CN109553395A - A kind of low cost preparation method of ceramic aerogel - Google Patents
A kind of low cost preparation method of ceramic aerogel Download PDFInfo
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- CN109553395A CN109553395A CN201811620414.9A CN201811620414A CN109553395A CN 109553395 A CN109553395 A CN 109553395A CN 201811620414 A CN201811620414 A CN 201811620414A CN 109553395 A CN109553395 A CN 109553395A
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Abstract
The invention discloses a kind of low cost preparation methods of ceramic aerogel, belong to aeroge preparation technical field.Include: 1) slurry preparation: preparing ceramic forerunner colloidal sol, chopped carbon fiber is evenly dispersed in precursor sol；2) form: chopped carbon fiber is formed, construct as it is sol bonded it is carbon fiber lapped made of porous three-dimensional block materials；3) solidify and crack: porous three-dimensional block materials being heated to presoma solidification temperature, presoma cracking temperature, then held for some time, furnace cooling are warming up to after isothermal holding；4) it removes carbon: resulting materials being heated to 400~1000 DEG C, heat preservation obtains ceramic aerogel.This method is suitable for the preparation of a variety of ceramic aerogels, without drying equipment at high cost and the drying process that time-consuming, has feature at low cost, high-efficient, can prepare the ceramic aerogel of various shape and size, is suitble to the large-scale production of aeroge.
Description
Technical field
The invention belongs to aeroge preparation technical fields, are related to a kind of low cost preparation method of ceramic aerogel.
Background technique
Aeroge is a kind of solid material formed by 90% with the gas of upper volume and 10% solid below, is had low
The features such as density, high-specific surface area, chemical property are stablized, and have unique acoustics, optics, calorifics, mechanics, electric property,
There is huge application value in the fields such as heat-insulation and heat-preservation, oxidation catalyst filter, energy-storage economical, intelligent sensing.Ceramic aerogel, which is removed, to be had
Other than above-mentioned advantage, also and meanwhile have both high temperature resistant, it is anti-oxidant, fire-retardant the features such as, be ideal high temperature insulating material.
The mainstream technology of preparing of ceramic aerogel is seasoning at present, it is therefore an objective to be obtained by the solvent in removal gel high
The porosity.Including three kinds of supercritical drying, freeze-drying and constant pressure and dry modes: 1) supercritical drying is current aeroge system
Earliest, most mature technique is studied in standby technology.Mainly by the control of pressure and temperature, locate solvent in the drying process
In vapor liquid equilibrium state, the density of liquid is identical with the saturated vapor density of its own at this time, and gas-liquid interface disappears, capillary force
It disappears, dried medium replaces the solvent in gel, is then slowly decreased pressure release fluid, obtains the gas of porous network structure
Gel.Supercritical drying is needed using autoclave, and requires height to the airtightness of autoclave, and complex operation is with high costs,
And solvent-oil ratio is big, there are problems that safety anti-explosive, this limits the large-scale production of aeroge to a certain extent；2) it freezes
Drying is that the mixed liquor elder generation cryogenic freezing for forming target particles or fiber and colloidal sol forms, in the process, a large amount of column ice
Crystals growth, target particles or fiber are assembled between these ice crystals, form tridimensional network, then the decompression that heats up makes solvent liter
China leaves the aeroge of high porosity.However in gel freezing, solvent is undergone phase transition, it will usually volume change is generated, in mesh
Stress is generated in mark particle and fibroplastic three-dimensional net structure, the hole configurations of gel is damaged, causes freezing dry
The reliability decrease of dry technology is not suitable for the preparation of large scale aeroge.It is taken in addition, freeze drying process prepares aeroge
Between it is longer, production efficiency is low, causes at high cost, it is difficult to the industrial volume production for aeroge；3) constant pressure and dry refers in normal pressure
Solvent is dried under environment, process conditions are simple, avoid the stringent process conditions of supercritical drying high temperature, high pressure.But
Since there are capillary force, constant pressure and dry process often will cause gel shrinks cracking, need to be modified gel to reduce
Gel shrinks.And constant pressure and dry process has solvent displacement, and time-consuming, and required low surface tension solvent is usual
Toxic, solvent-oil ratio is big, causes the application of constant pressure and dry technology of preparing limited.
The common feature of above-mentioned three kinds of methods be it is at high cost, complex process, the period is long, and low efficiency seriously limits ceramics
The preparation and application of aeroge.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of low costs of ceramic aerogel
Preparation method, this method simple process is low for equipment requirements, and preparation efficiency is high, it is easy to accomplish industrial scale production.
In order to achieve the above object, the present invention is achieved by the following scheme:
A kind of low cost preparation method of ceramic aerogel disclosed by the invention, comprising the following steps:
1) colloidal sol is prepared: according to target aeroge at the corresponding precursor sol of assignment system；
2) prepared by slurry: a certain amount of chopped carbon fiber being mixed with precursor sol, keeps chopped carbon fiber evenly dispersed
In precursor sol；
3) form: chopped carbon fiber is formed, construct as it is sol bonded it is carbon fiber lapped made of porous three-dimensional block material
Material；
4) solidify and crack: porous three-dimensional block materials are heated to presoma solidification temperature, keep the temperature, before then raising temperature to
Body cracking temperature is driven, then is kept the temperature, by the chemical reaction between cracked gas, generates monodimension nanometer material, and finally cold with furnace
But to room temperature, 1-dimention nano ceramics/carbon fiber composite block material is obtained；
5) it removes carbon: 1-dimention nano ceramics/carbon fiber composite block material is placed in air furnace, and it is heated to 400~
1000 DEG C, heat preservation obtains ceramic aerogel.
Preferably, in step 1), by selecting the ingredient of precursor sol, different types of ceramic airsetting can be prepared
Glue.
Preferably, in step 2), by adjusting the colloidal sol amount on chopped carbon fiber surface, the close of ceramic aerogel can be adjusted
Degree and intensity.
Preferably, by adjusting the length and chopped carbon fiber skeletal density of chopped carbon fiber, ceramic airsetting can be adjusted
The density and the porosity of glue.
Preferably, in step 4), by adjusting cracking temperature and atmosphere, different types of ceramic aerogel is prepared.
Preferably, it is mutually formed by overlapping using ceramic aerogel made from the method for the present invention with fiber network-like microcosmic
Structure.
Compared with prior art, the invention has the following advantages:
The preparation method of ceramic aerogel disclosed by the invention, when preparing slurry, with chopped carbon fiber and precursor colloidal sol
Mixing, the aqueous precursor gel of target aerogel material only exist at chopped carbon fiber template surface and node, and by the carbon that is chopped
It being free of in the gap formed between fiber or content is considerably less, entire chopped carbon fiber skeleton is still with high porosity, this
Just maximized space is provided for the generation of target material.Meanwhile the target material presoma in chopped carbon fiber skeleton is solidifying
Glue is also in accordingly porous skeleton structure, this is conducive to aqueous precursor gel and is utmostly converted to target material, obtained aeroge
Purity is high, impurity are very less or free from foreign meter.Entire preparation process is simple, is realized by oxidation removal chopped carbon fiber
High porosity, it is low for equipment requirements without expensive special drying equipment and the drying process that time-consuming, process conditions are harsh,
And mainstream technology can be prepared and be difficult to the various shape prepared and sized ceramics aeroge.Without consuming a large amount of solvent, and it is used
Nontoxic solvent can be recycled, and preparation efficiency height has the characteristics that high-efficient, at low cost.Therefore, the method for the present invention is suitable for
SiC、Si3N4、SiO2Etc. the preparation of a variety of ceramic aerogels.Meanwhile prepared ceramic aerogel all there is fiber mutually to overlap
Made of at network-like microstructure so that ceramic aerogel is keeping stable mechanical property to have excellent flexibility simultaneously,
The brittleness problems that ceramic aerogel prepared by mainstream technology has are overcome, so that the reliability of ceramic aerogel obtains significantly
It improves, makes the application scenarios more horn of plenty of aeroge.
Detailed description of the invention
Fig. 1 is the low cost preparation method process route chart of ceramic aerogel disclosed by the invention；
Fig. 2-1 is the photomacrograph of SiC aeroge prepared by embodiment 1；
Fig. 2-2 is the XRD diagram of SiC aeroge prepared by embodiment 1；
Fig. 2-3 is the SEM figure of SiC aeroge prepared by embodiment 1；
Fig. 3-1 is Si prepared by embodiment 23N4The photomacrograph of aeroge；
Fig. 3-2 is Si prepared by embodiment 23N4The XRD diagram of aeroge；
Fig. 3-3 is Si prepared by embodiment 23N4The SEM of aeroge schemes；
Fig. 4-1 is SiO prepared by embodiment 32The photomacrograph of aeroge；
Fig. 4-2 is SiO prepared by embodiment 32The XRD diagram of aeroge；
Fig. 4-3 is SiO prepared by embodiment 32The SEM of aeroge schemes.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Referring to Fig. 1, the method for low cost preparation ceramic aerogel of the invention, comprising the following steps:
1) prepared by slurry: preparing has certain density ceramic forerunner colloidal sol, and a certain amount of chopped carbon fiber is uniform
Ground is dispersed in precursor solution；
2) form: chopped carbon fiber is formed, construct as it is sol bonded it is carbon fiber lapped made of porous three-dimensional block material
Material；
3) solidify and crack: the porous three-dimensional block materials are heated to presoma solidification temperature, held for some time, with
After be warming up to presoma cracking temperature, then held for some time, furnace cooling；
4) it removes carbon: resulting materials being heated to 400-1000 DEG C, held for some time obtains ceramic aerogel.
Embodiment 1
The present embodiment is prepared for SiC aeroge, the specific steps are as follows:
1) precursor solution is prepared.With polysiloxanes colloidal sol (mass fraction 50wt.%) for raw material, dehydrated alcohol is as molten
Agent (mass fraction 50wt.%), prepares silica solution；
2) chopped carbon fiber (length 1mm, mass fraction 1wt.%) is dispersed in silica solution, and carries out machinery and stirs
It mixes, is dispersed in chopped carbon fiber in silica solution；
3) using the method for vacuum filtration, extra silica solution is removed, overlaps the carbon fiber being dispersed in colloidal sol mutually
The block of layered structure；
4) temperature rises to 100 DEG C, isothermal holding 4 hours, makes its solidification, is then heated to 1500 DEG C, argon gas isothermal holding
4h, gel are cracked to form SiC nanowire, cool to room temperature with the furnace, form SiC nanowire/carbon fiber skeleton intermediate structure；
5) intermediate structure is warming up to 700, isothermal holding 2h again, obtains SiC aeroge.
SiC aeroge photomacrograph made from the present embodiment is as shown in Fig. 2-1, it can be seen from the figure that the SiC airsetting
Glue is stood at the tip of asparagus fern vein, and therefore asparagus fern vein does not occur bending and deformation, embody SiC made from the present embodiment
Aeroge has ultralow density.
The XRD diagram of SiC aeroge is as shown in Fig. 2-2 made from the present embodiment, from XRD diagram as can be seen that the present embodiment system
The SiC aeroge obtained is 3C-SiC, and nearby shows a small peak at 33.7 °, this is because being had in silicon carbide nanometer line
Caused by some faults.Show that there is more fault in the nano wire in this method preparation carbonization silica aerogel, is conducive to drop
Low-carbon SiClx thermal conductivity.
The SEM photograph of SiC aeroge made from the present embodiment is referring to figure 2-3, it is seen then that SiC aeroge is received by a large amount of SiC
Rice noodles intertwine with each other constituted three-dimensional net structure.The length of silicon carbide nanometer line between 50~300 μm, diameter 30~
Between 200nm.
Embodiment 2
The present embodiment is prepared for Si3N4Aeroge, the specific steps are as follows:
1) precursor solution is prepared.With polysiloxanes colloidal sol (mass fraction 60wt.%) for raw material, dehydrated alcohol is as molten
Agent (mass fraction 40wt.%), prepares silica solution；
2) 10g chopped carbon fiber (average length is about 1mm) is dispersed in 1000ml silica solution, and carries out ultrasound plus machine
Tool stirring, is dispersed in chopped carbon fiber in silica solution；
3) method for using filters pressing, removes extra silica solution, carbon fiber is made mutually to be overlapped to form the block of layer structure；
4) 70 DEG C are warming up to, isothermal holding 8 hours, solidifies colloidal sol, then heats to 1550 DEG C of temperature, at nitrogen heat preservation
2h is managed, gel is cracked, reaction generates Si3N4Nanobelt, furnace cooling form Si3N4Knot among nanobelt/carbon fiber skeleton
Structure；
5) intermediate structure is placed in air furnace and is warming up to 1000 DEG C, isothermal holding 0.5h, oxidation removal carbon fiber,
Obtain Si3N4Aeroge.
Si made from the present embodiment3N4Aeroge photomacrograph as shown in figure 3-1, it can be seen from the figure that the Si3N4Gas
Gel, macroscopically white, millimetre-sized overlength silicon nitride nano band is contained on aeroge surface.
The XRD diagram of SiC aeroge made from the present embodiment as shown in figure 3-2, from XRD diagram as can be seen that the present embodiment system
The Si obtained3N4The characteristic peak of aeroge belongs to typical α-Si3N4, and no other impurity peaks show Si made from this method3N4Gas
Gel purity is high.
Si made from the present embodiment3N4The SEM photograph of aeroge is referring to Fig. 3-3, it is seen then that Si3N4Microcosmic aeroge is by nothing
Several silicon nitride nano bands intertwine with each other constituted network-like structure.The network-like structure of this high porosity makes silicon nitride gas
Gel has excellent heat preservation and insulation.
Embodiment 3
The present embodiment is prepared for SiO2Aeroge, the specific steps are as follows:
1) with ethyl orthosilicate (mass fraction 40wt.%) for raw material, dehydrated alcohol (mass fraction 60wt.%) is as molten
Agent prepares silica solution；
2) 2g chopped carbon fiber is dispersed in 300ml silica solution, carries out mechanical stirring 10min, make chopped carbon fiber point
It dissipates uniformly in silica solution；
3) using the method for vacuum filtration, carbon fiber is made mutually to be overlapped to form the block of layer structure；
4) 150 DEG C are warming up to, isothermal holding 3 hours, solidifies colloidal sol, 800 DEG C is warming up in argon atmosphere,
Isothermal holding 2h, gel are cracked to form SiO2, cool to room temperature with the furnace, obtain SiO2/ carbon fiber intermediate structure；
5) intermediate structure is placed in air furnace and is warming up to 400 DEG C, isothermal holding 10h, oxidation removal carbon fiber obtains
Obtain SiO2Aeroge.
SiO made from the present embodiment2Aeroge photomacrograph is as shown in Fig. 4-1, it can be seen from the figure that the SiO2Airsetting
Glue is macroscopically white.
SiO made from the present embodiment2The XRD diagram of aeroge as shown in the Fig. 4-2, from XRD diagram as can be seen that the present embodiment system
The SiO obtained2Aeroge belongs to amorphous silica.Compared to the silica aerogel of crystalline state, amorphous oxide silica aerogel has more
Low thermal conductivity is particularly suited for heat-insulation and heat-preservation application.
SiO made from the present embodiment2The SEM photograph of aeroge referring to fig. 4-3, it is seen then that SiO2Aeroge microstructure be by
The network-like structure of the silica micron tube composition of no several hollow forms, the diameter of micron tube is at 2 μm or so.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (6)
1. a kind of low cost preparation method of ceramic aerogel, which comprises the following steps:
1) colloidal sol is prepared: according to target aeroge at the corresponding precursor sol of assignment system；
2) prepared by slurry: a certain amount of chopped carbon fiber being mixed with precursor sol, before being dispersed in chopped carbon fiber
It drives in body colloidal sol；
3) form: chopped carbon fiber is formed, construct as it is sol bonded it is carbon fiber lapped made of porous three-dimensional block materials；
4) solidify and crack: porous three-dimensional block materials are heated to presoma solidification temperature, keep the temperature, then raise temperature to presoma
Cracking temperature, then keep the temperature, by the chemical reaction between cracked gas, monodimension nanometer material is generated, and finally cool to the furnace
Room temperature obtains 1-dimention nano ceramics/carbon fiber composite block material；
5) it removes carbon: 1-dimention nano ceramics/carbon fiber composite block material being placed in air furnace, and is heated to 400~1000 DEG C,
Heat preservation obtains ceramic aerogel.
2. the low cost preparation method of ceramic aerogel according to claim 1, which is characterized in that in step 1), pass through
The ingredient for selecting precursor sol, can prepare different types of ceramic aerogel.
3. the low cost preparation method of ceramic aerogel according to claim 1, which is characterized in that in step 2), pass through
The colloidal sol amount for adjusting chopped carbon fiber surface, can adjust the density and intensity of ceramic aerogel.
4. the low cost preparation method of ceramic aerogel according to claim 1, which is characterized in that by adjusting the carbon that is chopped
The length and chopped carbon fiber skeletal density of fiber, can adjust the density and the porosity of ceramic aerogel.
5. the low cost preparation method of ceramic aerogel according to claim 1, which is characterized in that in step 4), pass through
Cracking temperature and atmosphere are adjusted, different types of ceramic aerogel is prepared.
6. the low cost preparation method of ceramic aerogel described according to claim 1~any one of 5, which is characterized in that
The network-like microstructure that there is ceramic aerogel obtained fiber to be mutually formed by overlapping.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590394A (en) * | 2019-10-29 | 2019-12-20 | 中钢集团洛阳耐火材料研究院有限公司 | Low-cost preparation method of large-size SiC nanowire aerogel |
| CN112047742A (en) * | 2020-09-03 | 2020-12-08 | 中钢南京环境工程技术研究院有限公司 | Low-cost preparation method of large-size silicon nitride nanobelt aerogel |
| CN113754446A (en) * | 2020-06-02 | 2021-12-07 | 中国科学院化学研究所 | 3D printing silicon nitride fiber aerogel and preparation method and application thereof |
| CN114751764A (en) * | 2021-02-09 | 2022-07-15 | 海南大学 | Multifunctional ceramic nanofiber sponge and preparation method thereof |
| CN114890425A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Elastic silicon carbide nanowire aerogel with multilevel structure and 3D printing preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7560062B2 (en) * | 2004-07-12 | 2009-07-14 | Aspen Aerogels, Inc. | High strength, nanoporous bodies reinforced with fibrous materials |
| US20100189991A1 (en) * | 2008-11-17 | 2010-07-29 | Lytle Justin C | Macroporous carbon nanofoam composites and methods of making the same |
| CN104909798A (en) * | 2015-05-25 | 2015-09-16 | 航天材料及工艺研究所 | Silicon carbide fiber lightweight high-temperature insulating material, and preparation method thereof |
| CN107188527A (en) * | 2017-06-19 | 2017-09-22 | 西安交通大学 | A kind of SiC flexible ceramics constructed by nano wire and preparation method thereof |
-
2018
- 2018-12-28 CN CN201811620414.9A patent/CN109553395B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7560062B2 (en) * | 2004-07-12 | 2009-07-14 | Aspen Aerogels, Inc. | High strength, nanoporous bodies reinforced with fibrous materials |
| US20100189991A1 (en) * | 2008-11-17 | 2010-07-29 | Lytle Justin C | Macroporous carbon nanofoam composites and methods of making the same |
| CN104909798A (en) * | 2015-05-25 | 2015-09-16 | 航天材料及工艺研究所 | Silicon carbide fiber lightweight high-temperature insulating material, and preparation method thereof |
| CN107188527A (en) * | 2017-06-19 | 2017-09-22 | 西安交通大学 | A kind of SiC flexible ceramics constructed by nano wire and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590394A (en) * | 2019-10-29 | 2019-12-20 | 中钢集团洛阳耐火材料研究院有限公司 | Low-cost preparation method of large-size SiC nanowire aerogel |
| CN110590394B (en) * | 2019-10-29 | 2020-08-14 | 中钢集团洛阳耐火材料研究院有限公司 | Low-cost preparation method of large-size SiC nanowire aerogel |
| CN113754446A (en) * | 2020-06-02 | 2021-12-07 | 中国科学院化学研究所 | 3D printing silicon nitride fiber aerogel and preparation method and application thereof |
| CN112047742A (en) * | 2020-09-03 | 2020-12-08 | 中钢南京环境工程技术研究院有限公司 | Low-cost preparation method of large-size silicon nitride nanobelt aerogel |
| CN114751764A (en) * | 2021-02-09 | 2022-07-15 | 海南大学 | Multifunctional ceramic nanofiber sponge and preparation method thereof |
| CN114751764B (en) * | 2021-02-09 | 2023-06-09 | 海南大学 | Multifunctional ceramic nanofiber sponge and preparation method thereof |
| CN114890425A (en) * | 2022-04-02 | 2022-08-12 | 西安交通大学 | Elastic silicon carbide nanowire aerogel with multilevel structure and 3D printing preparation method and application thereof |
| CN114890425B (en) * | 2022-04-02 | 2023-12-19 | 西安交通大学 | Multilevel-structure elastic silicon carbide nanowire aerogel, and 3D printing preparation method and application thereof |
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