CN108689679A - A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material - Google Patents
A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high temperature resistant gradient fiber composite aerogel heat-insulating material, with cheap Ludox, alumina sol is as silicon source and silicon source, with inorganic glass fibre, alumina silicate fibre, alumina fibre etc. is used as aerogel structure reinforcement, with absolute ethyl alcohol, deionized water is as solvent, in conjunction with acidic catalyst, it is mixed according to a certain percentage, pass through sol-gel, the methods of aging and solvent displacement, prepare gradient fiber composite alcogel, again by simple, processing is dried to sample in the boulton process of low cost, finally obtain gradient fiber composite aeroge, the present invention is simple, it is at low cost, prepared composite material has high temperature resistant, high porosity, the features such as high-specific surface area.
Description
Technical field
The invention belongs to technical fields prepared by, high temperature resistant inorganic nano material heat-insulated with high efficiency gradient, more particularly to
A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material.
Background technology
Aeroge is mutually to coalesce the one kind constituted by colloidal particle or high-polymer molecular to have three-dimensional manometer network structure,
It is a kind of novel nano-porous materials.It is with high specific surface area, high porosity, low-refraction, extremely-low density, superpower suction
The features such as attached property, so being all with a wide range of applications in calorifics, optics, electricity, acoustics etc..In terms of calorifics, gas
The nanoporous network structure of gel can effectively inhibit the gentle phase heat transfer of solid phase heat transfer, have excellent heat insulation characteristics, be
The current minimum solid-state material of thermal conductivity in the world has wide answer in fields such as space flight and aviation, chemical industry metallurgical, energy saving buildings
Use foreground.
According to the SiO of existing domestic and international, traditional unitary system2Aerogel heat-insulating material has many excellent spies
Sign, but temperature in use steady in a long-term is only limited to 650 DEG C hereinafter, constraining SiO significantly2The application range of aerogel material.Research
Show Al2O3Aeroge is having stable molding and structural strength is big, and temperature tolerance is up to 1000 DEG C or more, but heat insulation is wanted
Compare SiO2Aerogel material is less better.It is well known that the intensity of the oxide silica aerogels such as pure silicon substrate, aluminium base is very low,
The sample of bulk can not be prepared, and be difficult to be machined, be molded, and large-scale application is difficult to realize.Therefore it is necessary to using
The reinforcing materials such as fiber carry out structure enhancing to pure nanoporous aerogel.So with alumina fibre REINFORCED Al2O3Aeroge is made
High temperature heat source, glass fiber reinforcement SiO are resisted for high-temperature-resistant layer2Aeroge is as effectively insulating layer, in order to preferably solve boundary
Face combines problem, and self-healing transition zone alumina silicate fibre in interface is inserted between both enhances SiO2/Al2O3Compound airsetting
Glue, forms complete integrated gradient fiber composite aerogel heat-insulating material, the composite material not only can with high temperature resistant, but also
Best heat insulation can be reached, there is great scientific research value and extensive actual application prospect.
Invention content
The purpose of the invention is to design a kind of novel fiber composite aeroge system, enhanced using alumina fibre
Al2O3Aeroge resists high temperature heat source, glass fiber reinforcement SiO as high-temperature-resistant layer2Aeroge is intermediate as effectively insulating layer
SiO is enhanced using interface self-healing transition zone alumina silicate fibre2/Al2O3Composite aerogel solves the problems, such as interface cohesion, provides one
Kind with high temperature resistant, it is easily molded processing, effectively insulating effect high temperature resistant gradient fiber composite aerogel heat-insulating material preparation
Method.
The technical scheme is that:A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material, tool
Steps are as follows for body:A kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material, is as follows:
(1) by Ludox, absolute ethyl alcohol, deionized water by volume 1:(0.5~2.0):(0.1~1.0) it is uniformly mixed
30~60min is mixed at 45~50 DEG C, obtains clear SiO for wiring solution-forming2Sol solution continuously adds acidity and urges
Agent, it is 4~6 to adjust solution ph, then sol solution is impregnated in the glass fibre in grinding tool, diaphragm seal, and is placed
3~6h in 50~60 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, will
Fiber composite wet gel A takes out together with grinding tool, and alumina silicate fibre is placed on surface on it;
(2) by Ludox, alumina sol, absolute ethyl alcohol, deionized water by volume 1:(0.2~5):(0.5~
3.0):(0.2~2.0) it is uniformly mixed wiring solution-forming, 30~60min is mixed at 45~50 DEG C, continuously adds acidity and urges
Agent, it is 4~6 to adjust solution ph, obtains clear SiO2-Al2O3Sol solution, by the SiO2-Al2O3Sol solution is slow
It is impregnated in the alumina silicate fibre in step (1) grinding tool, diaphragm seal, and is placed on 2~5h in 50~60 DEG C of vacuum drying chambers,
Fiber composite wet gel A-B is obtained and be denoted as, fiber composite wet gel A-B is taken out together with grinding tool, and surface is put on it
Set alumina fibre;
(3) by alumina sol, absolute ethyl alcohol, deionized water by volume 1:(0.1~1.0):(0.2~2.0) it mixes
30~60min is mixed in uniform wiring solution-forming at 45~50 DEG C, continuously adds acidic catalyst, and it is 4 to adjust solution ph
~6, obtain clear Al2O3Sol solution, by the Al2O3Sol solution is slowly impregnated in the fibre of the aluminium oxide in step (2) grinding tool
In dimension, diaphragm seal, and be placed on 1~3h in 60~65 DEG C of vacuum drying chambers, obtain and be denoted as fiber composite wet gel A-B-
C takes out fiber composite wet gel A-B-C, room temperature together with grinding tool, and Ageing solution is added, and is carried out to the compound wet gel
Burin-in process obtains the gradient fiber composite wet gel after aging;
(4) organic solvent is added into step (3) mold and solvent displacement is carried out to gradient fiber composite wet gel, obtain ladder
Spend fiber composite alcogel;
(5) processing is dried in the gradient fiber composite alcogel replaced in step (4), obtains gradient fiber composite
Aeroge;
(6) the gradient fiber composite aeroge in step (5) is subjected to high-temperature heat treatment, it is fine obtains a kind of high temperature resistant gradient
Tie up composite aerogel heat-barrier material.
Silica dioxide granule size is 10~20nm, SiO in Ludox described in preferred steps (1) and (2)2Quality
Content is 20~45%.
Alumina sol described in preferred steps (2) and (3) is positively charged featheriness nano aluminium oxide micelle point
Dissipate colloidal solution in water;Granular size is 10~20nm, large specific surface area, Al2O3Mass content be 20~30%.
Acidic catalyst described in preferred steps (1), (2) and (3) is one kind in hydrochloric acid, nitric acid or perchloric acid.
Ageing solution described in preferred steps (3) is tetraethyl orthosilicate, positive quanmethyl silicate, aluminium secondary butylate or isopropanol
One or two kinds of or more mixed solution in aluminium.
Organic solvent described in preferred steps (4) is one kind in ethyl alcohol, methanol or acetone.
Solvent is replaced into every 12~replaces an organic solvent for 24 hours in preferred steps (4), replaces 3~5 times altogether.
Drying process described in preferred steps (5) is:Boulton process, drying temperature be gradient control temperature-raising method, 45
~55 DEG C, drying time is 3~8h;60~70 DEG C, drying time is 5~15h;100~120 DEG C, drying time is 2~5h.
High-temperature heat treatment process described in preferred steps (6) is:Under aerobic conditions, heat treatment temperature is 300~500
DEG C, heat treatment time is 1~3h.
The pure SiO of document report2Aerogel material maximum operation (service) temperature is only 650 DEG C, SiO at this temperature2Airsetting collagen
Some three-dimensional net structures almost cave in, and specific surface area is down to 50m2/ g loses airsetting glue material hereinafter, porosity is extremely low
The heat insulation and preservation effect of material.And gradient fiber composite aerogel heat-insulating material is surveyed under aerobic conditions by coldface temperature instrument
Examination, 1200 DEG C of heat sources are in direct contact alumina fibre REINFORCED Al2O3Aeroge, testing time 5h, as a result, it has been found that:The gradient fiber
Aerogel composite structure keeps complete, has good heat-resisting quantity and heat insulation.Wherein, thermal conductivity is less than at 25 DEG C
0.05W/mK, thermal conductivity is less than 0.1W/mK when 800 DEG C of hot face, and thermal conductivity is 0.2W/mK, hot face when 1000 DEG C of hot face
Thermal conductivity is less than 0.3W/mK at 1200 DEG C.
Advantageous effect:
1, the present invention is prepared for gradient fiber composite aerogel heat-insulating material using vacuum drying technique.First by simple
Sol-gel method prepare fiber composite wet gel, recycle the technologies such as inexpensive vacuum drying, high-temperature heat treatment to prepare
High temperature resistant, easily molded processing gradient fiber composite aerogel heat-insulating material.
2, apply more and heat insulation it is still further preferred that silica-based aerogel, thermal conductivity can be down to 0.016W/ in heat-insulated field
MK, but temperature is used for a long time and is no more than 650 DEG C, and the aeroges such as aluminium base have 1000~1200 DEG C of high temperature resistant, but heat-insulated effect
Fruit is not as good as silica-based aerogel.So the present invention is with alumina fibre REINFORCED Al2O3High temperature resistant face of the aeroge as heat-barrier material,
The temperature tolerance for improving composite aerogel enhances SiO with alumina silicate fibre2/Al2O3Composite aerogel is as interface self-healing transition
Layer, not only solves interface cohesion problem, and the transition zone that the heat for playing the role of composite aerogel is transmitted, more so that glass
Glass fiber reinforcement SiO2Aeroge plays efficient thermal insulation layer effect.Therefore, the invention is improving making for fiber composite aeroge
There is great researching value and application prospect with temperature and heat insulation aspect.
Description of the drawings
Fig. 1 is the SEM photograph of the gradient fiber composite aeroge prepared by embodiment 1.
Specific implementation mode
Example 1
By Ludox (SiO2Granular size is 10nm, content 20wt%), absolute ethyl alcohol, deionized water by volume 1:
0.5:0.1 uniformly mixed wiring solution-forming, 30min is mixed at 45 DEG C, obtains clear SiO2Sol solution continuously adds
Hydrochloric acid, it is 4 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed on
3h in 50 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, takes out grinding tool, and
Alumina silicate fibre is placed on surface on it;Continue Ludox (SiO2Granular size is 10nm, content 20wt%), aluminium oxide
Colloidal sol (Al2O3Granular size is 10nm, content 20wt%), absolute ethyl alcohol, deionized water by volume 1:0.2:
0.5:0.2 uniformly mixed wiring solution-forming, 30min is mixed at 45 DEG C, continuously adds hydrochloric acid, and it is 4 to adjust solution ph, will
The SiO2/Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and is placed on 50 DEG C
2h in vacuum drying chamber obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and aluminium oxide fibre is placed on surface on it
Dimension;Again by alumina sol (Al2O3Granular size is 10nm, content 20wt%), absolute ethyl alcohol, deionized water by volume
By volume 1:0.1:0.2 uniformly mixed wiring solution-forming, 30min is mixed at 45 DEG C, continuously adds hydrochloric acid, adjusts solution
PH value is 4, by the Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal, and is placed
The 1h in 60 DEG C of vacuum drying chambers, obtains gradient fiber composite wet gel A-B-C, and room temperature is old with tetraethyl orthosilicate
Change liquid, burin-in process is carried out to the compound wet gel, it is primary per replacing for 24 hours, it replaces 3 times, it is multiple to obtain the gradient fiber after aging
Close wet gel.Into mold, alcohol solvent is added in sample again, and solvent is replaced 3 times, every time for 24 hours, finally obtains gradient fiber composite
Alcogel.Gradient fiber composite alcogel is put into vacuum drying chamber progress gradient increased temperature drying again, using 45 DEG C of dry 3h,
Gradient fiber composite aeroge is made in 60 DEG C of dry 10h, 100 DEG C of dry 5h, and 1h is heat-treated at 500 DEG C by high temperature, final to obtain
To gradient fiber composite aerogel heat-insulating material.The SEM photograph of prepared gradient fiber composite aeroge is as shown in Figure 1.Through
It crosses characterization to find, thermal conductivity is 0.043W/mK at 25 DEG C of the composite aerogel, and thermal conductivity is 0.086W/ when 800 DEG C of hot face
MK, thermal conductivity is 0.164W/mK when 1000 DEG C of hot face, and thermal conductivity is 0.273W/mK when 1200 DEG C of hot face.
Example 2
By Ludox (SiO2Granular size is 20nm, content 45wt%), absolute ethyl alcohol, deionized water by volume 1:
2:1 uniformly mixed wiring solution-forming, 60min is mixed at 50 DEG C, obtains clear SiO2Sol solution continuously adds salt
Acid, it is 6 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed on 60
6h in DEG C vacuum drying chamber, obtains glass fibre composite S iO2Wet gel, is denoted as fiber composite wet gel A, takes out grinding tool, and
Place alumina silicate fibre in its upper surface;Continue Ludox (SiO2Granular size is 20nm, content 45wt%), aluminium oxide it is molten
Glue (Al2O3Granular size is 20nm, content 30wt%), absolute ethyl alcohol, deionized water by volume 1:5:3:2
It is uniformly mixed wiring solution-forming, 60min is mixed at 50 DEG C, continuously adds hydrochloric acid, it is 6 to adjust solution ph, by the SiO2/
Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and it is dry to be placed on 60 DEG C of vacuum
5h in dry case obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and alumina fibre is placed on surface on it;Again will
Alumina sol (Al2O3Granular size is 20nm, content 30wt%), absolute ethyl alcohol, deionized water by volume
1:1:2 uniformly mixed wiring solution-formings, 60min is mixed at 50 DEG C, continuously adds hydrochloric acid, and it is 6 to adjust solution ph, by this
Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal, and it is dry to be placed on 65 DEG C of vacuum
3h in dry case, obtains gradient fiber composite wet gel A-B-C, and room temperature is molten with tetraethyl orthosilicate and aluminium secondary butylate mixing
Liquid is Ageing solution, carries out burin-in process to the compound wet gel, is replaced per 12h once, replace 5 times, obtain the gradient after aging
Fiber composite wet gel.Into mold, alcohol solvent is added in sample again, and solvent is replaced 5 times, each 12h, finally obtains gradient fibre
Tie up compound alcogel.Gradient fiber composite alcogel is put into progress gradient increased temperature drying in vacuum drying chamber again, using 55 DEG C
Dry 8h, 70 DEG C of dry 5h, 120 DEG C of dry 2h, are made gradient fiber composite aeroge, and 3h are heat-treated at 300 DEG C by high temperature,
Finally obtain gradient fiber composite aerogel heat-insulating material.It is found by characterization, thermal conductivity is at 25 DEG C of the composite aerogel
0.046W/mK, thermal conductivity is 0.091W/mK when 800 DEG C of hot face, and thermal conductivity is 0.169W/mK, heat when 1000 DEG C of hot face
Thermal conductivity is 0.282W/mK when 1200 DEG C of face.
Example 3
By Ludox (SiO2Granular size is 15nm, content 30wt%), absolute ethyl alcohol, deionized water by volume 1:
1:0.5 uniformly mixed wiring solution-forming, 50min is mixed at 45 DEG C, obtains clear SiO2Sol solution continuously adds nitre
Acid, it is 5 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed on 55
4h in DEG C vacuum drying chamber, obtains glass fibre composite S iO2Wet gel, is denoted as fiber composite wet gel A, takes out grinding tool, and
Place alumina silicate fibre in its upper surface;Again by Ludox (SiO2Granular size is 15nm, content 30wt%), alumina sol
(Al2O3Granular size is 15nm, content 25wt%), absolute ethyl alcohol, deionized water by volume 1:1:1:1 is mixed
Uniform wiring solution-forming is closed, 60min is mixed at 50 DEG C, continuously adds nitric acid, it is 5 to adjust solution ph, by the SiO2/
Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and it is dry to be placed on 50 DEG C of vacuum
3h in dry case obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and alumina fibre is placed on surface on it;Again will
Alumina sol (Al2O3Granular size is 15nm, content 25wt%), absolute ethyl alcohol, deionized water by volume
1:0.5:1 uniformly mixed wiring solution-forming, 45min is mixed at 50 DEG C, continuously adds nitric acid, and it is 5 to adjust solution ph, will
The Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal, and is placed on 60 DEG C of vacuum
2h in drying box, obtains gradient fiber composite wet gel A-B-C, room temperature, with the mixed of positive quanmethyl silicate and aluminium isopropoxide
Conjunction solution is Ageing solution, carries out burin-in process to the compound wet gel, replaces once, replace 4 times, after obtaining aging per 18h
Gradient fiber composite wet gel.Into mold, methanol solvate is added in sample again, and solvent is replaced 4 times, and each 18h finally obtains ladder
Spend fiber composite alcogel.Gradient fiber composite alcogel is put into progress gradient increased temperature drying in vacuum drying chamber again, is used
Gradient fiber composite aeroge is made in 50 DEG C of dry 5h, 65 DEG C of dry 15h, 110 DEG C of dry 3h, by 400 DEG C of heat of high temperature
2h is managed, gradient fiber composite aerogel heat-insulating material is finally obtained.It is found by characterization, thermal conductivity at 25 DEG C of the composite aerogel
Rate is 0.044W/mK, and thermal conductivity is 0.085W/mK when 800 DEG C of hot face, and thermal conductivity is 0.175W/m when 1000 DEG C of hot face
K, thermal conductivity is 0.277W/mK when 1200 DEG C of hot face.
Example 4
By Ludox (SiO2Granular size is 12nm, content 25wt%), absolute ethyl alcohol, deionized water by volume 1:
1.5:0.8 uniformly mixed wiring solution-forming, 40min is mixed at 45 DEG C, obtains clear SiO2Sol solution continuously adds
Nitric acid, it is 6 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed on
5h in 55 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, takes out grinding tool, and
Alumina silicate fibre is placed on surface on it;Again by Ludox (SiO2Granular size is 12nm, content 25wt%), aluminium oxide it is molten
Glue (Al2O3Granular size is 12nm, content 23wt%), absolute ethyl alcohol, deionized water by volume 1:2:1.5:
1.5 uniformly mixed wiring solution-formings, 50min is mixed at 50 DEG C, continuously adds nitric acid, and it is 6 to adjust solution ph, by this
SiO2/Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and is placed on 50 DEG C very
4h in empty drying box obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and alumina fibre is placed on surface on it;
Again by alumina sol (Al2O3Granular size is 12nm, content 23wt%), absolute ethyl alcohol, deionized water press body by volume
Product ratio 1:0.8:0.6 uniformly mixed wiring solution-forming, 60min is mixed at 45 DEG C, continuously adds nitric acid, adjusts solution ph
It is 6, by the Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal, and is placed on 65
1.5h in DEG C vacuum drying chamber, obtains gradient fiber composite wet gel A-B-C, room temperature is right using aluminium secondary butylate as Ageing solution
The compound wet gel carries out burin-in process, and primary, replacement 4 times is replaced per 20h, and it is wet solidifying to obtain the gradient fiber composite after aging
Glue.Into mold, methanol solvate is added in sample again, and solvent is replaced 3 times, every time for 24 hours, finally obtains gradient fiber composite alcogel.
Gradient fiber composite alcogel is put into progress gradient increased temperature drying in vacuum drying chamber again, using 48 DEG C of dry 6h, 60 DEG C dry
Gradient fiber composite aeroge is made in dry 12h, 120 DEG C of dry 4h, by 350 DEG C of heat treatment 3h of high temperature, finally obtains gradient
Fiber composite aerogel heat-insulating material.It being found by characterization, thermal conductivity is 0.048W/mK at 25 DEG C of the composite aerogel,
Thermal conductivity is 0.097W/mK when 800 DEG C of hot face, and thermal conductivity is 0.178W/mK when 1000 DEG C of hot face, heat when 1200 DEG C of hot face
Conductance is 0.285W/mK.
Example 5
By Ludox (SiO2Granular size is 18nm, content 40wt%), absolute ethyl alcohol, deionized water by volume 1:
0.9:0.6 uniformly mixed wiring solution-forming, 30min is mixed at 45 DEG C, obtains clear SiO2Sol solution continuously adds
Perchloric acid, it is 4 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed
The 3h in 55 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, takes out grinding tool,
And alumina silicate fibre is placed on surface on it;Again by Ludox (SiO2Granular size is 18nm, content 40wt%), aluminium oxide
Colloidal sol (Al2O3Granular size is 18nm, content 28wt%), absolute ethyl alcohol, deionized water by volume 1:4:
2.5:1.6 uniformly mixed wiring solution-formings, 40min is mixed at 50 DEG C, continuously adds perchloric acid, and it is 5 to adjust solution ph,
By the SiO2/Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and is placed on 55
3h in DEG C vacuum drying chamber obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and aluminium oxide is placed on surface on it
Fiber;Again by alumina sol (Al2O3Granular size is 18nm, content 28wt%), absolute ethyl alcohol, deionized water press volume
Than by volume 1:0.4:1.2 uniformly mixed wiring solution-formings, 60min is mixed at 45 DEG C, continuously adds perchloric acid, is adjusted
Solution ph is 5, by the Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal, and
It is placed on 1.5h in 65 DEG C of vacuum drying chambers, obtains gradient fiber composite wet gel A-B-C, room temperature, with positive silicic acid tetrem
The mixed solution of ester and aluminium isopropoxide is Ageing solution, carries out burin-in process to the compound wet gel, is replaced per 15h once, replace 5
It is secondary, obtain gradient fiber composite wet gel, then sample is added acetone solvent into mold, solvent replaces 4 times, each 20h, finally
Obtain gradient fiber composite alcogel.Gradient fiber composite alcogel progress gradient increased temperature in vacuum drying chamber is put into again to do
It is dry, using 50 DEG C of dry 7h, 70 DEG C of dry 7h, 100 DEG C of dry 4h, gradient fiber composite aeroge is made, is passing through high temperature 450
DEG C heat treatment 2h, finally obtain gradient fiber composite aerogel heat-insulating material.It is found by characterization, 25 DEG C of the composite aerogel
Lower thermal conductivity is 0.046W/mK, and thermal conductivity is 0.091W/mK when 800 DEG C of hot face, and thermal conductivity is when 1000 DEG C of hot face
0.181W/mK, thermal conductivity is 0.295W/mK when 1200 DEG C of hot face.
Example 6
By Ludox (SiO2Granular size is 16nm, content 28wt%), absolute ethyl alcohol, deionized water by volume 1:
1.4:0.7 uniformly mixed wiring solution-forming, 60min is mixed at 45 DEG C, obtains clear SiO2Sol solution continuously adds
Perchloric acid, it is 5 to adjust solution ph, then sol solution is impregnated in the glass mat in grinding tool, diaphragm seal, and is placed
The 4h in 55 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, takes out grinding tool,
And alumina silicate fibre is placed on surface on it;Again by Ludox (SiO2Granular size is 16nm, content 28wt%), aluminium oxide
Colloidal sol (Al2O3Granular size is 16nm, content 22wt%), absolute ethyl alcohol, deionized water by volume 1:3.5:
2.5:1.8 uniformly mixed wiring solution-formings, 30min is mixed at 50 DEG C, continuously adds perchloric acid, and it is 5 to adjust solution ph,
By the SiO2/Al2O3Sol solution is slowly impregnated in the alumina silicate fiber felt in above-mentioned grinding tool, diaphragm seal, and is placed on 60
4.5h in DEG C vacuum drying chamber obtains and is denoted as fiber composite wet gel A-B, takes out grinding tool, and oxidation is placed on surface on it
Aluminum fiber;Again by alumina sol (Al2O3Granular size is 16nm, content 22wt%), absolute ethyl alcohol, deionized water press body
Product is than by volume 1:0.3:1.2 uniformly mixed wiring solution-formings, 50min is mixed at 50 DEG C, continuously adds perchloric acid, is adjusted
It is 4 to save solution ph, by the Al2O3Sol solution is slowly impregnated in the alumina fiber blanket in above-mentioned grinding tool, diaphragm seal,
And it is placed on 2h in 50 DEG C of vacuum drying chambers, obtain gradient fiber composite wet gel A-B-C, room temperature, with positive silicic acid tetramethyl
The mixed solution of ester and aluminium secondary butylate is Ageing solution, carries out burin-in process to the compound wet gel, is replaced per 20h once, replace 3
It is secondary, obtain the gradient fiber composite wet gel after aging.The sample addition acetone solvent into mold again, solvent displacement 5 times, every time
15h finally obtains gradient fiber composite alcogel.Gradient fiber composite alcogel is put into vacuum drying chamber again and carries out gradient
Heat up drying, using 55 DEG C of dry 4h, 65 DEG C of dry 12h, 120 DEG C of dry 2h, gradient fiber composite aeroge is made, is passing through
380 DEG C of heat treatment 2.5h of high temperature, finally obtain gradient fiber composite aerogel heat-insulating material.It is found by characterization, the compound gas
Thermal conductivity is 0.047W/mK at 25 DEG C of gel, and thermal conductivity is 0.088W/mK when 800 DEG C of hot face, heat when 1000 DEG C of hot face
Conductance is 0.176W/mK, and thermal conductivity is 0.289W/mK when 1200 DEG C of hot face.
Claims (9)
1. a kind of preparation method of high temperature resistant gradient fiber composite aerogel heat-insulating material, is as follows:
(1) by Ludox, absolute ethyl alcohol, deionized water by volume 1:(0.5~2.0):(0.1~1.0) it is uniformly mixed and is made into
30~60min is mixed at 45~50 DEG C, obtains clear SiO for solution2Sol solution continuously adds acidic catalyst,
It is 4~6 to adjust solution ph, then sol solution is impregnated in the glass fibre in grinding tool, diaphragm seal, and it is placed on 50~
3~6h in 60 DEG C of vacuum drying chambers obtains glass fibre composite S iO2Wet gel is denoted as fiber composite wet gel A, fiber is answered
It closes wet gel A to take out together with grinding tool, and alumina silicate fibre is placed on surface on it;
(2) by Ludox, alumina sol, absolute ethyl alcohol, deionized water by volume 1:(0.2~5):(0.5~3.0):
(0.2~2.0) it is uniformly mixed wiring solution-forming, 30~60min is mixed at 45~50 DEG C, continuously adds acidic catalyst,
It is 4~6 to adjust solution ph, obtains clear SiO2-Al2O3Sol solution, by the SiO2-Al2O3Sol solution is impregnated in step
Suddenly in the alumina silicate fibre in (1) grinding tool, sealing, and it is placed on 2~5h in 50~60 DEG C of vacuum drying chambers, it obtains and is denoted as fibre
Compound wet gel A-B is tieed up, fiber composite wet gel A-B is taken out together with grinding tool, and alumina fibre is placed on surface on it;
(3) by alumina sol, absolute ethyl alcohol, deionized water by volume 1:(0.1~1.0):(0.2~2.0) it is uniformly mixed
30~60min is mixed in wiring solution-forming at 45~50 DEG C, continuously adds acidic catalyst, and it is 4~6 to adjust solution ph,
Obtain clear Al2O3Sol solution, by the Al2O3Sol solution is slowly impregnated in the alumina fibre in step (2) grinding tool
In, diaphragm seal, and it is placed on 1~3h in 60~65 DEG C of vacuum drying chambers, fiber composite wet gel A-B-C is obtained and is denoted as,
Fiber composite wet gel A-B-C is taken out together with grinding tool, is placed, Ageing solution is added, which is carried out at aging
Reason, obtains the gradient fiber composite wet gel after aging;
(4) organic solvent is added into step (3) mold and solvent displacement is carried out to gradient fiber composite wet gel, obtain gradient fibre
Tie up compound alcogel;
(5) processing is dried in the gradient fiber composite alcogel replaced in step (4), obtains gradient fiber composite airsetting
Glue;
(6) the gradient fiber composite aeroge in step (5) is subjected to high-temperature heat treatment, it is multiple obtains a kind of high temperature resistant gradient fiber
Close aerogel heat-insulating material.
2. preparation method according to claim 1, it is characterised in that dioxy in the Ludox described in step (1) and (2)
Silicon carbide particle size is 10~20nm, SiO2Mass content be 20~45%.
3. preparation method according to claim 1, it is characterised in that the alumina sol described in step (2) and (3) is
The colloidal solution that positively charged featheriness nano aluminium oxide micelle is dispersed in water;Granular size is 10~20nm, specific surface
Product is big, Al2O3Mass content be 20~30%.
4. preparation method according to claim 1, it is characterised in that the acidic catalyst described in step (1), (2) and (3)
Agent is one kind in hydrochloric acid, nitric acid or perchloric acid.
5. preparation method according to claim 1, it is characterised in that the Ageing solution described in step (3) is positive silicic acid tetrem
One or two kinds of or more mixed solution in ester, positive quanmethyl silicate, aluminium secondary butylate or aluminium isopropoxide.
6. preparation method according to claim 1, it is characterised in that the organic solvent described in step (4) is ethyl alcohol, first
One kind in alcohol or acetone.
7. preparation method according to claim 1, it is characterised in that in step (4) solvent be replaced into every 12~replace for 24 hours
Organic solvent is replaced 3~5 times altogether.
8. preparation method according to claim 1, it is characterised in that the drying process described in step (5) is:Vacuum is dry
Dry method, drying temperature are that gradient controls temperature-raising method, and 45~55 DEG C, drying time is 3~8h;60~70 DEG C, drying time be 5~
15h;100~120 DEG C, drying time is 2~5h.
9. preparation method according to claim 1, it is characterised in that the high-temperature heat treatment process described in step (6) is:
Heat treatment temperature is 300~500 DEG C, and heat treatment time is 1~3h.
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