CN117342880B - Continuous wet forming method for special-shaped surface ceramic fiber rigid heat-insulating tile - Google Patents
Continuous wet forming method for special-shaped surface ceramic fiber rigid heat-insulating tile Download PDFInfo
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- CN117342880B CN117342880B CN202311642272.7A CN202311642272A CN117342880B CN 117342880 B CN117342880 B CN 117342880B CN 202311642272 A CN202311642272 A CN 202311642272A CN 117342880 B CN117342880 B CN 117342880B
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- 239000000835 fiber Substances 0.000 title claims abstract description 151
- 239000000919 ceramic Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000002002 slurry Substances 0.000 claims abstract description 44
- 238000003860 storage Methods 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 238000000967 suction filtration Methods 0.000 claims abstract description 20
- 238000010009 beating Methods 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000004537 pulping Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 239000011148 porous material Substances 0.000 claims description 22
- 239000010453 quartz Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000012528 membrane Substances 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 5
- 229920002261 Corn starch Polymers 0.000 claims description 4
- 239000008120 corn starch Substances 0.000 claims description 4
- 239000012510 hollow fiber Substances 0.000 claims description 4
- 238000001471 micro-filtration Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims 1
- 238000009413 insulation Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 13
- 238000009826 distribution Methods 0.000 description 7
- 238000004062 sedimentation Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
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Abstract
The invention discloses a continuous wet forming method of a special-shaped ceramic fiber rigid heat-insulating tile, which comprises the following steps: mixing ceramic fibers, a sintering aid and a binder, adding water, pulping to obtain ceramic fiber slurry with a beating degree of 30-60 ︒ SR, and pumping the ceramic fiber slurry into a storage tank; transferring the filter screen to a storage tank, connecting a connecting pipe at the top of the filter screen with a vacuum pump, and performing vacuum suction filtration to obtain a wet blank on the surface of the filter screen; transferring the filter screen from the storage tank to a positioning die, transferring the next set of filter screen into the storage tank, and repeating the steps to form continuous preparation; and (3) taking the filter screen out of the wet blank in the positioning die, drying the wet blank and sintering. The invention can realize the continuous batch preparation of the special-shaped surface ceramic fiber rigid heat-insulating tile, and the special-shaped surface rigid heat-insulating tile with uniform green body density and high fiber orientation degree is obtained by controlling the beating degree of ceramic fiber slurry and adjusting the suction filtration mode and the filter screen structure and the fiber arrangement direction.
Description
Technical Field
The invention relates to the technical field of rigid heat-insulating tiles, in particular to a continuous wet forming method of a special-shaped ceramic fiber rigid heat-insulating tile.
Background
The ceramic fiber rigid heat-insulating tile is a key material of a reusable heat protection system of spacecrafts such as spacecrafts. The traditional wet forming method is limited by a process method, so that the cuboid block-shaped rigid heat-insulating tile can be prepared generally only. The simple rotating body thin-wall oxide ceramic fiber rigid heat-insulating tile component with the structural forms of a conical cylinder, a cylindrical surface cylinder body with the upper bottom surface and the lower bottom surface communicated with each other can be used as a hypersonic missile radome/window fiber matrix, a wave-transmitting heat-insulating cap in the radome, a high-temperature muffle furnace heat-insulating lining and the like. Due to the wide application field, the preparation of the simple special-shaped surface rigid heat insulation tile is getting more and more attention in recent years. At present, when preparing the rigid heat-insulating tile with the special-shaped surface of the simple rotating body, the blocky ceramic fiber rigid heat-insulating tile is generally reprocessed into a cone cylinder or a cylindrical cylinder with the upper bottom surface and the lower bottom surface communicated through a numerical control machine tool. The utilization rate of raw materials is less than or equal to 15%, and the arrangement direction of ceramic fibers in the processed member is uneven, so that the cover body has uneven key performances such as electrical performance and apparent heat conductivity coefficient.
In Chinese patent publication No. CN108252163A, which is the research of aerospace special materials and process technologies, a molding method of a simple special-shaped rigid heat-insulating tile blank body is disclosed, and only one blank body can be molded at a time, so that the efficiency is low; and the fiber orientation can not be controlled, which is not beneficial to improving the uniformity of the density, mechanical property and electrical property distribution in the rigid heat insulation tile-shaped surface. Chinese patent publication No. CN108727028A discloses a method for manufacturing a rigid heat-insulating tile blank by an additive manufacturing method, by which semi-automatic manufacturing of the rigid heat-insulating tile blank can be achieved, but the device is mainly used for manufacturing a rigid heat-insulating tile flat-plate blank, and is not applicable to a simple special-shaped-surface rotating body blank.
Disclosure of Invention
The invention provides a continuous wet forming method of a special-shaped ceramic fiber rigid heat-insulating tile, which aims to solve the problems that a special-shaped rigid heat-insulating tile of a simple rotating body cannot realize wet continuous forming, fiber orientation cannot be controlled and density uniformity of the manufactured special-shaped rigid heat-insulating tile is poor in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a continuous wet method forming method of a special-shaped ceramic fiber rigid heat-insulating tile comprises the following steps:
s1: mixing ceramic fibers, a sintering aid and a binder in a mass ratio of 1-1.5:0.04-0.05:0.01-0.03, adding water, pulping to obtain ceramic fiber slurry with a beating degree of 30-60 ︒ SR, and pumping the ceramic fiber slurry into a storage tank;
s2: transferring the filter screen into a storage tank to enable the filter screen to be immersed in the ceramic fiber slurry; the top and the bottom of the filter screen are closed, the inside of the filter screen is hollow, the side surface is a required special-shaped surface and is provided with filter holes with gradually reduced pore diameters from top to bottom, and the interval between the filter holes is gradually increased from top to bottom; the top of the filter screen is provided with a connecting pipe for communicating the inside of the filter screen with the vacuum pump;
s3: connecting the connecting pipe with a vacuum pump, performing vacuum suction filtration, and obtaining a wet blank on the surface of the filter screen;
s4: transferring the filter screen from the storage tank to a positioning die, transferring the next set of filter screen into the storage tank, and repeating S1 to S4 to form continuous preparation;
s5: and (3) taking the filter screen in the positioning die out of the wet blank, drying the wet blank, and sintering to obtain the special-shaped ceramic fiber rigid heat-insulating tile.
The invention firstly mixes ceramic fiber, sintering aid and binder and adds water to prepare ceramic fiber slurry with certain beating degree, then immerses the filter screen in the ceramic fiber slurry for vacuum filtration, when in suction filtration, the water in the slurry penetrates through the filter holes on the filter screen to enter the filter screen and is extracted from the connecting pipe at the top, the ceramic fiber and sintering aid are deposited on the surface of the filter screen, a wet blank is formed under the bonding action of the binder, and the wet blank is dried and sintered to obtain the special-shaped ceramic fiber rigid heat-insulating tile. When the wet blank is prepared, the filter screen is only required to be moved in and out of the storage tank, so that continuous preparation can be realized; the filter screen is moved by the assistance of an automatic device such as a mechanical arm, and automatic batch continuous preparation can be realized.
In the conventional wet forming process of the ceramic fiber rigid heat-insulating tile, suction filtration is carried out on the filter screen from the lower part of the filter screen Cheng Yiban, so that ceramic fiber slurry is deposited on the upper surface of the filter screen, and a wet blank is obtained. The process is only suitable for manufacturing a flat blank body, and when the blank body with the special-shaped surface rotating body is manufactured by using the process, because the ceramic fibers and the sintering auxiliary agent are deposited by gravity, more fibers and auxiliary agents are deposited at the bottom of the blank body, and the thickness and density distribution of the top and the bottom of the obtained wet blank are uneven, so that the finally manufactured special-shaped surface rigid heat-insulating tile is uneven in mechanical property and heat-insulating property distribution. In order to improve the distribution uniformity of ceramic fibers and sintering aids in the special-shaped surface blank, the invention strictly controls the consumption of each component in the ceramic fiber slurry and the slurry beating degree, and can avoid the gravity sedimentation of the ceramic fibers and the sintering aids in the slurry as much as possible in the range of the ratio and the beating degree, and meanwhile, the slurry has better fluidity, so that the ceramic fibers are oriented in the suction filtration process. In the suction filtration process, the suction filtration is carried out from the upper part of the filter screen through the connecting pipe at the top part of the filter screen, so that the uneven thickness of a green body caused by the gravity sedimentation of ceramic fibers and sintering aids in the suction filtration process can be overcome; meanwhile, the invention sets the pore size and the pore spacing of the filter pores on the surface of the filter screen according to the principle of hydrodynamics, the pore size of the filter pores is gradually reduced from top to bottom, the pore spacing is gradually increased, and when the filter screen structure and the suction filtration method are adopted for suction filtration, the arrangement direction of ceramic fibers deposited on the surface of the filter screen is consistent, and the orientation degree of the ceramic fibers in a green body is improved, so that the special-shaped surface ceramic fiber rigid heat insulation tile with uniform mechanical property and apparent heat conductivity coefficient is obtained, and the special-shaped surface ceramic fiber rigid heat insulation tile can be applied to a plurality of engineering scenes such as a hypersonic weapon radome heat insulation cap, a high-temperature muffle furnace lining, a crystal growth furnace lining and the like.
Preferably, the maximum aperture of the filter holes at the top of the filter screen is 3-5 mm, and the minimum aperture of the filter holes at the bottom of the filter screen is 0.5-1 mm; quartz fiber filter cloth is paved on the outer wall of the filter screen. The pore size distribution of the filter pores is in the range, which is more beneficial to the consistent orientation of the ceramic fibers on the surface of the filter screen. However, the sintering aid and the binder particles with the pore diameter in the range can be pumped out through the filter holes, so that the quartz fiber filter cloth is arranged outside the filter screen to intercept the sintering aid and the binder in the ceramic fiber slurry, thereby being beneficial to preparing the special-shaped ceramic fiber rigid heat-insulating tile with uniform density and excellent mechanical and heat conducting properties.
Preferably, the ceramic fiber in the S1 comprises quartz fiber and alumina fiber with the mass ratio of 1:0.2-0.3; the ceramic fiber has a length of 2-5 mm and a diameter of 1-3 μm. The ceramic fiber in the invention adopts the mixed fiber of quartz fiber and alumina fiber, so that the prepared rigid heat-insulating tile has high strength and high-temperature stability. And the length of the ceramic fiber is controlled to be 2-5 mm, so that the ceramic fiber can be uniformly distributed on the surface of the filter screen when the method is used for suction filtration.
Preferably, the sintering aid in S1 comprises boron nitride powder and silicon carbide powder in a mass ratio of 0.02-0.03:0.02; the binder is corn starch. According to the invention, the boron nitride powder and the silicon carbide powder are added as sintering aids, the boron nitride powder is beneficial to reducing the sintering temperature and improving the mechanical properties of the rigid heat-insulating tile; the silicon carbide powder can be used as a high-temperature radiation resistant agent to improve the high-temperature resistance and the high-temperature shrinkage resistance of the rigid heat insulation tile.
Preferably, compressed air is introduced into the storage tank through a membrane diffuser at the bottom of the storage tank in the S1, wherein the membrane diffuser is a hollow fiber microfiltration membrane component; and/or the ceramic fiber slurry is stirred in the storage tank through a stirring device. Compressed air is introduced into the bottom of the storage tank through the membrane diffuser, fine bubbles can be formed in the ceramic fiber slurry, gravity sedimentation of ceramic fibers and sintering aids in the slurry can be avoided under the action of the bubbles, and density uniformity of wet blanks is ensured. The slurry is stirred by the stirring device, so that the sedimentation of fibers and sintering aids in the slurry can be reduced, and the slurry is prevented from sedimentation and layering.
Preferably, the filter screen is in an inverted conical shape or a cylindrical shape.
Preferably, the connecting pipe is made of hard materials, a grabbing cover is arranged at the top of the connecting pipe, and a convex connecting port is arranged on the side wall of the connecting pipe. Adopt the connecting pipe that hard material was made to set up at the connecting pipe top and snatch the lid, can snatch the lid and remove the filter screen through snatching in the preparation process, the filter screen of being convenient for is followed the shift-in and is shifted out in the liquid storage pot. The connecting port on the connecting pipe can be connected with the vacuum pump through a flexible pipe.
Preferably, the positioning die surface used in S4 is provided with a placement groove matching the shape of the filter screen.
Preferably, in S5, after the filter screen in the positioning mold is removed from the wet blank, the wet blank is placed in an inner limiting device made of a quartz fiber needled felt to be dried. The wet blank is separated from the surface of the filter screen and then is placed in an inner limiting device for drying, and the inner limiting device can limit the volume expansion of the wet blank in the drying process.
Preferably, when the material is dried in the step S5, the material is firstly subjected to heat preservation at 100-140 ℃ for 1-5 hours, and then is subjected to heat preservation at 150-180 ℃ for 10-15 hours.
Preferably, during sintering in S5, firstly, heat is preserved for 0.5-2 hours at 400-600 ℃, then the temperature is raised to 1200-1400 ℃ for heat preservation for 1-5 hours, and then the temperature is naturally lowered to room temperature.
Therefore, the invention has the following beneficial effects:
(1) The method can continuously produce the ceramic fiber rigid heat-insulating tile component with the special-shaped surface of the simple rotating body, has simple process, uniform density of the prepared finished product and good high-temperature heat insulation effect, and can be applied to a plurality of engineering scenes such as hypersonic weapon radome heat-insulating caps, high-temperature muffle furnace linings, crystal growth furnace linings and the like.
(2) The method of suction filtration is changed, and the reverse suction filtration is carried out from the top of the filter screen, so that the uneven thickness of a green body caused by the gravity sedimentation of ceramic fibers and sintering aids in the suction filtration process can be overcome;
(3) According to the principle of fluid mechanics, the pore size of the filter holes on the surface of the filter screen and the interval between the filter holes are set, the pore size of the filter holes is gradually reduced from top to bottom, and the interval between the filter holes is gradually increased; the component proportion and the beating degree of the ceramic fiber slurry are limited, so that the arrangement direction of ceramic fibers deposited on the surface of the filter screen is consistent, the orientation degree of the ceramic fibers in the green body is improved, and the special-shaped surface ceramic fiber rigid heat-insulating tile with uniform mechanical property and apparent heat conductivity is obtained.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present invention;
FIG. 2 is a side expanded view of the screen of example 1 of the present invention;
FIG. 3 is a side expanded view of the screen of example 2 of the present invention;
FIG. 4 is an SEM image of a profiled ceramic fiber rigid heat insulating tile made in example 1 of the invention;
in fig. 1 to 3: the device comprises a filter screen 1, a filter hole 101, a connecting pipe 102, a grabbing cover 103, a connecting port 104, a mechanical arm 2, a storage tank 3, a positioning die 4, a ceramic fiber rigid heat insulation tile with a special-shaped surface 5, ceramic fiber slurry 6, a vacuum pump 7, a flexible pipe 8, a membrane diffuser 9 and a stirring device 10.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
In the present invention, all the equipment and raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
General examples:
a continuous wet method forming method of a special-shaped ceramic fiber rigid heat-insulating tile, the technological process of which is shown in figure 1, comprises the following steps:
s1: mixing ceramic fibers, a sintering aid and a binder in a mass ratio of 1-1.5:0.04-0.05:0.01-0.03, adding water, and pulping to obtain ceramic fiber slurry with a beating degree of 30-60 ︒ SR, wherein the ceramic fibers comprise quartz fibers and alumina fibers in a mass ratio of 1:0.2-0.3, and have a length of 2-5 mm and a diameter of 1-3 mu m; the sintering aid comprises boron nitride powder and silicon carbide powder in a mass ratio of 0.02-0.03:0.02; the binder is corn starch;
pumping ceramic fiber slurry into a storage tank 3, and introducing compressed air into the storage tank through a membrane diffuser 9 at the bottom of the storage tank, wherein the membrane diffuser is a hollow fiber microfiltration membrane component; and/or the ceramic fiber slurry is stirred in the storage tank through the stirring device 10;
s2: transferring the filter screen 1 into a storage tank 3 through a mechanical arm 2, so that the filter screen is immersed in ceramic fiber slurry 6; the top and the bottom of the filter screen are closed, the inside of the filter screen is hollow, the side surface is a required special-shaped surface and is provided with filter holes with gradually reduced pore diameters from top to bottom, and the interval between the filter holes is gradually increased from top to bottom; the maximum aperture of the filter holes at the top of the filter screen is 3-5 mm, and the minimum aperture of the filter holes at the bottom is 0.5-1 mm; quartz fiber filter cloth is paved on the outer wall of the filter screen; the top of the filter screen is provided with a connecting pipe 102 for communicating the inside of the filter screen with the vacuum pump, the connecting pipe is made of hard materials, the top of the connecting pipe is provided with a grabbing cover 103, and the side wall of the connecting pipe is provided with a convex connecting port 104;
s3: connecting a connecting port on the connecting pipe with a vacuum pump 7 through a flexible pipe 8, opening the vacuum pump to perform vacuum suction filtration, and obtaining a wet blank on the surface of a filter screen;
s4: transferring the filter screen from the storage tank to a positioning die 4 with a placing groove matched with the filter screen in shape on the surface through a mechanical arm, transferring the next set of filter screen into the storage tank, and repeating S1 to S4 to form continuous preparation;
s5: removing the filter screen in the positioning die from the wet blank, placing the wet blank in an inner limiting device made of quartz fiber needled felt, drying to obtain a dry blank, firstly preserving heat at 100-140 ℃ for 1-5 h, and then raising the temperature to 150-180 ℃ for 10-15 h;
s6: and (3) sintering the dry blank to obtain the special-shaped ceramic fiber rigid heat-insulating tile 5, wherein during sintering, the heat is preserved for 0.5-2 h at 400-600 ℃, then the temperature is raised to 1200-1400 ℃ for 1-5 h, and then the temperature is naturally lowered to room temperature.
Example 1:
a continuous wet method forming method of a conical cylindrical ceramic fiber rigid heat-insulating tile comprises the following steps:
s1: mixing quartz fiber, alumina fiber, boron nitride powder, silicon carbide powder, corn starch and water according to a mass ratio of 1:0.25:0.02:0.025:0.02:100, adding into a stirring barrel, and pulping to be uniform to obtain ceramic fiber slurry with a beating degree of 40 ︒ SR, wherein the length of the quartz fiber and the alumina fiber is 3mm, and the diameter of the quartz fiber and the alumina fiber is 1-3 mu m; pumping ceramic fiber slurry into a storage tank, and introducing compressed air into the storage tank through a membrane diffuser at the bottom of the storage tank, wherein the membrane diffuser is a hollow fiber microfiltration membrane component; stirring the ceramic fiber slurry by a stirring device;
s2: transferring the filter screen into a storage tank through a mechanical arm, so that the filter screen is immersed in the ceramic fiber slurry; the filter screen is in an inverted conical shape, the top and the bottom are closed, the inside is hollow, as shown in fig. 2, the side surface of the filter screen is provided with filter holes with gradually reduced pore diameters from top to bottom, the maximum pore diameter of the filter holes at the top is 5mm, the minimum pore diameter of the filter holes at the bottom is 1mm, and the interval between the filter holes is gradually increased from top to bottom; quartz fiber filter cloth is paved on the outer wall of the filter screen; a hard connecting pipe is arranged at the top of the filter screen, a grabbing cover is arranged at the top of the connecting pipe, and a convex connecting port is arranged on the side wall of the connecting pipe;
s3: connecting a connecting port on the connecting pipe with a vacuum pump through a flexible pipe, opening the vacuum pump to perform vacuum suction filtration, and obtaining a wet blank with the wall thickness of 20mm on the surface of a filter screen;
s4: transferring the filter screen from the storage tank to a placing groove on the surface of the positioning die through a mechanical arm, transferring the next set of filter screen into the storage tank, and repeating S1 to S4 to form continuous preparation;
s5: removing the filter screen in the positioning die from the wet blank, placing the wet blank in an inner limiting device made of quartz fiber needled felt, drying to obtain a dry blank, and firstly preserving heat for 2 hours at 120 ℃ and then preserving heat for 12 hours at 160 ℃ during drying;
s6: the dry blank is sintered to obtain the conical cylindrical ceramic fiber rigid heat-insulating tile, and when in sintering, the heat is preserved for 1h at 500 ℃, then the temperature is raised to 1300 ℃ for 2h, and then the temperature is naturally lowered to the room temperature; an SEM image of the resulting conical cylindrical ceramic fiber rigid insulating tile is shown in fig. 4.
Example 2:
example 2 differs from example 1 in that the filter screen used is cylindrical, the side expanded view of the filter screen is shown in fig. 3, the maximum pore diameter of the filter holes at the top is 5mm, the minimum pore diameter of the filter holes at the bottom is 1mm, the intervals of the filter holes are gradually increased from top to bottom, and finally the cylindrical ceramic fiber rigid heat insulation tile with the wall thickness of 20mm is manufactured; the remainder was the same as in example 1.
Examples 3 to 6 are different from example 1 in that the length of the quartz fiber and the alumina fiber in the ceramic fiber slurry, the degree of beating of the ceramic fiber slurry (only the water addition amount and beating parameters are changed, and the mass ratio of the ceramic fiber, sintering aid and binder is unchanged) and the process parameters during wet blank drying and sintering are changed, and the rest are the same as in example 1. The different process parameters of examples 3-6 and example 1 are shown in Table 1.
Table 1: process parameters employed in the various examples
Comparative example 1:
the conical cylindrical ceramic fiber rigid heat-insulating tile with the same shape as that in the embodiment 1 of the invention is prepared by adopting a suction filtration method in a patent CN 108252163A; the filter pore distribution on the filter screen, the component ratio of the ceramic fiber slurry, and the drying and sintering methods of the wet blank used in the preparation process are the same as those in example 1.
Comparative example 2:
comparative example 2 differs from example 1 in that the pore diameters of the filter screen used in comparative example 2 are 5mm, and the filter holes are uniformly distributed along the conical surface (the pitch is the same); the remaining steps and parameters were the same as in example 1.
Comparative example 3:
comparative example 3 is different from example 1 in that the ceramic fiber slurry has a tapping degree of 70 ︒ SR, and the remaining steps and parameters are the same as in example 1.
Comparative example 4:
comparative example 4 is different from example 1 in that the ceramic fiber slurry has a tapping degree of 20 ︒ SR, and the remaining steps and parameters are the same as in example 1.
The degree of fiber orientation (the tip of the conical rigid heat insulating tile is the bottom and the other end is the top) and apparent thermal conductivity of the different portions of the ceramic fiber rigid heat insulating tiles produced in the above examples and comparative examples were measured, and the results are shown in table 2.
The method for testing the apparent heat conductivity coefficient refers to GB/T10294-2008; test conditions: testing was performed at 1000 c under nitrogen atmosphere at 1 atmosphere.
Degree of fiber orientation α=σ xy /σ N ，σ xy In-plane tensile strength, sigma, of rigid insulating tile N The normal tensile strength of the rigid heat insulation tile; the larger the alpha value is, the higher the fiber orientation degree is, and the better the heat insulation performance of the special-shaped surface rigid heat insulation tile along the thickness direction is.
Table 2: special-shaped surface ceramic fiber rigid heat-insulating tile performance test result
As can be seen from FIG. 4, the ceramic fibers in the special-shaped rigid heat-insulating tile prepared by the method of the invention are uniformly distributed. As can be seen from the data in table 2, the special-shaped surface rigid heat insulation tiles prepared by the method in examples 1 to 6 have high fiber orientation degree, no difference in top and bottom fiber orientation degrees and low apparent heat conductivity; the method can lead the fibers to be distributed uniformly in the whole curved surface, and the arrangement direction of the fibers is favorable for obtaining good heat insulation effect.
In contrast, in comparative example 1, the ceramic fiber gravity sedimentation is adopted to cause uneven thickness of the blank, and the difference of fiber orientation degree between the top and the bottom of the manufactured rigid heat-insulating tile is large; when the method is adopted, the fiber arrangement direction is inconsistent, so that good heat insulation effect is not facilitated to be obtained, the fiber orientation degree is obviously reduced compared with that in the embodiment 1, and the apparent heat conductivity coefficient of the rigid heat insulation tile is obviously improved.
In comparative example 2, the filter screen with uniform filter hole size and distribution is adopted for suction filtration, the uniformity of the thickness of the blank body is reduced, the uniform orientation of the fibers is not facilitated, and the apparent heat conductivity coefficient of the rigid heat insulation tile is obviously improved compared with that of the embodiment.
The ceramic fiber slurry in comparative example 3 has too high beating degree, the ceramic fiber slurry in comparative example 4 has too low beating degree, and the ceramic fiber slurry is not beneficial to the uniform orientation of fibers beyond the scope of the invention, and the apparent heat conductivity coefficient of the rigid heat insulation tile performance is improved compared with that of the embodiment, so that the apparent heat conductivity coefficient of the rigid heat insulation tile performance is improved, and the apparent influence of the beating degree of the slurry on the arrangement of the fibers is demonstrated.
Claims (10)
1. A continuous wet method forming method of a special-shaped ceramic fiber rigid heat-insulating tile is characterized by comprising the following steps:
s1: mixing ceramic fibers, a sintering aid and a binder in a mass ratio of 1-1.5:0.04-0.05:0.01-0.03, adding water, pulping to obtain ceramic fiber slurry with a beating degree of 30-60 ︒ SR, and pumping the ceramic fiber slurry into a storage tank;
s2: transferring the filter screen into a storage tank to enable the filter screen to be immersed in the ceramic fiber slurry; the top and the bottom of the filter screen are closed, the inside of the filter screen is hollow, the side surface is a required special-shaped surface and is provided with filter holes with gradually reduced pore diameters from top to bottom, the pore diameter of the filter hole at the top of the filter screen is 3-5 mm, and the interval between the filter holes is gradually increased from top to bottom; the top of the filter screen is provided with a connecting pipe for communicating the inside of the filter screen with the vacuum pump; quartz fiber filter cloth is paved on the outer wall of the filter screen;
s3: connecting the connecting pipe with a vacuum pump, performing vacuum suction filtration, and obtaining a wet blank on the surface of the filter screen;
s4: transferring the filter screen from the storage tank to a positioning die, transferring the next set of filter screen into the storage tank, and repeating S1 to S4 to form continuous preparation;
s5: and (3) taking the filter screen in the positioning die out of the wet blank, drying the wet blank, and sintering to obtain the special-shaped ceramic fiber rigid heat-insulating tile.
2. The continuous wet molding method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1, wherein the aperture of the filter holes at the bottom of the filter screen is 0.5-1 mm.
3. The continuous wet method forming method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1 or 2, wherein the ceramic fibers in the S1 comprise quartz fibers and alumina fibers in a mass ratio of 1:0.2-0.3; the length of the ceramic fiber is 2-5 mm, and the diameter is 1-3 mu m; the sintering aid comprises boron nitride powder and silicon carbide powder in a mass ratio of 0.02-0.03:0.02; the binder is corn starch.
4. The continuous wet method forming method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1, wherein the bottom of the storage tank in the step S1 is filled with compressed air through a membrane diffuser, and the membrane diffuser is a hollow fiber micro-filtration membrane component; and/or the ceramic fiber slurry is stirred in the storage tank through a stirring device.
5. The continuous wet process for forming ceramic fiber rigid heat insulating tiles with special-shaped surfaces according to claim 1 or 2, wherein the filter screen is in an inverted conical shape or a cylindrical shape.
6. The continuous wet process for forming ceramic fiber rigid heat-insulating tiles with special-shaped surfaces according to claim 1 or 2, wherein the connecting pipe is made of hard materials, the top of the connecting pipe is provided with a grabbing cover, and the side wall of the connecting pipe is provided with a convex connecting port.
7. The continuous wet molding method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1, wherein the surface of the positioning mold used in the step S4 is provided with a placing groove matched with the shape of the filter screen.
8. The continuous wet molding method of profiled ceramic fiber rigid heat-insulating tiles according to claim 1, wherein in S5, after the filter screen in the positioning mold is removed from the wet blank, the wet blank is placed in an inner limiting device made of a quartz fiber needled felt for drying.
9. The continuous wet molding method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1 or 8, wherein when the tile is dried in the step S5, the tile is firstly subjected to heat preservation at 100-140 ℃ for 1-5 hours, and then is subjected to heat preservation at 150-180 ℃ for 10-15 hours.
10. The continuous wet molding method of the special-shaped ceramic fiber rigid heat-insulating tile according to claim 1, wherein during sintering in S5, heat preservation is carried out at 400-600 ℃ for 0.5-2 h, then the temperature is raised to 1200-1400 ℃ for 1-5 h, and then natural cooling is carried out to room temperature.
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