CN113135768B - Preparation method of hollow porous SiC fibers - Google Patents
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
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- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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Abstract
The invention discloses a preparation method of hollow porous SiC fibers, which comprises the following steps: firstly, preparing impregnation liquid by utilizing camphene and polycarbosilane powder; mixing the carbon fiber with the impregnation liquid, performing ultrasonic treatment, and drying to obtain a green body sample; placing the green body sample in a crucible, drying, performing crosslinking curing, then placing the sample in a vacuum tube furnace, and performing pyrolysis to obtain a prefabricated body; and finally, placing the prefabricated body in a box type furnace, and performing decarburization heat treatment to obtain the hollow porous SiC fiber. The hollow porous SiC fiber is obtained by using carbon fiber as a raw material to dip a precursor solution and combining a polymer conversion ceramic process. On the premise of ensuring the porous functionality, a simpler preparation method is provided, the specific surface area of the porous polymer converted SiC ceramic fiber is increased, and the porous polymer converted SiC ceramic fiber has a wide application prospect in the field of thermal insulation materials.
Description
Technical Field
The invention belongs to the technical field of fiber material preparation, and particularly relates to a preparation method of a hollow porous SiC fiber.
Background
The hollow silicon carbide fiber has the characteristics of light weight, larger specific surface area, adsorption, filtration, wave absorption and the like due to the special cavity structure, and has good advantages and application prospects in the applications of heat insulation, gas-sensitive materials, corrosive fluid filtration, high-temperature gas separation, microreactors, catalyst carriers, solid oxide fuel cells, electromagnetic shielding and the like. For example, hollow or tubular fibers are used in gas-sensitive materials to facilitate the adsorption and diffusion of gases in the fibers, the target gas diffuses both towards the outer surface of the fibers and into the fiber tubes, and the gas adsorbed on the outer surface of the fibers and into the tubes diffuses both towards the interior of the fibers from both sides. The diffusion time of the gas in the fiber is shortened as much as possible, and the gas is rapidly contacted and reacted with all effective active sites in the fiber, so that the sensitivity is improved, and meanwhile, the response time to the target gas is shortened.
Currently, the following methods are generally used for preparing the hollow SiC fiber: (1) spinneret spinning; (2) electron beam irradiation cross-linking method; (3) template method; (4) electrostatic spinning; (4) a phase inversion method; (5) vapor deposition method. Since 2002, the coaxial electrostatic spinning technology is reported to be widely researched and applied in the field of hollow nano-fiber preparation, and is the most common method for preparing hollow nano-fiber at present, and the coaxial electrostatic spinning technology has higher requirements on spinning nozzles, nuclear layer solution and spinning process parameters, long-time exploration on spinning conditions is required, and the difficulty in preparing hollow nano-SiC fiber is increased. Therefore, the research of a new method for preparing the hollow SiC fiber has wide development prospect.
Disclosure of Invention
The invention aims to provide a preparation method of hollow porous SiC fibers, which solves the problems of complex preparation process and harsh preparation conditions of SiC fibers in the prior art.
The technical scheme adopted by the invention is that the preparation method of the hollow porous SiC fiber is implemented according to the following steps:
step 1, preparing impregnation liquid by utilizing camphene and polycarbosilane powder;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
step 3, placing the green body sample in an alumina crucible, and then placing the alumina crucible in an electrothermal blowing dry box for crosslinking and curing to obtain a crosslinked and cured sample;
step 4, placing the prepared cross-linked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a preform;
and 5, placing the prefabricated body in a box type furnace, and performing decarburization heat treatment to obtain the hollow porous SiC fiber.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps: heating and stirring camphene crystallized at room temperature in water bath at 40-80 deg.C to convert camphene into liquid, adding polycarbosilane powder, and stirring at 40-80 deg.C for 2-6h to obtain impregnation liquid;
the mass ratio of camphene to polycarbosilane powder is 1: 0.1-0.2.
In the step 2, the ultrasonic treatment temperature is 60-80 ℃, and the ultrasonic treatment time is 1-3 h; the drying temperature is 60-80 ℃.
In the step 2, the diameter of the carbon fiber is 1-5 μm, and the length is 3-6 mm; the mass ratio of the carbon fibers to the impregnation liquid is 1: 2.
in the step 3, the crosslinking curing temperature is 180-.
In the step 4, the pyrolysis temperature is 1000-.
In step 5, the heat treatment temperature is 300-.
The invention has the beneficial effect that the hollow porous SiC fiber is obtained by taking the carbon fiber as the raw material and combining the precursor solution with the polymer conversion ceramic process. On the premise of ensuring the porous functionality, a simpler and more convenient preparation method is provided, the specific surface area of the porous polymer converted SiC ceramic fiber is improved, and the preparation method has a wide application prospect in the field of thermal insulation materials.
Drawings
FIG. 1 is a first topographical view of a hollow porous SiC fiber prepared in example 1 of the present invention;
fig. 2 is a morphology diagram (ii) of a hollow porous SiC fiber prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a hollow porous SiC fiber, which is implemented according to the following steps:
step 1, preparing a steeping fluid: heating and stirring camphene crystallized at room temperature in water bath at 40-80 deg.C to convert camphene into liquid, adding polycarbosilane powder, and stirring at 40-80 deg.C for 2-6h to obtain impregnation liquid;
the mass ratio of camphene to polycarbosilane powder is 1: 0.1-0.2;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
the mass ratio of the carbon fibers to the impregnating solution is 1: 2;
the ultrasonic treatment temperature is 60-80 ℃, and the ultrasonic treatment time is 1-3 h; the drying temperature is 60-80 ℃;
the diameter of the carbon fiber is 1-5 μm, and the length is 3-6 mm;
step 3, placing the green body sample in an alumina crucible, placing the alumina crucible in an electric heating forced air drying oven, and crosslinking for 1-2h at the temperature of 180-200 ℃ to obtain a crosslinked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
the pyrolysis temperature is 1000-1600 ℃, and the pyrolysis time is 1-2 h;
and 5, placing the prefabricated body in a box type furnace, and performing decarburization heat treatment for 1-2h at the temperature of 300-500 ℃ to obtain the hollow porous SiC fiber.
Example 1
The invention relates to a preparation method of a hollow porous SiC fiber, which is implemented according to the following steps:
step 1, preparing a steeping fluid: heating and stirring camphene crystallized at room temperature in water bath at 60 deg.C to convert camphene into liquid, adding polycarbosilane powder, and stirring at 60 deg.C for 3 hr to obtain impregnation liquid;
the mass ratio of camphene to polycarbosilane powder is 1: 0.1;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
the mass ratio of the carbon fibers to the impregnation liquid is 1: 2;
the ultrasonic treatment temperature is 60 ℃, and the ultrasonic treatment time is 1 h; the drying temperature is 60 ℃;
the diameter of the carbon fiber is 3 μm, and the length is 3 mm;
step 3, placing the green body sample in an alumina crucible, placing the alumina crucible in an electrothermal blowing dry box, and crosslinking for 2 hours at 190 ℃ to obtain a crosslinked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
the pyrolysis temperature is 1600 ℃, and the pyrolysis time is 2 hours;
and 5, placing the preform in a box furnace, and performing decarburization heat treatment for 1 hour at the temperature of 400 ℃ to obtain the hollow porous SiC fiber.
The topography of the hollow porous SiC fiber prepared in this example is shown in fig. 1 and 2, from which it is apparent that the interior of the fiber is hollow and the surface of the fiber is densely packed. The hollow porous SiC fiber is successfully obtained by utilizing the preparation method provided by the invention.
Example 2
The invention relates to a preparation method of a hollow porous SiC fiber, which is implemented according to the following steps:
step 1, preparing a steeping fluid: heating and stirring camphene crystallized at room temperature in water bath at 80 ℃ to convert camphene into liquid, adding polycarbosilane powder, and continuously stirring for 3h at 80 ℃ to obtain a soaking solution;
the mass ratio of camphene to polycarbosilane powder is 1: 0.2;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
the mass ratio of the carbon fibers to the impregnating solution is 1: 2;
the ultrasonic treatment temperature is 80 ℃, and the ultrasonic treatment time is 3 hours; the drying temperature is 80 ℃;
the diameter of the carbon fiber is 5 μm, and the length is 6 mm;
step 3, placing the green body sample in an alumina crucible, placing the alumina crucible in an electrothermal blowing dry box, and crosslinking for 2 hours at 200 ℃ to obtain a crosslinked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
the pyrolysis temperature is 1600 ℃, and the pyrolysis time is 2 hours;
and 5, placing the preform in a box type furnace, and performing decarburization heat treatment for 2 hours at the temperature of 500 ℃ to obtain the hollow porous SiC fiber.
Example 3
The invention relates to a preparation method of a hollow porous SiC fiber, which is implemented according to the following steps:
step 1, preparing a steeping fluid: heating and stirring camphene crystallized at room temperature in water bath at 40 deg.C to convert camphene into liquid, adding polycarbosilane powder, and stirring at 40 deg.C for 2 hr to obtain impregnation liquid;
the mass ratio of camphene to polycarbosilane powder is 1: 0.1;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
the mass ratio of the carbon fibers to the impregnating solution is 1: 2;
the ultrasonic treatment temperature is 70 ℃, and the ultrasonic treatment time is 1.5 h; the drying temperature is 60 ℃;
the diameter of the carbon fiber is 1 μm, and the length is 6 mm;
step 3, placing the green body sample in an alumina crucible, placing the alumina crucible in an electrothermal blowing dry box, and crosslinking for 2 hours at 180 ℃ to obtain a crosslinked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
the pyrolysis temperature is 1000 ℃, and the pyrolysis time is 2 hours;
and 5, placing the prefabricated body in a box furnace, and performing decarburization heat treatment for 1h at the temperature of 450 ℃ to obtain the hollow porous SiC fiber.
Example 4
The invention relates to a preparation method of a hollow porous SiC fiber, which is implemented according to the following steps:
step 1, preparing a steeping fluid: heating and stirring camphene crystallized at room temperature in water bath at 50 ℃ to convert camphene into liquid, adding polycarbosilane powder, and continuously stirring at 50 ℃ for 4 hours to obtain impregnation liquid;
the mass ratio of camphene to polycarbosilane powder is 1: 0.2;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, then taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried;
the mass ratio of the carbon fibers to the impregnating solution is 1: 2;
the ultrasonic treatment temperature is 60 ℃, and the ultrasonic treatment time is 1 h; the drying temperature is 60 ℃;
the diameter of the carbon fiber is 4 μm, and the length is 3 mm;
step 3, placing the green body sample in an alumina crucible, placing the alumina crucible in an electrothermal blowing dry box, and crosslinking for 1h at 190 ℃ to obtain a crosslinked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
the pyrolysis temperature is 1200 ℃, and the pyrolysis time is 1.5 h;
and 5, placing the preform in a box furnace, and performing decarburization heat treatment for 1.5 hours at 350 ℃ to obtain the hollow porous SiC fiber.
Claims (4)
1. A preparation method of hollow porous SiC fibers is characterized by comprising the following steps:
step 1, preparing impregnation liquid by utilizing camphene and polycarbosilane powder; the method comprises the following specific steps: heating and stirring camphene crystallized at room temperature in water bath at 40-80 deg.C to convert camphene into liquid, adding polycarbosilane powder, and stirring at 40-80 deg.C for 2-6h to obtain impregnation liquid; the mass ratio of camphene to polycarbosilane powder is 1: 0.1-0.2;
step 2, mixing the carbon fibers with the impregnation liquid, carrying out ultrasonic treatment, then taking the carbon fibers out of the impregnation liquid, placing the carbon fibers in a culture dish, placing the culture dish in an oven for drying, and obtaining a green body sample after the surface liquid is dried; the diameter of the carbon fiber is 1-5 μm, and the length is 3-6 mm; the mass ratio of the carbon fibers to the impregnating solution is 1: 2;
step 3, placing the green body sample in an alumina crucible, and then placing the alumina crucible in an electrothermal blowing dry box for cross-linking and curing to obtain a cross-linked and cured sample;
step 4, putting the prepared crosslinked and cured sample in a vacuum tube furnace, and pyrolyzing the sample under the protection of Ar gas to obtain a prefabricated body;
step 5, placing the prefabricated body in a box type furnace, and performing decarburization heat treatment to obtain hollow porous SiC fibers;
the heat treatment temperature is 300-500 ℃, and the heat treatment time is 1-2 h.
2. The method for preparing the hollow porous SiC fiber according to claim 1, wherein in the step 2, the ultrasonic treatment temperature is 60-80 ℃, and the ultrasonic treatment time is 1-3 h; the drying temperature is 60-80 ℃.
3. The method as claimed in claim 1, wherein the cross-linking curing temperature in step 3 is 180-200 ℃ and the time is 1-2 h.
4. The method for preparing hollow porous SiC fiber according to claim 1, wherein in the step 4, the pyrolysis temperature is 1000-1600 ℃, and the pyrolysis time is 1-2 h.
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| JP2523147B2 (en) * | 1987-12-08 | 1996-08-07 | 帝人株式会社 | Method for producing inorganic fiber |
| JP3613486B2 (en) * | 1995-02-23 | 2005-01-26 | 大倉工業株式会社 | Method for manufacturing silicon carbide whisker |
| CN100506703C (en) * | 2007-04-18 | 2009-07-01 | 大连理工大学 | Method of preparing titanium dioxide, tin dioxide and doping composite fiber material thereof |
| US7910082B2 (en) * | 2008-08-13 | 2011-03-22 | Corning Incorporated | Synthesis of ordered mesoporous carbon-silicon nanocomposites |
| CN104532549B (en) * | 2014-12-10 | 2016-08-31 | 张家港市东大工业技术研究院 | A kind of method based on Microwave Induced Plasma quick obtaining carbon/coaxial fiber of carborundum and application |
| CN108456949B (en) * | 2018-01-23 | 2020-11-10 | 中国科学院宁波材料技术与工程研究所 | Hollow silicon carbide ceramic fiber and preparation method thereof |
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