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A kind of SICN ceramic airgel and its preparation method and application

A technology of airgel and ceramics, which is applied in the field of SiCN ceramic airgel and its preparation, can solve the problems of affecting high-temperature oxidation resistance and mechanical properties, unfavorable airgel microstructure control, and increased free carbon content, so as to benefit Effect of strengthening, low free carbon content and high porosity

Active Publication Date: 2022-03-22
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method for preparing SiCN ceramic airgel by polyvinylsilazane containing C=C double bond and Si-H, because it is a precursor molecule containing C=C double bond and Si-H at the same time, in the gel reaction In the later stage, the reaction will be terminated due to steric hindrance, so there are problems such as low crosslinking degree and weak airgel skeleton, which is not conducive to the control of airgel microstructure
The method of preparing SiCN ceramic airgel by polyvinylsilazane containing C=C double bond and divinylbenzene, since the theoretical carbon content in divinylbenzene is 92%, its addition will inevitably cause ceramic aircondensation The increase of free carbon content in the gel will affect its high temperature oxidation resistance and mechanical properties, and it cannot have low density, high airgel purity, good oxidation resistance, low free carbon content, high porosity, and high specific surface area.

Method used

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  • A kind of SICN ceramic airgel and its preparation method and application
  • A kind of SICN ceramic airgel and its preparation method and application
  • A kind of SICN ceramic airgel and its preparation method and application

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preparation example Construction

[0020] As mentioned above, the present invention provides a kind of preparation method of SiCN ceramic airgel in the first aspect, described preparation method comprises the following steps:

[0021] (1) Preparation of precursor solution: polysilazane containing Si-H bond in molecular structure and -CH=CH 2 The silazane oligomer is used as a precursor, and is prepared into a precursor solution under an inert protective atmosphere;

[0022] (2) Preparation of precursor wet sol: adding a curing agent to the precursor solution for curing reaction to obtain a precursor wet gel;

[0023] (3) Preparation of precursor airgel: drying the precursor wet gel to obtain precursor airgel;

[0024] (4) Preparation of ceramic airgel: in an inert protective atmosphere, the precursor airgel is pyrolyzed to obtain SiCN ceramic airgel.

[0025] In some preferred embodiments, the molecular structure of the polysilazane is shown in the following formula (I):

[0026]

[0027] The molecular st...

Embodiment 1

[0043] Under the protection of flowing nitrogen, the polysilazane (n is 5, m is 12.5) with formula (I) and the silazane oligomer (x is 9) with formula (II) are in a molar ratio of 1.2:1 , dissolved in cyclohexane, and stirred evenly to obtain a precursor solution containing 60% solvent, then add 0.01wt% platinum catalyst to it, continue to stir until uniform, transfer to a pressure reactor filled with nitrogen, at 180 ℃ reaction for 20h to obtain a light yellow silicon nitride precursor wet gel; after taking it out, soak it in cyclohexane for 6 days, during which the cyclohexane was replaced 3 times (replaced at 24h, 60h and 90h after soaking); The wet gel was passed through supercritical CO 2 Dry to obtain the precursor airgel; place the airgel in a high-temperature tube furnace, raise the temperature to 800°C at a rate of 2°C / min under high-purity argon, and keep it for 3 hours to obtain SiCN ceramic airgel glue. The obtained SiCN ceramic airgel has a density of 0.114g / cm ...

Embodiment 2

[0045] Under the protection of flowing argon, the polysilazane (n is 10, m is 25) with formula (I) and the silazane oligomer (x is 10) with formula (II) are 1.5 according to molar ratio: 1. Dissolve in n-hexane and stir evenly to obtain a precursor solution containing 65% solvent, then add 0.35wt% dicumyl peroxide to it, continue stirring until uniform, and transfer to a pressure reactor filled with nitrogen in 160°C for 10 hours to obtain a light yellow silicon nitride precursor wet gel; after taking it out, soak it in n-hexane for 6 days, during which n-hexane was replaced 3 times (replaced at 24h, 60h and 90h after soaking) ; The wet gel was freeze-dried to obtain a precursor airgel; the airgel was placed in a high-temperature tube furnace, and under high-purity argon, the temperature was raised to 1400 °C at a rate of 10 °C / min, and Keep it warm for 1 hour to get SiCN ceramic airgel. The obtained SiCN ceramic airgel has a density of 0.116g / cm 3 , the specific surface are...

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Abstract

The invention provides a SiCN ceramic airgel and its preparation method and application. The preparation method includes: using polysilazane containing Si-H bonds in molecular structure and containing -CH=CH 2 The silazane oligomer is used as a precursor, and is prepared into a precursor solution under an inert protective atmosphere; the preparation of the precursor wet sol: adding a curing agent to the precursor solution for curing reaction to obtain a precursor wet gel ; Preparation of precursor airgel: dry the precursor wet gel to obtain precursor airgel; Preparation of ceramic airgel: pyrolyze the precursor airgel in an inert protective atmosphere , to obtain SiCN ceramic airgel. The invention also provides the SiCN ceramic airgel prepared by the method and its application. The structure of the precursor used in the method of the present invention has strong designability, avoids the addition of unsaturated aromatic hydrocarbon compounds, and the obtained SiCN ceramic airgel has adjustable components, low free carbon content, high ceramic yield, low density, porosity and specific surface area High, can be used in thermal protection, stealth, fuel reforming or lithium-ion batteries and other fields.

Description

technical field [0001] The invention belongs to the field of ceramic airgel, and in particular relates to a SiCN ceramic airgel and a preparation method and application thereof. Background technique [0002] Airgel is a nanoporous material composed of nanoparticles and has a three-dimensional network skeleton structure. The developed porous structure endows it with different properties from traditional porous materials, especially ultra-low solid content and ultra-high porosity, etc. The characteristics make it have significant advantages in the fields of heat insulation, electromagnetic shielding, energy and chemical industry. At present, the research on aerogels mainly focuses on silica aerogels and carbon aerogels, but pure silica aerogels can be used for a long time below 650 °C, and can only be used for a short time at around 800 °C, and with the increase of temperature As the temperature increases, the thermal conductivity at high temperature increases rapidly, for ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/584C04B35/624C04B38/00
CPCC04B35/591C04B35/589C04B35/624C04B38/0054C04B2235/483C04B2235/6567C04B2235/656C04B2235/96C04B2235/77C04B38/0045C04B38/0067
Inventor 贺丽娟刘韬高翠雪刘圆圆李文静张昊赵英民
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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