en) * 2023-11-28 2023-12-29 上海南极星高科技股份有限公司 Preparation method of high-strength heat-insulating composite alumina fiber-based porous ceramic

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