CN108178647A - A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light - Google Patents

A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light Download PDF

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CN108178647A
CN108178647A CN201711497591.8A CN201711497591A CN108178647A CN 108178647 A CN108178647 A CN 108178647A CN 201711497591 A CN201711497591 A CN 201711497591A CN 108178647 A CN108178647 A CN 108178647A
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fiber
porous
binding agent
obtains
ceramics
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杜海燕
李玲玉
胡小侠
陈小平
王文杰
杨立娜
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Tianjin University
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Tianjin University
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Abstract

The present invention relates to a kind of preparation methods of the heat-insulated porous mullite fiber ceramics of high-strength light.By deionized water, polyacrylamide, boron carbide powder and Ludox mixing, planetary ball mill ball milling is put into, obtains being uniformly mixed binding agent slurry；Chopped polycrystalline mullite fibre is added in binding agent slurry and is stirred, obtains fibre stuff；Fibre stuff is poured into mold of the lower end with filter screen, is filtered with vacuum pump, obtains the wet base of porous fiber ceramic；After the wet base demoulding of porous fiber ceramic, it is put into ultra low temperature freezer and is freezed；It complete green body will be freezed is put into freeze drier freeze-drying and obtain porous mullite fiber ceramics dry body, dry body is put into sintering in high temperature furnace obtains porous mullite fiber ceramics.The present invention overcomes lead to the problem of porous fiber ceramic density is high, and the porosity is low, and compression strength is low due to bonding to be unevenly distributed.The porous ceramics binding agent of the present invention is evenly distributed at fiber nodes, and fiber is served and is supported and fixed.

Description

A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light
Technical field
The present invention relates to porous fiber ceramic technical fields, more more particularly to a kind of heat-insulated mullite fiber of high-strength light The preparation method of hole ceramics.
Background technology
With the rapid development of aerospace field, various countries increasingly rise the development of novel high speed aerospace craft Temperature.Due to spacecraft in atmosphere to be subjected to the complex environments such as serious heat, vibration and impact during High Mach number flight It influences, therefore higher requirement is proposed to the thermally protective materials and structure of spacecraft, need it with relatively low density, it is higher Intensity and preferable heat-proof quality etc..
Porous mullite fiber ceramics are the materials based on mullite fiber, and mutually overlap joint forms the fibre similar to Bird's Nest Pass through high-temperature agglomerant firm connection at the node of dimension network structure, fiber and fiber.Mullite with this microstructure Porous fiber ceramic has the porosity of superelevation, relatively low density, higher intensity and relatively low thermal conductivity, it is ensured that space flight Safety of the device in high-speed flight.Therefore, porous mullite fiber ceramics are with its lightweight, high-strength, high temperature resistant, anti-oxidant, corrosion resistant The advantages that erosion, is as important candidate material a kind of in spacecraft thermal protection system.
The preparation process of porous mullite fiber ceramics mainly includes molding, dry, several steps such as high-temperature calcination, specifically Using vacuum filtration method or pressurization fluid-discharge therapy shaping fiber porous ceramics, to carry out hot-air to the wet base of porous fiber ceramic and doing It is dry, porous fiber ceramic most is made through high-temperature heat treatment afterwards.Existed using porous mullite fiber ceramics made from such technique Microstructure is uneven, and then leads to the problem of intensity is low, and thermal insulation is poor.It is main reason is that wet base is done using hot-air During dry, high-temperature agglomerant can be migrated with moisture evaporation to the surface of material so that material surface binder content is high, internal Binder content is few, greatly influences the mechanical property and thermal property of porous fiber ceramic.Chinese patent CN105565845A Using the gelatinization and ablation characteristics of starch, fiber multihole thermal insulation tile is prepared for using starch in-situ solidifying method, in certain journey Solves the migration problem of binding agent in drying process on degree.But the preparation method provided according to this patent, complex process, compared with It is difficult to control, it is unfavorable for the large-scale production and industrialization of material, so by using the change of drying mode, is dried by hot-air It is changed to be freeze-dried, binding agent is made to be solidificated in node location rapidly, prepare binding agent and be evenly distributed and be only distributed at node Porous mullite fiber ceramics.It is up to now, porous there is no mullite fiber is prepared using freeze-drying by looked into patent The report of ceramics, therefore the present invention, using Ludox as binding agent, is molded using mullite fiber as basis material by being filtered by vacuum, Freeze-drying, the method for high temperature sintering have prepared the heat-insulated porous mullite fiber ceramics of high-strength light.
Invention content
It is an object of the invention to overcome existing porous mullite fiber ceramics due to binding agent caused by preparation process point The technical issues of cloth is uneven, poor mechanical property provides a kind of preparation of the heat-insulated porous mullite fiber ceramics of high-strength light Method, selection polycrystalline mullite fibre are matrix, and Ludox is high-temperature agglomerant, and boron carbide powder is sintering aid, by true Sky filters molding and wet base is made, and wet base is freeze-dried, and high temperature sintering obtains having the mullite fiber of three-dimensional net structure more Hole ceramics.
To achieve the above object, the specific technical solution of use is as follows：
A kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light, step are as follows：
(1) it by deionized water, polyacrylamide, boron carbide powder and Ludox mixing, is stirred with blender until mixing Uniformly, it is put into planetary ball mill and carries out ball milling, obtain uniformly mixed binding agent slurry；
(2) polycrystalline mullite fibre through washing, being chopped, being sieved is added in the binding agent slurry that step (1) obtains, It is stirred while adding with blender, continues to stir after fiber has added, until fiber is uniformly dispersed in binding agent slurry In material, well dispersed fibre stuff is obtained；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump tune Section filters pressure and is filtered, and obtains the wet base of porous fiber ceramic；
(4) after the wet base demoulding of the porous mullite fiber ceramics that obtain step (3), be put into ultra low temperature freezer control it is cold Freeze temperature to be freezed, it is complete until freezing；
(5) the complete green body of freezing for obtaining step (4) is put into drying in freeze drier, obtains dry green body, Green body is put into high temperature furnace later, sintering obtains porous mullite fiber ceramics.
Binding agent is polyacrylamide by mass ratio in the step (1)：Boron carbide：Ludox：Water=(0.27~ 0.63)：(0.3~0.7)：10：90 component composition；It is 10min~20min, Ball-milling Time 8h with blender mixing time ~12h.
A diameter of 8 μm~12 μm of the chopped mullite fiber that the step (2) adds in, length are 400 μm~700 μm, are accounted for The 5%~15% of binding agent stock quality, mixing time are 15min~25min.
It is 0.06MPa~0.08MPa that pressure is filtered in the step (3).
Cryogenic temperature is -20 DEG C~-80 DEG C in the step (4), and cooling time is 8h~for 24 hours.
In the step (5) in -50 DEG C, the freeze drier of 75Pa, for 24 hours~30h is dried.
Sintering schedule control is is heated to the heating rate of 2 DEG C/min~5 DEG C/min in step (5) the high temperature stove 200 DEG C~400 DEG C, then 1300 DEG C~1500 DEG C are heated to the heating rate of 5 DEG C/min~7 DEG C/min, keep the temperature 3h~5h.
The present invention adjusts vacuum filtration molding by improving each group distribution ratio in binder solution, and freeze-drying is high Each process procedures such as temperature sintering make preparation process be suitable for preparing the heat-insulated porous mullite fiber ceramics of high-strength light.This Invent prepare porous mullite fiber ceramics in 0.30g/cm3~0.42g/cm3Between, compression strength reach 1.3MPa~ 1.9MPa, thermal conductivity is between 0.08W/ (mK)~0.12W/ (mK), and its microstructure is mutually overlapped for fiber in three Tie up network, binding agent viscose fibre node.
Compared with the preparation method of existing porous mullite fiber ceramics, the invention mainly has following advantage：
1st, the present invention adds in surfactant polyacrylamide in silicon sol solution improves the viscosity of slurry, utilizes high score The space steric effect of sub- surfactant improves dispersion suspension characteristic of the fiber in binder solution, more conducively fiber three Tie up the structure of network.
2nd, the present invention adds in sintering aid boron carbide powder, B in binder solution4C powder is at 700 DEG C~900 DEG C The B of oxidation reaction generation melting occurs2O3, it is wrapped in SiO2Around particle, make SiO2Particle softens at low temperature, promotees Into SiO2Particle is sintered, and improves its secure bond to fiber.
3rd, freeze-drying is used to prepare porous fiber ceramic by the present invention for the first time, utilizes the rapid cured excellent of freeze-drying Point, efficiently solve shell caused by binding agent is migrated with moisture evaporation to sample surfaces in hot-air drying process it is hard in The loose heterojunction structure problem in portion.
4th, the porous mullite fiber ceramics internal bond agent prepared by the present invention is evenly distributed, and is only bonded in fiber nodes Place, plays fiber and supports and fixes.
Description of the drawings
Fig. 1 is the microscopic appearance figure (SEM figures) of porous mullite fiber ceramics obtained in embodiment 1.
Fig. 2 is the microscopic appearance figure (SEM figures) of porous mullite fiber ceramics obtained in embodiment 3.
Fig. 3 is the microscopic appearance figure (SEM figures) of porous mullite fiber ceramics obtained in embodiment 6.
Specific embodiment
In order to better understand the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the embodiment.
Embodiment 1：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.27g polyacrylamides, 0.3g boron carbide powders, (the Ludox density used is 8ml Ludox 1.25g/cm3, similarly hereinafter), the mixing of 90ml deionized waters with blender stirring 10min until being uniformly mixed, is put into planetary ball mill Ball milling 8h is carried out, obtains uniformly mixed binding agent slurry；
(2) a diameter of 8 μm of 6.32g is weighed, length is that 400 μm of chopped polycrystalline mullite fibre is added to 100ml steps (1) it in the binding agent slurry obtained, is stirred while adding with blender, continues to stir 15min after fiber has added, directly It is uniformly dispersed in binding agent slurry to fiber, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.06MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -20 DEG C of ultra low temperature freezers It is freezed, freezing is for 24 hours；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa For 24 hours, dry green body is obtained, dry green body is put into high temperature furnace, sintering schedule control is with the heating rate of 2 DEG C/min 200 DEG C are heated to, then 1300 DEG C are heated to the heating rate of 5 DEG C/min, keeps the temperature 3h, sintering obtains the porous pottery of mullite fiber Porcelain, the density of the SEM image sample as shown in Figure 1 obtained by sample is 0.34g/cm3, compression strength reaches 1.5MPa, thermal conductivity Rate is at 0.089W/ (mK).
Embodiment 2：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.3g polyacrylamides, 0.5g boron carbide powders, 8ml Ludox, 90ml deionized waters mixing, with stirring Device stirring 15min is put into planetary ball mill and carries out ball milling 9h, obtain uniformly mixed binding agent slurry up to being uniformly mixed；
(2) a diameter of 10 μm of 6.32g is weighed, length is that 500 μm of chopped mullite fiber is added to 100ml steps (1) It in obtained binding agent slurry, is stirred while adding with blender, continues to stir 20min after fiber has added, until Fiber is uniformly dispersed in binding agent slurry, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.06MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -20 DEG C of ultra low temperature freezers It is freezed, freezing is for 24 hours；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa 26h obtains dry green body, and dry green body is put into high temperature furnace, and sintering schedule control is with the heating rate of 2 DEG C/min 200 DEG C are heated to, then 1300 DEG C are heated to the heating rate of 5 DEG C/min, keeps the temperature 4h, sintering obtains the porous pottery of mullite fiber Porcelain, the density of sample is 0.30g/cm3, compression strength reaches 1.5MPa, and thermal conductivity is at 0.087W/ (mK).
Embodiment 3：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.5g polyacrylamides, 0.5g boron carbide powders, 8ml Ludox, 90ml deionized waters mixing, with stirring Device stirring 20min is put into planetary ball mill and carries out ball milling 12h, obtain uniformly mixed binding agent slurry up to being uniformly mixed；
(2) a diameter of 10 μm of 10g is weighed, length is that 600 μm of chopped polycrystalline mullite fibre is added to step (1) and obtains Binding agent slurry in, stirred while adding with blender, continue after fiber has added stir 25min, until fiber It is uniformly dispersed in binding agent slurry, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.07MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -60 DEG C of ultra low temperature freezers It is freezed, cooling time 18h；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa For 24 hours, dry green body is obtained, dry green body is put into high temperature furnace, sintering schedule control is with the heating rate of 3 DEG C/min 300 DEG C are heated to, then 1400 DEG C are heated to the heating rate of 7 DEG C/mim, keeps the temperature 4h, sintering obtains the porous pottery of mullite fiber Porcelain, the SEM image obtained by sample is as shown in Fig. 2, the density of sample is 0.33g/cm3, compression strength reaches 1.8MPa, thermal conductivity Rate is at 0.12W/ (mK).
Embodiment 4：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.63g polyacrylamides, 0.7g boron carbide powders, 8ml Ludox, 90ml deionized waters mixing, with stirring Device stirring 20min is put into planetary ball mill and carries out ball milling 12h, obtain uniformly mixed binding agent slurry up to being uniformly mixed；
(2) a diameter of 12 μm of 6.32g is weighed, the chopped polycrystalline mullite fibre that length is 700 μm is added to step (3) and obtains To binding agent slurry in, stirred while adding with blender, continue after fiber has added stir 25min, until fibre Dimension is uniformly dispersed in binding agent slurry, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.08MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -80 DEG C of ultra low temperature freezers It is freezed, cooling time 10h；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa 30h obtains dry green body, and dry green body is put into high temperature furnace, and sintering schedule control is with the heating rate of 5 DEG C/min 400 DEG C are heated to, then 1400 DEG C are heated to the heating rate of 7 DEG C/mim, keeps the temperature 5h, sintering obtains the porous pottery of mullite fiber Porcelain, the density of sample is 0.30g/cm3, and compression strength reaches 1.4MPa, and thermal conductivity is at 0.102W/ (mK).
Embodiment 5：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.63g polyacrylamides, 0.7g boron carbide powders, 8ml Ludox, 90ml deionized waters mixing, with stirring Device stirring 10min enters planetary ball mill and carries out ball milling 10h, obtain uniformly mixed binding agent slurry up to being uniformly mixed；
(2) a diameter of 10 μm of 6.32g is weighed, the chopped polycrystalline mullite fibre that length is 600 μm is added to step (3) and obtains To binding agent slurry in, stirred while adding with blender, continue after fiber has added stir 25min, until fibre Dimension is uniformly dispersed in binding agent slurry, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.08MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -80 DEG C of ultra low temperature freezers It is freezed, cooling time 8h；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa 28h obtains dry green body, and dry green body is put into high temperature furnace, and sintering schedule control is with the heating rate of 4 DEG C/min 300 DEG C are heated to, then 1300 DEG C are heated to the heating rate of 6 DEG C/min, keeps the temperature 3h, sintering obtains the porous pottery of mullite fiber Porcelain, the density of sample is 0.30g/cm3, compression strength reaches 1.3MPa, and thermal conductivity is at 0.08W/ (mK).
Embodiment 6：
The preparation method of the heat-insulated porous mullite fiber ceramics of a kind of high-strength light of the present embodiment, specifically according to following step Suddenly it carries out：
(1) by 0.27g polyacrylamides, 0.6g boron carbide powders, 8ml Ludox, 90mi deionized waters mixing, with stirring Device stirring 10min is put into planetary ball mill and carries out ball milling 10h, obtain uniformly mixed binding agent slurry up to being uniformly mixed；
(2) a diameter of 10 μm of 15.80g is weighed, length is that 600 μm of chopped polycrystalline mullite fibre is added to step (1) it in the binding agent slurry obtained, is stirred while adding with blender, continues to stir 25min after fiber has added, directly It is uniformly dispersed in binding agent slurry to fiber, obtains well dispersed fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump, It sets suction filtration pressure to be filtered as 0.08MPa, obtains the wet base of porous fiber ceramic；
(4) it after the wet base demoulding of porous mullite fiber ceramics obtained step (3), is put into -80 DEG C of ultra low temperature freezers It is freezed, cooling time 9h；
(5) the complete green body of freezing for obtaining step (4), is put into -50 DEG C, dry in the freeze drier of 75Pa 30h obtains dry green body, and dry green body is put into high temperature furnace, and sintering schedule control is with the heating rate of 2 DEG C/min 200 DEG C are heated to, then 1500 DEG C are heated to the heating rate of 5 DEG C/min, keeps the temperature 4h, sintering obtains the porous pottery of mullite fiber Porcelain, the SEM image obtained by sample is as shown in figure 3, the density of sample is 0.42g/cm3, compression strength reaches 1.9MPa, thermal conductivity Rate is at 0.12W/ (mK).

Claims (9)

1. a kind of preparation method of the heat-insulated porous mullite fiber ceramics of high-strength light, it is characterized in that step is as follows：
(1) it by deionized water, polyacrylamide, boron carbide powder and Ludox mixing, is stirred with blender up to being uniformly mixed, It is put into planetary ball mill and carries out ball milling, obtain uniformly mixed binding agent slurry；
(2) polycrystalline mullite fibre through washing, being chopped, being sieved is added in the binding agent slurry that step (1) obtains, on one side Addition is stirred on one side with blender, continues to stir after fiber has added, until fiber is uniformly dispersed in binding agent slurry, Obtain fibre stuff；
(3) fibre stuff obtained in step (2) is poured into mold of the lower end with filter screen, opens vacuum pump and adjust pumping Filtering pressure power is filtered, and obtains the wet base of porous fiber ceramic；
(4) after the wet base demoulding of porous mullite fiber ceramics obtained step (3), it is put into control freezing temperature in ultra low temperature freezer Degree is freezed, complete until freezing；
(5) the complete green body of freezing for obtaining step (4) is put into drying in freeze drier, obtains dry green body, later Green body is put into high temperature furnace, sintering obtains porous mullite fiber ceramics.
2. the method as described in claim 1, it is characterized in that binding agent by mass ratio is polyacrylamide in the step (1)： Boron carbide：Ludox：Water=(0.27~0.63)：(0.3~0.7)：10：90 component composition.
3. the method as described in claim 1, it is characterized in that in the step (1) blender mixing time for 10min~ 20min, Ball-milling Time are 8h~12h.
4. the method as described in claim 1, it is characterized in that a diameter of 8 μm of the chopped mullite fiber that the step (2) adds in ~12 μm, length is 400 μm~700 μm, accounts for the 5%~15% of binding agent stock quality.
5. the method as described in claim 1, it is characterized in that the step (2) mixing time is 15min~25min.
6. the method as described in claim 1, it is characterized in that it is 0.06MPa~0.08MPa that pressure is filtered in the step (3).
7. the method as described in claim 1, it is characterized in that cryogenic temperature is -20 DEG C~-80 DEG C in the step (4), freezing Time is 8h~for 24 hours.
8. the method as described in claim 1, it is characterized in that in the step (5) in -50 DEG C, the freeze drier of 75Pa, Dry for 24 hours~30h.
9. the method as described in claim 1, it is characterized in that in the step (5) high temperature stove sintering schedule control be with 2 DEG C/ The heating rate of min~5 DEG C/min is heated to 200 DEG C~400 DEG C, then is heated to the heating rate of 5 DEG C/min~7 DEG C/min 1300 DEG C~1500 DEG C, keep the temperature 3h~5h.
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CN110498610A (en) * 2019-09-20 2019-11-26 景德镇陶瓷大学 A kind of ceramic surface jewel adornment high-temperature agglomerant and its application method
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Application publication date: 20180619