CN112537964A - Preparation method of silicon carbide aerogel - Google Patents

Preparation method of silicon carbide aerogel Download PDF

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CN112537964A
CN112537964A CN201910898466.0A CN201910898466A CN112537964A CN 112537964 A CN112537964 A CN 112537964A CN 201910898466 A CN201910898466 A CN 201910898466A CN 112537964 A CN112537964 A CN 112537964A
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silicon carbide
aerogel
ceramic precursor
carbide ceramic
precursor
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贺丽娟
赵佳明
张恩爽
黄红岩
孔德隆
刘圆圆
张凡
李文静
杨洁颖
赵英民
张昊
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Aerospace Research Institute of Materials and Processing Technology
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract

The invention provides a preparation method of silicon carbide aerogel, which comprises the following steps: mixing polycarbosilane with an organic solvent to prepare a uniformly dispersed silicon carbide ceramic precursor solution; heating the silicon carbide ceramic precursor solution in an inert atmosphere, optionally adding a platinum catalyst, and carrying out a hydrosilylation reaction to obtain a silicon carbide ceramic precursor gel; drying the silicon carbide ceramic precursor gel to obtain a silicon carbide ceramic precursor aerogel; and heating the silicon carbide ceramic precursor aerogel to perform pyrolysis under an inert atmosphere to obtain the silicon carbide aerogel. The method combines a precursor conversion method and an aerogel method, has simple raw material source, does not need to be matched with vinyl substances for use, has simple precursor synthesis, mild precursor gel preparation conditions, high yield of the obtained silicon carbide aerogel ceramic and adjustable C/Si ratio which is close to the stoichiometric ratio.

Description

Preparation method of silicon carbide aerogel
Technical Field
The invention belongs to the field of aerogel, and particularly relates to a preparation method of silicon carbide aerogel.
Background
The aerogel is a nano porous material with a continuous three-dimensional network structure, has the characteristics of low density, high specific surface area, high porosity, low thermal conductivity and the like due to the unique structure, and can be widely applied to the fields of aerospace detection, environmental protection, high-efficiency catalysis, super capacitors, wave-absorbing materials and the like.
Silicon carbide aerogels have attracted considerable attention due to their excellent high temperature oxidation resistance and chemical stability. Chinese patent CN103864076A uses SiO2The aerogel is used as a template, and discloses a preparation method of silicon carbide aerogel. The Chinese patent CN105600785B and CN105601316B both adopt polycarbosilane, divinyl substance and solvent as starting materials, and the starting materials are subjected to a crosslinking reaction under the action of a curing agent to form silicon carbide gel, and the silicon carbide aerogel is obtained through the steps of drying treatment, high-temperature cracking and the like. The silicon carbide aerogel prepared by the methods has more raw material types and complicated preparation process; divinyl substance is easy to self-cross under catalytic heating conditionJointly influence the aerogel structure, also can cause the aerogel rich carbon, influence its performance. Chinese patent CN107324339A discloses a silicon carbide aerogel and its preparation method, which is prepared by selecting a material containing Si-H and Si-CH ═ CH2The precursor solution is subjected to hydrosilylation reaction to obtain precursor gel, and then the precursor gel is subjected to high-temperature heat treatment to obtain the silicon carbide aerogel. The precursor adopted by the method is difficult to synthesize, the preparation temperature of the precursor gel is higher, and the yield of the prepared ceramic aerogel ceramic is lower.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of silicon carbide aerogel. The method combines a precursor conversion method and an aerogel method, the raw material source is simple, the method does not need to be matched with vinyl substances for use, the precursor synthesis is simple, the preparation condition of the precursor gel is mild, the yield of the obtained silicon carbide aerogel ceramic is high, and the C/Si ratio is adjustable and is close to the stoichiometric ratio.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of silicon carbide aerogel comprises the following steps:
(1) firstly, mixing polycarbosilane with an organic solvent to prepare a uniformly dispersed silicon carbide ceramic precursor solution;
(2) heating the silicon carbide ceramic precursor solution in an inert atmosphere, optionally adding a platinum catalyst, and carrying out a hydrosilylation reaction to obtain a silicon carbide ceramic precursor gel;
(3) drying the silicon carbide ceramic precursor gel to obtain a silicon carbide ceramic precursor aerogel;
(4) and heating the silicon carbide ceramic precursor aerogel to perform pyrolysis under an inert atmosphere to obtain the silicon carbide aerogel.
Preferably, the polycarbosilane of step (1) has the following structural formula:
Figure BDA0002211047050000021
wherein n and m are natural numbers larger than 1, and n/m is 0.01-0.5.
Preferably, the organic solvent in step (1) includes n-hexane, tetrahydrofuran, dichloromethane or chloroform.
Preferably, the concentration of the silicon carbide ceramic precursor solution in the step (1) is 10 wt% -30 wt%.
Preferably, the condition of the silicon hydride addition reaction of the silicon carbide ceramic precursor in the step (2) is that the heating temperature is 100-300 ℃ under the condition of inert atmosphere; or under the condition of adding a platinum catalyst, the heating temperature is 120-180 ℃ in an inert atmosphere.
Preferably, the platinum catalyst added in step (2) is Karstedt's catalyst.
Preferably, the amount of platinum catalyst added in step (2) is from 0.1 wt% to 0.8 wt% of the polycarbosilane
Preferably, the silicon carbide ceramic precursor polycarbosilane hydrosilylation reaction time in the step (2) is 2-10 h.
Preferably, the drying method of the silicon carbide ceramic precursor gel in the step (3) is supercritical drying or freeze drying.
Preferably, the pyrolysis condition of the silicon carbide ceramic precursor aerogel in the step (4) is that the pyrolysis temperature in an inert atmosphere is 800-1600 ℃.
Preferably, the pyrolysis time of the silicon carbide ceramic precursor aerogel in the step (4) is 2-6 h.
Preferably, the temperature increase rate in step (4) is 1 to 5 ℃/min.
The silicon carbide aerogel prepared by the method has the density of 0.143-0.476g/cm3Specific surface area of 120-780m2(ii)/g, the average pore diameter is 10-36 nm.
Compared with the prior art, the beneficial technical effects of the invention are as follows:
1. the invention utilizes a polymer precursor conversion technology to prepare the ceramic aerogel by combining with an aerogel technology.
2. The invention utilizes the liquid polycarbosilane containing both Si-H and Si-CH ≡ CH structures as the silicon carbide ceramic precursor, and the silicon carbide ceramic precursor can be cured by hydrosilylation reaction under certain conditions, so that the reaction conditions are mild, the silicon carbide ceramic precursor is not required to be matched with vinyl substances, the raw material source is simple, and the preparation cost is reduced.
3. The polymer precursor adopted in the invention has strong designability and simple synthesis, the obtained silicon carbide aerogel ceramic has high yield, and the C/Si ratio is adjustable and is close to the stoichiometric ratio.
Drawings
FIG. 1 is an SEM image of a silicon carbide aerogel prepared according to example 1 of the present invention.
FIG. 2 is an XRD spectrum of a silicon carbide aerogel prepared according to example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be noted that the purpose of the examples is to more clearly illustrate the practical application process of the present invention, and not to limit the protection scope of the present invention.
The first embodiment is as follows:
under the protection of nitrogen, 30g of precursor polymer is weighed, dissolved in 70g of dichloromethane and stirred uniformly to obtain a precursor solution with the concentration of 30 wt%; adding 5 mu L of 0.8 wt% Karstedt catalyst, stirring uniformly under the protection of nitrogen, transferring to a pressure reaction kettle filled with nitrogen, and reacting at 120 ℃ for 2h to obtain light yellow silicon carbide precursor wet gel; taking out, soaking in dichloromethane for 2 days, and replacing dichloromethane for 3 times; passing the wet gel through supercritical CO2Drying for 3 times, each time for 3 days, to obtain silicon carbide precursor aerogel; and (3) placing the aerogel in a high-temperature tube furnace, heating to 1600 ℃ at the speed of 1 ℃/min under high-purity argon, and preserving heat for 3h to obtain the silicon carbide aerogel. The density of the obtained silicon carbide aerogel is 0.329g/cm3A specific surface area of 316m2G, average pore diameter of 27 nm.
Example two:
under the protection of nitrogen, 23g of precursor polymer is weighed and dissolved in 77g of n-hexane, and the mixture is stirred uniformly to obtain a precursor solution with the concentration of 23 wt%; under the protection of nitrogen, the nitrogen gas is used for protecting the reaction vessel,after being uniformly stirred, the mixture is transferred to a pressure reaction kettle filled with nitrogen, and the mixture reacts for 10 hours at 265 ℃ to obtain faint yellow silicon carbide precursor wet gel; taking out, soaking in n-hexane for 2 days, and replacing n-hexane for 3 times; freezing and drying the wet gel to obtain silicon carbide precursor aerogel; and (3) placing the aerogel in a high-temperature tube furnace, heating to 1200 ℃ at the speed of 3 ℃/min under high-purity argon, and preserving heat for 4h to obtain the silicon carbide aerogel. The obtained silicon carbide aerogel has a density of 0.182g/cm3Specific surface area of 692m2In g, the mean pore diameter is 14 nm.
Example three:
under the protection of nitrogen, 10g of precursor polymer is weighed and dissolved in 90g of chloroform, and the mixture is stirred uniformly to obtain a precursor solution with the concentration of 30 wt%; adding 5 mu L of 0.1 wt% Karstedt catalyst, stirring uniformly under the protection of nitrogen, transferring to a pressure reaction kettle filled with nitrogen, and reacting at 180 ℃ for 10h to obtain light yellow silicon carbide precursor wet gel; taking out, soaking in chloroform for 2 days, and replacing chloroform for 3 times; passing the wet gel through supercritical CO2Drying for 3 times, each time for 3 days, to obtain silicon carbide precursor aerogel; placing the aerogel in a high-temperature tube furnace, heating to 1300 ℃ at the speed of 5 ℃/min under high-purity argon, and preserving heat for 6 hours to obtain the silicon carbide aerogel. The obtained silicon carbide aerogel has the density of 0.267g/cm3A specific surface area of 533m2(ii)/g, average pore diameter 23 nm.
Example four:
under the protection of nitrogen, 15g of precursor polymer is weighed and dissolved in 85g of tetrahydrofuran, and the mixture is stirred uniformly to obtain a precursor solution with the concentration of 10 wt%; adding 2 mu L of 0.31 wt% Karstedt catalyst, stirring uniformly under the protection of nitrogen, transferring to a pressure reaction kettle filled with nitrogen, and reacting at 150 ℃ for 6h to obtain light yellow silicon carbide precursor wet gel; taking out, soaking in tetrahydrofuran for 2 days, and replacing tetrahydrofuran for 3 times; passing the wet gel through supercritical CO2Drying for 3 times, each time for 3 days, to obtain silicon carbide precursor aerogel; placing the aerogel in a high temperature tube furnaceAnd heating to 1400 ℃ at the speed of 3 ℃/min under high-purity argon, and preserving the heat for 2 hours to obtain the silicon carbide aerogel. The obtained silicon carbide aerogel has a density of 0.255g/cm3Specific surface area of 628m2In terms of/g, the mean pore diameter is 19 nm.
Example five:
under the protection of nitrogen, weighing 20g of precursor polymer, dissolving the precursor polymer in 80g of n-hexane, and stirring uniformly to obtain a precursor solution with the concentration of 20 wt%; under the protection of nitrogen, stirring uniformly, transferring the mixture into a pressure reaction kettle filled with nitrogen, and reacting at 300 ℃ for 3 hours to obtain light yellow silicon carbide precursor wet gel; taking out, soaking in n-hexane for 2 days, and replacing n-hexane for 3 times; passing the wet gel through supercritical CO2Drying for 3 times, each time for 3 days, to obtain silicon carbide precursor aerogel; placing the aerogel in a high-temperature tube furnace, heating to 1500 ℃ at the speed of 1 ℃/min under high-purity argon, and preserving heat for 5 hours to obtain the silicon carbide aerogel. The density of the obtained silicon carbide aerogel is 0.143g/cm3780m in specific surface area2(ii)/g, average pore diameter of 10nm, C/Si ratio of 1.27, and yield of silicon carbide ceramic of 69%.
Example six:
under the protection of nitrogen, 25g of precursor polymer is weighed and dissolved in 75g of tetrahydrofuran, and the mixture is stirred uniformly to obtain a precursor solution with the concentration of 25 wt%; under the protection of nitrogen, stirring uniformly, transferring the mixture into a pressure reaction kettle filled with nitrogen, and reacting for 5 hours at 100 ℃ to obtain light yellow silicon carbide precursor wet gel; taking out, soaking in tetrahydrofuran for 2 days, and replacing tetrahydrofuran for 3 times; passing the wet gel through supercritical CO2Drying for 3 times, each time for 3 days, to obtain silicon carbide precursor aerogel; placing the aerogel in a high-temperature tube furnace, heating to 800 ℃ at the speed of 5 ℃/min under high-purity argon, and preserving heat for 4h to obtain the silicon carbide aerogel. The resulting silicon carbide aerogel had a density of 0.476g/cm3Specific surface area of 127m2In g, the mean pore diameter is 36 nm.
Comparative example:
this comparative example prepared a silicon carbide aerogel using the method described in patent CN107324339A, in comparison to example five, as follows:
and dissolving 5g of silicon carbide precursor mucus in 20g of n-hexane, preparing a silicon carbide precursor solution with the concentration of 20 wt%, and uniformly stirring. Wherein R in the silicon carbide precursor is Al, and m/n is 20. And reacting the silicon carbide precursor solution in a pressure reaction kettle at 330 ℃ for 3h under the protection of nitrogen to obtain the light yellow silicon carbide precursor gel. Using liquid CO for the obtained silicon carbide precursor gel2And replacing for 2 days, and performing supercritical drying (60 ℃, 20m & Pa, 3 days) to obtain the silicon carbide precursor aerogel. And (3) placing the obtained silicon carbide precursor aerogel in a tubular furnace, heating to 800 ℃ at the speed of 2 ℃/min under the condition of nitrogen, preserving heat for 5h, naturally cooling, transferring to a muffle furnace, heating to 550 ℃ in air, preserving heat for 1.5h, and naturally cooling. The density of the obtained silicon carbide aerogel is 0.572g/cm3The specific surface area is 310m2G, average pore diameter of 14nm, C/Si ratio of 1.39, and yield of silicon carbide ceramic of 50%.
As can be seen from a comparison of the results of example 5 and comparative example, the yield of the ceramic obtained by the method of the present invention is higher than that obtained by the method disclosed in the published patent CN 107324339A. The reason is that the invention adopts precursor materials and preparation conditions different from those of the published patent CN107324339A, the difficulty in synthesizing the precursor vinyl polycarbosilane adopted in CN107324339A is high, and the synthesis of the precursor polycarbosilane is simple and easy to control; the method has the advantages of mild conditions for forming precursor gel, high ceramic yield (69%, which is far higher than 53% of ceramic yield of CN 107324339A), and capability of regulating and controlling the C/Si in the ceramization product by adjusting the feeding ratio of the main monomers to be close to the stoichiometric ratio (1.15, which is lower than 1.24% of the C/Si ratio of the ceramization product obtained by the vinyl polycarbosilane in CN 107324339A). Therefore, the method has the advantages that the preparation conditions of the precursor gel are mild, the yield of the silicon carbide aerogel ceramic is high, and the C/Si ratio is lower.

Claims (10)

1. The preparation method of the silicon carbide aerogel is characterized by comprising the following steps of:
mixing polycarbosilane with an organic solvent to prepare a uniformly dispersed silicon carbide ceramic precursor solution;
the structural formula of the polycarbosilane is as follows:
Figure FDA0002211047040000011
wherein n and m are natural numbers larger than 1, and n/m is 0.01-0.5;
the silicon carbide ceramic precursor solution is subjected to hydrosilylation reaction at the temperature of 100-plus-300 ℃ in an inert atmosphere, or the silicon carbide ceramic precursor solution is added with a platinum catalyst in the inert atmosphere and subjected to hydrosilylation reaction at the temperature of 120-plus-180 ℃ to obtain silicon carbide ceramic precursor gel;
drying the silicon carbide ceramic precursor gel to obtain a silicon carbide ceramic precursor aerogel;
and heating the silicon carbide ceramic precursor aerogel to 800-1600 ℃ in an inert atmosphere for pyrolysis to obtain the silicon carbide aerogel.
2. The method of claim 1, wherein the organic solvent comprises n-hexane, tetrahydrofuran, dichloromethane, or chloroform.
3. The method of claim 1, wherein the silicon carbide ceramic precursor solution has a concentration of 10 wt% to 30 wt%.
4. The method of claim 1, wherein the platinum catalyst is a Karstedt catalyst.
5. The method of claim 1 or 4, wherein the amount of platinum catalyst added is from 0.1 wt% to 0.8 wt% of the polycarbosilane.
6. The method of claim 1, wherein the silicon carbide ceramic precursor polycarbosilane hydrosilylation reaction time is from 2 to 10 hours.
7. The method of claim 1, wherein the silicon carbide ceramic precursor gel drying method is supercritical drying or freeze drying.
8. The method of claim 1, wherein the silicon carbide ceramic precursor aerogel pyrolysis time is in the range of 2 to 6 hours.
9. The method of claim 1, wherein the pre-pyrolysis ramp rate is from 1 to 5 ℃/min.
10. A silicon carbide aerogel prepared by the method of any of claims 1-9, wherein the silicon carbide aerogel has a density of 0.143 to 0.476g/cm3Specific surface area of 120-780m2(ii)/g, the average pore diameter is 10-36 nm.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115583836A (en) * 2022-09-09 2023-01-10 航天特种材料及工艺技术研究所 High-temperature-resistant complex-phase ceramic aerogel and preparation method thereof

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Publication number Priority date Publication date Assignee Title
KR20110089243A (en) * 2011-07-13 2011-08-05 이재환 Illite-aerogel paint compositions
CN102675649A (en) * 2012-05-10 2012-09-19 航天材料及工艺研究所 Novel polycarbosilane and preparation method thereof
CN103772709A (en) * 2014-01-03 2014-05-07 航天材料及工艺研究所 Si/C/Zr ceramic precursor and preparation method thereof
CN103864076A (en) * 2012-12-11 2014-06-18 河南工业大学 Preparation method of silicon carbide aerogel on basis of SiO2 aerogel as template
CN105600785A (en) * 2015-12-24 2016-05-25 中国科学院宁波材料技术与工程研究所 Preparation method for silicon carbide aerogel
CN107324339A (en) * 2017-07-31 2017-11-07 西安天运新材料科技有限公司 One kind carbonization silica aerogel and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110089243A (en) * 2011-07-13 2011-08-05 이재환 Illite-aerogel paint compositions
CN102675649A (en) * 2012-05-10 2012-09-19 航天材料及工艺研究所 Novel polycarbosilane and preparation method thereof
CN103864076A (en) * 2012-12-11 2014-06-18 河南工业大学 Preparation method of silicon carbide aerogel on basis of SiO2 aerogel as template
CN103772709A (en) * 2014-01-03 2014-05-07 航天材料及工艺研究所 Si/C/Zr ceramic precursor and preparation method thereof
CN105600785A (en) * 2015-12-24 2016-05-25 中国科学院宁波材料技术与工程研究所 Preparation method for silicon carbide aerogel
CN107324339A (en) * 2017-07-31 2017-11-07 西安天运新材料科技有限公司 One kind carbonization silica aerogel and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115583836A (en) * 2022-09-09 2023-01-10 航天特种材料及工艺技术研究所 High-temperature-resistant complex-phase ceramic aerogel and preparation method thereof
CN115583836B (en) * 2022-09-09 2023-09-19 航天特种材料及工艺技术研究所 High-temperature-resistant complex-phase ceramic aerogel and preparation method thereof

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Application publication date: 20210323