CN109704781A - A kind of silicon nitride nano band aeroge and preparation method thereof - Google Patents
A kind of silicon nitride nano band aeroge and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of silicon nitride nano band aeroge and preparation method thereof, 1) prepare polysiloxanes colloidal sol；2) slurry is prepared；3) the three-dimensional porous carbon fiber skeleton that formation is mutually overlapped by the chopped carbon fiber of siloxane sol bonding is constructed；4) solidify and crack: three-dimensional porous carbon fiber skeleton is heated to the solidification temperature of polysiloxanes colloidal sol, isothermal holding heating and heat preservation in nitrogen atmosphere handles, cools to room temperature with the furnace, obtain carbon fiber/silicon nitride nano fiber composite block；5) it removes carbon: carbon fiber/silicon nitride nano fiber composite block is heated to 400 DEG C~1000 DEG C, and 2~4h of isothermal holding in air, obtain silicon nitride nano band aeroge.Nitridation silica aerogel using this method preparation has very excellent high-temperature stability and heat-proof quality, and overcome the brittleness problems of traditional ceramics aeroge, it is at low cost, high-efficient without expensive drying equipment and inefficient drying process, it is suitably applied the fields such as heat-insulated, heat preservation, wave transparent.
Description
Technical field
The invention belongs to the preparation technical fields of aeroge, are related to a kind of silicon nitride nano band aeroge and its preparation side
Method.
Background technique
Aeroge is solid most light known to the current mankind, there is the superelevation porosity, thus with very excellent heat-insulated
Thermal insulation property, it is considered to be substitute the best new material of traditional heat-insulating heat-preserving material.The service life of aeroge is that tradition is heat-insulated
Ten times or more of thermal insulation material, and using aeroge as heat-insulating heat-preserving material, the thickness of material requested is only the heat-insulated guarantor of tradition
/ 5th of adiabator arrive half, and quality is lighter, this not only shows great application value in civil field, and
And there is unmatched advantage in military heat-insulation and heat-preservation field.So far, aeroge is mainly in the application of civilian aspect
The heat-insulation and heat-preservations of some industry heat supply pipelines, LNG storage, new energy bus the fields such as the heat-insulated protective plate of battery；In military side
The utilization in face is mainly on the heat insulating member of aircraft.All in all, the application scenarios of aeroge are also far from reaching at present
Expection of the people to it, the preparation cost that this is primarily due to aeroge is high, and maximum operation (service) temperature is limited, and usually in crisp
Property, it can not directly use, need just to can guarantee certain reliability after compound with other inorfils, but also while also will increase
The density of aeroge.
At present in ceramic aerogel technology of preparing it is the most mature be aerosil, signified aeroge in the market
Almost it is defaulted as aerosil.But aerosil has brittleness big, and temperature tolerance is poor, uses temperature for a long time
No more than 650 DEG C, because there is " the pearl neck " formed that contacted with each other by nanometer silicon dioxide particle in high temperature aerobic environment
Structure easily shrinks the disadvantages of failure.It is same although the use temperature of conventional aluminium oxide aeroge can reach 1000 DEG C
Also there is brittleness disadvantage, reliability is low, greatly limits the application field and depth of ceramic aerogel.As national defence is to material
Military service performance requirement in extreme environment is higher and higher and industrial circle is to energy-efficient material increasing need, compels
New technology of preparing will be improved and research and develop by being essential, and prepare that high temperature stability performance is excellent, and heat-proof quality is good with lower cost, and
Ceramic aerogel material with excellent mechanical performances.
Silicon nitride also has very excellent thermostabilization because all having good mechanical property under high temperature and room temperature
Property, high ablation resistance, compared to conventional oxide ceramics, silicon nitride possesses outstanding high-temperature comprehensive property.But it nitrogenizes
Silica aerogel is but rarely reported.We during early-stage study, applied one about the " silicon nitride nano of compressible reply
(application number: being the method preparation nanometer using quasi- CVD 201610566429.6) to the patent of line aeroge and its technology of preparing "
Line paper, then block aeroge is obtained after compound, although nitridation silica aerogel, but low output, period has been prepared in this method
It is long, at high cost.
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 silicon nitride nano band aeroges
And preparation method thereof, this method is easy to operate, low for equipment requirements, process safety is controllable, high-efficient；Through nitrogen made from this method
SiClx nanobelt aeroge high-temperature stability, thermal insulation and mechanical property are excellent, and size is controllable.
In order to achieve the above object, the present invention is achieved by the following scheme:
A kind of preparation method the invention discloses silicon nitride nano with aeroge, comprising the following steps:
1) it prepares polysiloxanes colloidal sol: after siloxane sol, water and dehydrated alcohol are mixed, polysiloxanes colloidal sol is made；
2) it prepares slurry: chopped carbon fiber being dispersed in polysiloxanes colloidal sol made from step 1), carbon fiber is made
Surface coats one layer of siloxane sol；
3) it forms: constructing the three-dimensional porous carbon fiber bone for mutually overlapping formation by the chopped carbon fiber of siloxane sol bonding
Frame；
4) solidify and crack: three-dimensional porous carbon fiber skeleton is heated to the solidification temperature of polysiloxanes colloidal sol, at heat preservation
4~8h is managed, 1200 DEG C~1700 DEG C are warming up in nitrogen atmosphere, 1~3h of isothermal holding cools to room temperature with the furnace, obtains
Carbon fiber/silicon nitride nano fiber composite block；
5) it removes carbon: carbon fiber/silicon nitride nano fiber composite block is heated to 400 DEG C~1000 DEG C in air, and
1~8h of isothermal holding obtains silicon nitride nano band aeroge.
Preferably, in step 1), by percentage to the quality, comprising: 10%~70% siloxane sol, 10%~50%
Water and 10%~80% dehydrated alcohol；And siloxane sol uses methyltrimethoxysilane and/or dimethylformamide dimethyl oxygen
Base silane.
3, preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that step 2)
In, chopped carbon fiber average length used is 0.5mm~2mm.
4, preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that step 3) is adopted
Unreacted siloxane sol is removed with vacuum filtration method or filter press technique, forms chopped carbon fiber sol bonded by polysiloxanes
Three-dimensional porous carbon fiber skeleton.
5, preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that step 4)
In, the solidification temperature of polysiloxanes colloidal sol is 80~120 DEG C, and nitrogen pressure is 0.1~2MPa, heating rate is 2~10 DEG C/
min。
6, preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that step 5)
In, 400~1000 DEG C are risen in air with the heating rate of 1 DEG C~10 DEG C/min.
7, according to claim 1~any one of 6 described in preparation method of the silicon nitride nano with aeroge, feature
It is, intensity of the silicon nitride nano with aeroge and density are adjustable, it is embodied in:
By changing the solubility or crosslinking degree of siloxane sol, regulate and control intensity of the silicon nitride nano with aeroge and close
Degree；
Alternatively, regulating and controlling intensity and density of the silicon nitride nano with aeroge by the average length for changing chopped carbon fiber；
Alternatively, regulating and controlling silicon nitride nano by the retention amount for changing polysiloxanes colloidal sol in three-dimensional porous carbon fiber skeleton
Intensity and density with aeroge；
Alternatively, regulating and controlling intensity and density of the silicon nitride nano with aeroge by control nitrogen pressure.
8, using silicon nitride nano made from preparation method described in any one of claim 1~7 band aeroge,
It is characterized in that, density of the silicon nitride nano with aeroge is 5mg/cm3~50mg/cm3, thermal conductivity be 0.030W/mK~
0.051W/mK, silicon nitride nano strip length are 100 μm~500 μm, and width is 0.2~3 μm.
Compared with prior art, the invention has the following advantages:
Preparation method of the silicon nitride nano disclosed by the invention with aeroge, by siloxane sol, water, dehydrated alcohol with one
Certainty ratio is mixed with polysiloxanes colloidal sol, and then chopped carbon fiber is dispersed in prepared polysiloxanes colloidal sol,
The three-dimensional porous skeleton that formation is mutually overlapped by the chopped carbon fiber that siloxane sol bonds is constructed, at then cured and cracking
Reason obtains silicon nitride nano fiber aeroge.In the methods of the invention, Silica hydrogel is only in chopped carbon fiber template surface and node
Place exists, and is free of in the gap by being formed between chopped carbon fiber or content is considerably less, and entire chopped carbon fiber skeleton is still
With high porosity, this just provides maximized space for the growth of silicon nitride nano band, is the high porosity of aeroge
Provide guarantee.Meanwhile the Silica hydrogel in chopped carbon fiber skeleton is also accordingly in porous skeleton structure, and therefore, after Pintsch process,
The Silica hydrogel of high porosity (high-specific surface area) can be cracked into gas phase with maximum conversion ratio, and generate nitrogen as reactant
SiClx nanobelt, after last oxidation removes chopped carbon fiber template, obtained aeroge is that pure phase nitrogenizes silica aerogel, purity
Height, it is very less or free from foreign meter containing other impurity.The present invention is by introducing life of the carbon fiber skeleton as silicon nitride nano fiber
Long template increases its growing space, by control template size be can control final aerogel block body size, it can be achieved that
The magnanimity preparation of low cost, provides further technical foundation for the industrialization of silicon nitride ceramics aeroge.
Nitridation silica aerogel using this method preparation has very excellent high-temperature stability and heat-proof quality, and overcomes
The brittleness problems of traditional ceramics aeroges, it is at low cost, high-efficient without expensive drying equipment and inefficient drying process,
It is suitably applied the fields such as heat-insulated, heat preservation, wave transparent.
Detailed description of the invention
Fig. 1 is nitridation silica aerogel preparation flow artwork of the invention；
Fig. 2 is the macro morphology photo of the nitridation silica aerogel obtained of embodiment 1；
Fig. 3 is the microcosmic scanned photograph of nitridation silica aerogel of the nitridation silica aerogel obtained of embodiment 1；
Fig. 4, which is that embodiment 2 is obtained, nitrogenizes silica aerogel XRD diagram；
Fig. 5 is the thermogravimetric curve in air atmosphere of the nitridation silica aerogel obtained of embodiment 2；
Fig. 6 is the stress-strain diagram of the nitridation silica aerogel obtained of embodiment 2.
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 term " includes " and " having " and their any deformation, it is intended that cover non-exclusive packet
Contain, for example, what the process, method, system, product or equipment for containing a series of steps or units were not necessarily limited to be clearly listed
Those step or units, but may include be not clearly listed or it is intrinsic for these process, methods, product or equipment
Other step or units.
The invention will be described in further detail with reference to the accompanying drawing:
It is the preparation method process flow chart of silicon nitride nano fiber aeroge of the invention, including following step referring to Fig. 1
It is rapid:
It 1) is raw material with siloxane precursors, such as methyltrimethoxysilane, dimethyldimethoxysil,ne, water is as friendship
Join agent, dehydrated alcohol is solvent, prepares polysiloxanes colloidal sol with certain proportion；
2) a certain amount of chopped carbon fiber is evenly dispersed in polysiloxanes colloidal sol, makes carbon fiber surface with one layer
Siloxane sol；
3) it forms: removing most silica solution, such as using vacuum filtration or the method for filters pressing, form chopped carbon fiber
By the sol bonded three-dimensional porous carbon fiber skeleton of polysiloxanes；
4) solidify: three-dimensional porous carbon fiber skeleton is placed in 4~8h of isothermal holding in 80 DEG C~120 DEG C environment；
5) it cracks: the carbon fiber skeleton after curing process being placed under certain nitrogen pressure, is warming up to 1200 DEG C~1700
DEG C, and 1~3h is kept the temperature, it then cools to room temperature with the furnace, obtains carbon fiber/silicon nitride nano fiber composite block；
6) 400 DEG C~1000 DEG C and 1~8h of isothermal holding are risen in air with certain heating rate, obtain silicon nitride
Aeroge.
Embodiment 1
It is 5mg/cm that the present embodiment, which is prepared for density,3, and the adjustable nitridation silica aerogel of size, density, specific steps are such as
Under:
1) with methyltrimethoxysilane (mass fraction 10wt.%) and raw materials of silica sol, using water as crosslinking agent (quality
Score 30wt.%) dehydrated alcohol as solvent (mass fraction 60wt.%), prepares silica solution；
2) 2g chopped carbon fiber (length about 2mm) is dispersed in 100ml silica solution, mechanical stirring 10min；
3) using the method for vacuum filtration, the carbon fiber being dispersed in colloidal sol is made mutually to be overlapped to form three-dimensional porous carbon fiber bone
Frame；
4) porous carbon fiber skeleton is placed in 100 DEG C of environment, isothermal holding 4 hours；
5) 1400 DEG C of temperature are risen in the nitrogen that pressure is 0.2Mpa, isothermal holding 2h is generated in carbon fiber skeleton
A large amount of silicon nitride nano fibers, furnace cooling；
6) 400 DEG C, isothermal holding 8h are risen in air with the heating rate of 10 DEG C/min, oxidation removal carbon fiber obtains
Silica aerogel must be nitrogenized.
It as a result referring to fig. 2, is nitridation silica aerogel photomacrograph obtained, from figure 2 it can be seen that using present invention side
Nitridation silica aerogel obtained by method is macroscopically white, and millimetre-sized overlength silicon nitride nano band is contained on aeroge surface.
It is the microcosmic scanned photograph of nitridation silica aerogel obtained referring to Fig. 3.It can be seen from the figure that nitridation silica aerogel
Microcosmic is by intertwineing with each other constituted network-like structure without several silicon nitride nano bands.The network-like structure of this high porosity
Nitridation silica aerogel is set to have excellent heat preservation and insulation.
Embodiment 2
It is 15mg/cm that the present embodiment, which is prepared for density,3, and the adjustable nitridation silica aerogel of size, density, specific steps are such as
Under:
1) with dimethyldimethoxysil,ne (mass fraction 40wt.%) for raw material, using water as crosslinking agent (mass fraction
10wt.%) dehydrated alcohol prepares polysiloxanes colloidal sol as solvent (mass fraction 50wt.%)；
2) chopped carbon fiber (length is about 1mm) is dispersed in silica solution, carries out mechanical stirring 10min；
3) using the method for vacuum filtration, the carbon fiber being dispersed in colloidal sol is made mutually to be overlapped to form three-dimensional porous carbon fiber bone
Frame；
4) porous carbon fiber skeleton is placed in 70 DEG C of baking ovens, isothermal holding 8 hours；
5) 1550 DEG C, isothermal holding 2h are risen in the nitrogen that pressure is 0.5Mpa, is generated in carbon fiber skeleton a large amount of
Silicon nitride nano fiber, furnace cooling；
6) 1000 DEG C, isothermal holding 1h are risen in air with the heating rate of 2 DEG C/min, oxidation removal carbon fiber obtains
Silica aerogel must be nitrogenized.
It referring to fig. 4, is the XRD spectra of the present embodiment nitridation silica aerogel obtained.It can be seen from the figure that silicon nitride gas
The characteristic peak of gel belongs to typical α-Si3N4, and no other impurity peaks show that this method is obtained and nitrogenize silica aerogel purity
It is high.
It is the thermogravimetric curve in air atmosphere of the present embodiment nitridation silica aerogel obtained referring to Fig. 5.Heating rate
For 10 DEG C/min, it can be seen from the figure that the quality technology for nitrogenizing silica aerogel is protected in 10100 DEG C of air environments below
It holds constant, shows extremely excellent high-temperature oxidation resistance and high-temperature stability；When temperature is higher than 10100 DEG C, SiC aeroge
Quality starts to be slowly increased, this mainly nitrogenizes the silicon oxide layer of the beta-silicon nitride nanowire Surface Creation in silica aerogel and is led
It causes.When temperature rises to 1200 DEG C, it is only 103wt.% that the weight gain for nitrogenizing silica aerogel, which is less than, this shows that nitrogenizing silica aerogel exists
There is excellent antioxygenic property and thermal stability in high temperature air environment, be suitable as the materials such as high temperature insulating, filtering.
It is density made from the present embodiment is 16mg/cm referring to Fig. 63Nitridation silica aerogel stress-strain diagram.From
As can be seen that being 16mg/cm using density prepared by method disclosed by the invention in figure3, the porosity be 99.5% nitridation
Silica aerogel overcomes the brittleness problems of traditional ceramics aeroge, has certain elasticity and compression and back renaturation.When compressed shape variable
After reaching 90%, nitridation silica aerogel overall structure keeps very complete, and no macroscopic cracking generates, and compression stress is up to
0.15MPa, this belongs to the extremely excellent one kind of performance in other aerogel materials that the porosity is up to 99.5%.Without brittleness,
This compressible, high-intensitive three big mechanical characteristic makes nitridation silica aerogel produced by the present invention can be realized answering for various scenes
With, such as heat supply pipeline, new energy battery thermal insulation board, LNG storage transport.
Embodiment 3
It is 30mg/cm that the present embodiment, which is prepared for density,3, and the adjustable nitridation silica aerogel of size, density, specific steps are such as
Under:
1) with methyltrimethoxysilane (mass fraction 60wt.%) for raw material, using water as crosslinking agent (mass fraction
30wt.%) dehydrated alcohol prepares silica solution as solvent (mass fraction 10wt.%)；
2) 2g chopped carbon fiber (length is about 0.5mm) is dispersed in 100ml silica solution, carries out mechanical stirring and ultrasound
5min；
3) method for using filters pressing, makes the carbon fiber being dispersed in colloidal sol mutually be overlapped to form three-dimensional porous carbon fiber skeleton；
4) porous carbon fiber skeleton is placed in 70 DEG C of baking ovens, isothermal holding 8 hours；
5) 1700 DEG C are risen in the nitrogen that pressure is 1Mpa, isothermal holding 3h generates a large amount of nitrogen in carbon fiber skeleton
SiClx nanofiber, furnace cooling；
6) 700 DEG C, isothermal holding 4h are risen in air with the heating rate of 1 DEG C/min, oxidation removal carbon fiber obtains
Nitrogenize silica aerogel.
Embodiment 4
It is 50mg/cm that the present embodiment, which is prepared for density,3, and the adjustable nitridation silica aerogel of size, density, specific steps are such as
Under:
1) with methyltrimethoxysilane (mass fraction 70wt.%) for raw material, using water as crosslinking agent (mass fraction
20wt.%) dehydrated alcohol prepares silica solution as solvent (mass fraction 10wt.%)；
2) 2g chopped carbon fiber (length is about 1.5mm) is dispersed in 100ml silica solution, carries out mechanical stirring and ultrasound
5min；
3) method for using filters pressing, makes the carbon fiber being dispersed in colloidal sol mutually be overlapped to form three-dimensional porous carbon fiber skeleton；
4) porous carbon fiber skeleton is placed in 80 DEG C of baking ovens, isothermal holding 6 hours；
5) 1600 DEG C are risen in the nitrogen that pressure is 1Mpa, isothermal holding 3h generates a large amount of nitrogen in carbon fiber skeleton
SiClx nanofiber, furnace cooling；
6) 650 DEG C, isothermal holding 5h are risen in air with the heating rate of 1 DEG C/min, oxidation removal carbon fiber obtains
Nitrogenize silica aerogel.
The method of the present invention preparation nitridation silica aerogel is not related to costly, time consuming, inefficient needed for traditional aeroge preparation
Drying equipment, it is only necessary to common gas pressure sintering furnace and air furnace can meet preparation and require, and raw material is simple, at low cost, nothing
A large amount of solvent need to be consumed, preparation process is simple, and the period is the 1/8~1/5 of conventional method, significantly reduces the system of aeroge
Standby period and cost, while yield is greatly improved.
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 (8)
1. a kind of preparation method of silicon nitride nano with aeroge, which comprises the following steps:
1) it prepares polysiloxanes colloidal sol: after siloxane sol, water and dehydrated alcohol are mixed, polysiloxanes colloidal sol is made；
2) it prepares slurry: chopped carbon fiber being dispersed in polysiloxanes colloidal sol made from step 1), carbon fiber surface is made
Coat one layer of siloxane sol；
3) it forms: constructing the three-dimensional porous carbon fiber skeleton for mutually overlapping formation by the chopped carbon fiber of siloxane sol bonding；
4) solidify and crack: three-dimensional porous carbon fiber skeleton is heated to the solidification temperature of polysiloxanes colloidal sol, isothermal holding 4~
8h, is warming up to 1200 DEG C~1700 DEG C in nitrogen atmosphere, and 1~3h of isothermal holding cools to room temperature with the furnace, obtains carbon fiber
Dimension/silicon nitride nano fiber composite block；
5) it removes carbon: carbon fiber/silicon nitride nano fiber composite block is heated to 400 DEG C~1000 DEG C in air, and kept the temperature
1~8h is handled, silicon nitride nano band aeroge is obtained.
2. preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that in step 1), with
Mass percent meter, comprising: 10%~70% siloxane sol, 10%~50% water and 10%~80% anhydrous second
Alcohol；And siloxane sol uses methyltrimethoxysilane and/or dimethyldimethoxysil,ne.
3. preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that in step 2), institute
It is 0.5mm~2mm with chopped carbon fiber average length.
4. preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that step 3) is using true
Empty suction method or filter press technique remove unreacted siloxane sol, make chopped carbon fiber formed by polysiloxanes it is sol bonded three
Tie up porous carbon fiber skeleton.
5. preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that in step 4), gather
The solidification temperature of siloxane sol is 80~120 DEG C, and nitrogen pressure is 0.1~2MPa, and heating rate is 2~10 DEG C/min.
6. preparation method of the silicon nitride nano according to claim 1 with aeroge, which is characterized in that in step 5),
400~1000 DEG C are risen in air with the heating rate of 1 DEG C~10 DEG C/min.
7. preparation method of the silicon nitride nano described according to claim 1~any one of 6 with aeroge, feature exist
In, intensity of the silicon nitride nano with aeroge and density are adjustable, it is embodied in:
By changing the solubility or crosslinking degree of siloxane sol, regulate and control intensity and density of the silicon nitride nano with aeroge；
Alternatively, regulating and controlling intensity and density of the silicon nitride nano with aeroge by the average length for changing chopped carbon fiber；
Alternatively, regulating and controlling silicon nitride nano band gas by the retention amount for changing polysiloxanes colloidal sol in three-dimensional porous carbon fiber skeleton
The intensity and density of gel；
Alternatively, regulating and controlling intensity and density of the silicon nitride nano with aeroge by control nitrogen pressure.
8. using silicon nitride nano band aeroge, feature made from preparation method described in any one of claim 1~7
It is, density of the silicon nitride nano with aeroge is 5mg/cm3~50mg/cm3, thermal conductivity be 0.030W/mK~
0.051W/mK, silicon nitride nano strip length are 100 μm~500 μm, and width is 0.2~3 μm.
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