CN110498691A - A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology - Google Patents
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology Download PDFInfo
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Abstract
The silicon based ceramic aeroge preparation process based on ceramic sintering technology that the invention discloses a kind of, including weighing following raw material: 10-15 parts of ethyl orthosilicates, 50-65 parts of deionized waters, 50-70 parts of dehydrated alcohols, 15-20 parts of zirconium oxychlorides, 10-12 parts of zirconium nitrates, 3-5 parts of sodium fluorides, 3-8 parts of silica, 5-8 parts of silicon nitrides, 30-50 parts of glycerol and 50-70 parts of trim,ethylchlorosilanes；It is replaced by glycerol and trim,ethylchlorosilane, the network structure of gel can be enhanced, in the capillary for reducing gel network simultaneously, it can effectively avoid that gel is caused to generate collapsing during suction filtration, it is generally poor to solve the mechanical properties such as the aeroge intensity obtained after drying and toughness, heat treatment temperature is excessively high, and nanoscale hole hole will occur to collapse and aeroge is caused to densify completely, and aeroge stomata easily collapses broken technical problem.
Description
Technical field
The invention belongs to aeroge preparation field, specially a kind of silicon based ceramic aeroge system based on ceramic sintering technology
Standby technique.
Background technique
Porous material is since it has the characteristics that light weight, large specific surface area, thermal coefficient are small, world in recent years model
Extensive research boom has been started in enclosing.Studies have shown that in the case where not changing configuration state, the porosity of porous material
It is bigger, aperture is smaller, heat-proof quality is more excellent.
Porous material includes aeroge, porous ceramics, porous metals etc..Aerogel material has high porosity, and
And its aperture size is minimum, it is most of within nano-scale range.Because aeroge These characteristics, heat-proof quality are excellent
It is different, or even it is referred to as super insulating material.Aeroge is dried by wet gel and is obtained, the aeroge intensity that obtains after dry and tough
Property etc. mechanical properties it is generally poor, the mechanical property of aeroge can preferably be improved by carrying out heat treatment at a certain temperature.But
It is that heat treatment temperature is usually no more than 500 DEG C, if heat treatment temperature is excessively high, nanoscale hole hole will occur to collapse and lead to gas
Gel densifies completely.Therefore cause the use temperature of aeroge not high, even across heat treatment, its use temperature is also difficult
More than 1000 DEG C, and aerogel product mechanical property is bad, and stomata easily collapses broken under external force.
Chinese invention patent CN102910926A discloses a kind of system of high-temperature resistant silicon carbide aerogel heat-insulation
Preparation Method.The high-temperature resistant silicon carbide aerogel composite is a kind of by alumina silicate fiber felt and carbonization silica aerogel structure
At can be with the heat-barrier material of resistance to 1200 °C of high temperature in air atmosphere.Preparation method be benzenediol, formaldehyde, silicon source, water,
Ethyl alcohol is uniformly mixed, and by sol-gel, aging and is dried to obtain fiber reinforcement carbon-silicon compound aerogel fiber reinforcement carbon-silicon
Composite aerogel carries out carbothermic reduction reaction under protection of argon gas, and then calcining obtains fiber reinforced high-temperature-resistant carbon in air
SiClx aerogel heat-proof composite material.
Summary of the invention
In order to overcome above-mentioned technical problem, the present invention provides a kind of silicon based ceramic aeroge based on ceramic sintering technology
Preparation process.
The technical problems to be solved by the invention:
(1) mechanical properties such as the aeroge intensity and toughness that obtain after drying are generally poor, and heat treatment temperature is excessively high, nano grade pore
Hole will occur to collapse and aeroge is caused to densify completely, and aeroge stomata easily collapses and is crushed；
(2) in prior art preparation aerogel process, aeroge skeleton surface does not have hydrophobicity, and between skeleton and solvent
Contact angle it is smaller, cause the additonal pressure of capillary larger, and the process of gelation is slower.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, includes the following steps:
Step S1, following raw material: 10-15 parts of ethyl orthosilicates, 50-65 parts of deionized waters, 50-70 parts of anhydrous second are weighed
Alcohol, 15-20 parts of zirconium oxychlorides, 10-12 parts of zirconium nitrates, 3-5 parts of sodium fluorides, 3-8 parts of silica, 5-8 parts of silicon nitrides, 30-50 parts
Glycerol and 50-70 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide of mass fraction is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, mass fraction is added
10% dilute hydrochloric acid adjusts pH, until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with
The revolving speed magnetic agitation of 150r/min, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Hydroxide ion and silicon ion or silicon ion group hydroxylating in step S1 in zirconium oxychloride form eight-coordinate body, it
Zirconium ion forms eight-coordinate body in acid condition afterwards, latter two eight-coordinate body mutually with apex angle be connected, dehydration crystallization, formed
Zirconium oxide octahedron and silicon-oxygen tetrahedron, are interconnected to form zirconium silicate；Joined sodium fluoride, fluorine ion can replace oxygen from
Son forms Zr-F key and Si-F key, can reduce the crystallization potential barrier of zirconium silicate, and then accelerates zirconium silicate crystallization, and manufactured glue
Body particle is smaller, and total surface area is big, and activity is higher than sediment, is advantageously implemented crystal growth and can reduce reaction temperature and shortening
Reaction time;It is replaced in step S3 by glycerol and trim,ethylchlorosilane, the network structure of gel can be enhanced, subtracted simultaneously
It in the capillary of small gel network, can effectively avoid that gel is caused to generate collapsing during suction filtration.
Further, the process of constant pressure and dry includes the following steps: in step S2
(1) formamide and propylene oxide are added into presoma, is transferred in 50 DEG C of insulating boxs, aging 20h is warming up to 65 DEG C,
And with soaked in absolute ethyl alcohol, 12h, every 4h change a not good liquor, then at 70 DEG C with impregnating 2h, Zhi Houyong in 80% ethanol water
Dehydrated alcohol washs three times；
(2) it is added after the completion of washing in the mixed solution of ethyl orthosilicate and 80% ethanol water and impregnates 8h, every 2h is changed once
Liquid is washed three times after immersion with dehydrated alcohol, is transferred in 60 DEG C of thermostatic drying chambers dry 4h, is transferred to 80 DEG C of perseverances later
Until being completely dried in warm drying box.
Formamide is added as dry additive in step (1) in drying process, and propylene oxide is added as gel inducing agents
Presoma surface can be modified, the quantity and surface electrical behavior of regulation and control surface hydroxyl, so that presoma Skeleton Table
Face has hydrophobicity, and the contact angle between skeleton and solvent increases, and greatly reduces the additonal pressure of capillary in turn
So that presoma reduces dry requirement, and is added propylene oxide and can speed up the process of aqueous precursor gel, and work as first
When in amide addition system, the concentration of system increases, and the formamide Micelle being dispersed in system is more, therefore as template, most
The quantity for being grown in the gel hole outside it eventually increases, so final gel specific surface area obtained and corresponding pore volume increase
Greatly；Uniform eventually by gel structure made from the constant pressure and dry process that formamide and propylene oxide is added, partial size reduces, so that
Next aeroge density made of reduces, and specific surface area increases, and the microstructure of aeroge is also more perfect.
Further, the weight ratio of presoma, formamide and propylene oxide is 1: 2: 0.3 in step (1).
Further, the weight ratio of ethyl orthosilicate and 80% ethanol water is 1: 5.
Further, the average pore size of silicon based ceramic aeroge made from step S5 is 30-40nm, porosity 75%-
80%。
Beneficial effects of the present invention:
(1) silicon based ceramic aeroge of the present invention hydroxide ion and silicon ion in step S1 in zirconium oxychloride during the preparation process
Or silicon ion group hydroxylating formed eight-coordinate body, zirconium ion forms eight-coordinate body in acid condition later, latter two eight match
Position body is mutually connected with apex angle, dehydration crystallization, forms that zirconium oxide is octahedra and silicon-oxygen tetrahedron, is interconnected to form silicic acid
Zirconium；It joined sodium fluoride, fluorine ion can replace oxonium ion to form Zr-F key and Si-F key, can reduce the crystallization gesture of zirconium silicate
It builds, and then accelerates zirconium silicate crystallization, and manufactured colloidal particle is smaller, total surface area is big, and activity is higher than sediment, is conducive to
It realizes crystal growth and reaction temperature can be reduced and shorten the reaction time;It is carried out in step S3 by glycerol and trim,ethylchlorosilane
Displacement, can enhance the network structure of gel, while reducing in the capillary of gel network, can effectively avoid in suction filtration process
In cause gel to generate collapsing, solve it is dry after the mechanical properties such as obtained aeroge intensity and toughness it is generally poor, at heat
It is excessively high to manage temperature, nanoscale hole hole will occur to collapse and aeroge is caused to densify completely, and aeroge stomata easily collapses
Broken technical problem；
(2) formamide is added as dry additive in step (1) during constant pressure and dry in step S2 of the present invention, and epoxy third is added
Alkane can modify presoma surface as gel inducing agents, the quantity and surface electrical behavior of regulation and control surface hydroxyl,
So that presoma Skeleton Table face has hydrophobicity, and the contact angle between skeleton and solvent increases, and greatly reduces capillary
The additonal pressure of pipe is so that presoma reduces dry requirement, and propylene oxide is added and can speed up aqueous precursor gel
The process of change, and when in formamide addition system, the concentration of system increases, and the formamide Micelle being dispersed in system is more,
Therefore be used as template, the quantity for being finally grown in the gel hole outside it increases, so final obtained gel specific surface area and
Corresponding pore volume increases；It is equal eventually by gel structure made from the constant pressure and dry process that formamide and propylene oxide is added
Even, partial size reduces, so that aeroge density made of next reduces, specific surface area increases, and the microstructure of aeroge is also more
Add kind, solve in prior art preparation aerogel process, aeroge skeleton surface does not have a hydrophobicity, and skeleton with it is molten
Contact angle between agent is smaller, causes the additonal pressure of capillary larger, and the slower technical problem of process of gelation.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, includes the following steps:
Step S1, following raw material: 10 parts of ethyl orthosilicates, 50 parts of deionized waters, 50 parts of dehydrated alcohols, 15 parts of oxygen are weighed
Zirconium chloride, 10 parts of zirconium nitrates, 3 parts of sodium fluorides, 3 parts of silica, 5 parts of silicon nitrides, 30 parts of glycerol and 50 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
The process of constant pressure and dry includes the following steps:
(1) formamide and propylene oxide are added into presoma, is transferred in 50 DEG C of insulating boxs, aging 20h is warming up to 65 DEG C,
And with soaked in absolute ethyl alcohol, 12h, every 4h change a not good liquor, then at 70 DEG C with impregnating 2h, Zhi Houyong in 80% ethanol water
Dehydrated alcohol washs three times；
(2) it is added after the completion of washing in the mixed solution of ethyl orthosilicate and 80% ethanol water and impregnates 8h, every 2h is changed once
Liquid is washed three times after immersion with dehydrated alcohol, is transferred in 60 DEG C of thermostatic drying chambers dry 4h, is transferred to 80 DEG C of perseverances later
Until being completely dried in warm drying box.
The weight ratio for controlling presoma, formamide and propylene oxide is 1: 2: 0.3；Ethyl orthosilicate and 80% ethyl alcohol are water-soluble
The weight ratio of liquid is 1: 5.
Embodiment 2
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, includes the following steps:
Step S1, following raw material: 12 parts of ethyl orthosilicates, 55 parts of deionized waters, 52 parts of dehydrated alcohols, 16 parts of oxygen are weighed
Zirconium chloride, 10 parts of zirconium nitrates, 4 parts of sodium fluorides, 5 parts of silica, 6 parts of silicon nitrides, 35 parts of glycerol and 55 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Embodiment 3
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, includes the following steps:
Step S1, following raw material: 13 parts of ethyl orthosilicates, 60 parts of deionized waters, 65 parts of dehydrated alcohols, 18 parts of oxygen are weighed
Zirconium chloride, 11 parts of zirconium nitrates, 4 parts of sodium fluorides, 6 parts of silica, 6 parts of silicon nitrides, 45 parts of glycerol and 65 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Embodiment 4
A kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, includes the following steps:
Step S1, following raw material: 15 parts of ethyl orthosilicates, 65 parts of deionized waters, 70 parts of dehydrated alcohols, 20 parts of oxygen are weighed
Zirconium chloride, 12 parts of zirconium nitrates, 5 parts of sodium fluorides, 8 parts of silica, 8 parts of silicon nitrides, 50 parts of glycerol and 70 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Comparative example 1
Compared with Example 1, dry instead of constant pressure and dry with 80 DEG C, preparation method is as follows for this comparative example:
Step S1, following raw material: 10 parts of ethyl orthosilicates, 50 parts of deionized waters, 50 parts of dehydrated alcohols, 15 parts of oxygen are weighed
Zirconium chloride, 10 parts of zirconium nitrates, 3 parts of sodium fluorides, 3 parts of silica, 5 parts of silicon nitrides, 30 parts of glycerol and 50 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, gel is made in 80 DEG C of dry 10h；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Comparative example 2
This comparative example compared with Example 1, does not carry out the displacement of glycerol and trim,ethylchlorosilane in step S3, preparation method is as follows
It is shown:
Step S1, following raw material: 10 parts of ethyl orthosilicates, 50 parts of deionized waters, 50 parts of dehydrated alcohols, 15 parts of oxygen are weighed
Zirconium chloride, 10 parts of zirconium nitrates, 3 parts of sodium fluorides, 3 parts of silica, 5 parts of silicon nitrides, 30 parts of glycerol and 50 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, it is after suction filtration, filter residue is dry at 70-90 DEG C
Silica-based aerogel is made in 1h；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
Comparative example 3
This comparative example is a kind of silica-based aerogel in market.
The porosity, average pore size and apparent density of embodiment 1-4 and comparative example 1-3 are detected, it is as a result as follows
Shown in table；
It can be seen that the porosity of embodiment 1-4 is 75-80% from upper table, the porosity of comparative example 1-3 is 50-55%, is implemented
The average pore size of example 1-4 is 30-40nm, and the average pore size of comparative example 1-3 is 20-24nm, and the apparent density of embodiment 1-4 is
0.10-0.15g/cm3, the apparent density of comparative example 1-3 is 0.20-0.25g/cm3；So working as formamide in step S2 of the present invention
When in addition system, the concentration of system increases, and the formamide Micelle being dispersed in system is more, therefore as template, most throughout one's life
The quantity for growing the gel hole outside it increases, so final gel specific surface area obtained and corresponding pore volume increase；Most
The gel structure as made from being added the constant pressure and dry process of formamide and propylene oxide is uniform eventually, and partial size reduces, so that connecing down
Aeroge density made of coming reduces, and specific surface area increases, and the microstructure of aeroge is also more perfect, solves the prior art
It prepares in aerogel process, aeroge skeleton surface does not have hydrophobicity, and the contact angle between skeleton and solvent is smaller, leads
Cause the additonal pressure of capillary larger, and the slower technical problem of process of gelation.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (5)
1. a kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology, which comprises the steps of:
Step S1, following raw material: 10-15 parts of ethyl orthosilicates, 50-65 parts of deionized waters, 50-70 parts of anhydrous second are weighed
Alcohol, 15-20 parts of zirconium oxychlorides, 10-12 parts of zirconium nitrates, 3-5 parts of sodium fluorides, 3-8 parts of silica, 5-8 parts of silicon nitrides, 30-50 parts
Glycerol and 50-70 parts of trim,ethylchlorosilanes；
Step S2, ethyl orthosilicate, deionized water and dehydrated alcohol are added in beaker, 50 DEG C of waters bath with thermostatic control heating and with
10% ammonium hydroxide is added dropwise in the revolving speed magnetic agitation of 120r/min, until occurring floccule in beaker, 10% dilute hydrochloric acid is added and adjusts pH,
Until pH is 5.6, zirconium oxychloride is mixed with zirconium nitrate and is added in beaker, sodium fluoride is added, with the revolving speed magnetic force of 150r/min
Stirring, until forming colloid；
Step S3, silica and alpha-silicon nitride powders are added into colloid, 5min, ultrasonic 5min are stirred with the revolving speed of 1000r/min,
Presoma is made, carries out constant pressure and dry, gel is made；
Step S4, gel is pulverized, 2h is washed with deionized, filtered, glycerol and trim,ethylchlorosilane are immersed after suction filtration
It is replaced, control displacement temperature is filtered after being 60 DEG C, time swap 2h, agitator treating 20min, by filter residue in 70-
Dry 1h, is made silica-based aerogel at 90 DEG C；
Step S5, it is sintered 1-2h at 1200-1500 DEG C after drying filter cake at 120 DEG C, silicon based ceramic aeroge is made.
2. a kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology according to claim 1, feature
It is, the process of constant pressure and dry includes the following steps: in step S2
(1) formamide and propylene oxide are added into presoma, is transferred in 50 DEG C of insulating boxs, aging 20h is warming up to 65 DEG C,
And with soaked in absolute ethyl alcohol, 12h, every 4h change a not good liquor, then at 70 DEG C with impregnating 2h, Zhi Houyong in 80% ethanol water
Dehydrated alcohol washs three times；
(2) it is added after the completion of washing in the mixed solution of ethyl orthosilicate and 80% ethanol water and impregnates 8h, every 2h is changed once
Liquid is washed three times after immersion with dehydrated alcohol, is transferred in 60 DEG C of thermostatic drying chambers dry 4h, is transferred to 80 DEG C of perseverances later
Until being completely dried in warm drying box.
3. a kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology according to claim 2, feature
It is, the weight ratio of presoma, formamide and propylene oxide is 1: 2: 0.3 in step (1).
4. a kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology according to claim 2, feature
It is, the weight ratio of ethyl orthosilicate and 80% ethanol water is 1: 5.
5. a kind of silicon based ceramic aeroge preparation process based on ceramic sintering technology according to claim 1, feature
It is, the average pore size of silicon based ceramic aeroge made from step S5 is 30-40nm, porosity 75%-80%.
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