CN109534351A - A kind of yttrium silicate Aerogel Nanocomposites material and preparation method thereof - Google Patents
A kind of yttrium silicate Aerogel Nanocomposites material and preparation method thereof Download PDFInfo
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- CN109534351A CN109534351A CN201910030443.8A CN201910030443A CN109534351A CN 109534351 A CN109534351 A CN 109534351A CN 201910030443 A CN201910030443 A CN 201910030443A CN 109534351 A CN109534351 A CN 109534351A
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Abstract
The present invention relates to a kind of yttrium silicate Aerogel Nanocomposites material and preparation method thereof.The preparation component of the preparation method includes presoma, soluble yttrium salt, ethanol water and the gel auxiliary agent of silicon, wet gel is made in the preparation component by sol-gel method, wet gel replaces through solvent, is dried to obtain aeroge, aeroge is subjected to high-temperature heat treatment again, obtains yttrium silicate Aerogel Nanocomposites material.Yttrium silicate Aerogel Nanocomposites material made from the preparation method has high-specific surface area, low-density, the characteristic of lower thermal conductivity, preparation process simply easily realizes, and good heat-proof quality, high-temperature stability are shown in ultra-high temperature environment, superhigh temperature extreme environment various kinds of equipment, which be on active service, has positive meaning.
Description
Technical field
The present invention relates to the technical field of nano material of superhigh temperature heat-proof quality more particularly to a kind of yttrium silicate aeroge to receive
Nano composite material and preparation method thereof.
Background technique
Requirement with fields such as aerospace, chemical industry metallurgical, hot parts to material heat-proof quality is more and more harsher, passes
The heat-barrier material of system is unable to satisfy the insulation requirement under ultra-high temperature.Current common heat-barrier material system, such as SiO2Porous pottery
Porcelain intensity is lower and non-refractory, Al2O3The high temperature resistance of porous ceramics preferably but thermal conductivity also it is relatively high cause its every
Thermal effect is bad, and YSZ ceramic material high-temperature shrinkage rate is big and density is higher, and mullite ceramic material is unable to satisfy pair at high temperature
The requirement etc. of intensity, it is difficult to meet superhigh temperature use condition.Therefore, stability excellent with heat-proof quality is currently needed in a hurry
The characteristics such as good, excellent in mechanical performance, are adapted to the heat-barrier material of thermal extremes environment.
Aerogel material is porous material of the aggregation with three-dimensional net structure that be cross-linked with each other by nano particle.Aeroge tool
There are the characteristics such as low-density, lower thermal conductivity, low-k, high porosity, high-specific surface area, in aerospace, building energy conservation, ring
The fields such as border improvement have biggish application value.Since its unique texture can substantially weaken solid phase heat transfer and gaseous heat transfer,
So that aeroge has extremely low thermal conductivity coefficient, it is a kind of heat-barrier material haveing excellent performance.However, traditional aerogel material is not
Can in hyperthermal environments steady operation, such as SiO2The steady in a long-term of aeroge is only limited to 650 DEG C using temperature, carbon aerogels without
Method is used as high temperature insulating material in aerobic environment, introduces Al2O3The SiO of component2Aeroge has the hair of phase transformation under high temperature environment
Life is so as to cause structure collapses etc..Thus, for further developing heat-barrier material, improvement aerogel material can be super
Steady operation is a kind of feasible method in hot environment.
Yttrium silicate (Y-Si-O), including Y2Si2O7, Y2SiO5And 2Y2O3·3SiO2, it is a kind of with extensive multifarious crystalline substance
The material of body structure.Yttrium silicate material because its higher fusing point, good antioxygenic property, excellent mechanical performance it is novel every
Contain huge potentiality in the research and development of hot system.Wherein Y2SiO5、Y2Si2O7The fusing point of two kinds of crystal forms is respectively 1980 DEG C, 1775
DEG C, belong to infusibility silicate material, can be on active service in hyperthermal environments, and excellent mechanical property, durability can be protected
The processing and fabricating of card yttrium silicate material is easier.Yttrium silicate material has good mechanics as a kind of new heat-barrier material system
Performance, heat-proof quality, high-temperature stability, corrosion resistance have good prospect in the heat-insulated field of hot environment.
Summary of the invention
A kind of blocky yttrium silicate is provided the purpose of the present invention is the high-temperature behavior based on existing light heat-insulating material is insufficient
Aerogel composite has the characteristics that high-temperature stability is good, effectively heat-insulated, mechanical stability is excellent.
To achieve the goals above, the present invention provides the following technical scheme that
1, a kind of preparation method of yttrium silicate Aerogel Nanocomposites material, the preparation component of the preparation method include silicon
Presoma, soluble yttrium salt, ethanol water and gel auxiliary agent, the preparation component is made up of sol-gel method wet
Gel, wet gel replaces through solvent, is dried to obtain aeroge, then aeroge is carried out high-temperature heat treatment, obtains yttrium silicate airsetting
Glue nanocomposite；Wherein, high-temperature heat treatment includes:
First stage: it is warming up to the first temperature from room temperature according to the heating rate of 2-4 DEG C/min, and is protected at the first temperature
1-2 hours warm, the first temperature is 400-600 DEG C；
Second stage: it is warming up to second temperature from the first temperature according to the heating rate of 3-5 DEG C/min, and in second temperature
Lower heat preservation 1-2 hours, second temperature are 800-1200 DEG C.
2, the presoma of preparation method according to technical solution 1, the silicon is selected from ethyl orthosilicate, methyl trimethoxy oxygen
Base silane, waterglass are any one or more of.
3, preparation method according to technical solution 1, the solubility yttrium salt are selected from yttrium chloride, yttrium nitrate, yttrium sulfate
It is any one or more of.
4, the mole of preparation method according to technical solution 3, the solubility yttrium salt is the presoma of the silicon
1-6 times of mole.
5, preparation method according to technical solution 1, the gel auxiliary agent be selected from propylene oxide, methyloxetane,
Ethylene oxide, epoxychloropropane are any one or more of.
6, the preparation method according to technical solution 5, the mole of the gel auxiliary agent are that the soluble yttrium salt is rubbed
6-8 times of that amount.
7, according to the described in any item preparation methods of technical solution 1 to 6, the preparation method includes the following steps:
(1) presoma of silicon, soluble yttrium salt, ethanol water are mixed, obtains preliminary solution；
(2) gel auxiliary agent is added into preliminary solution, is uniformly dispersed, obtain colloidal sol, stood, obtain wet gel；
(3) wet gel is subjected to solvent displacement, is then dried, obtains aeroge；
(4) aeroge is subjected to high-temperature heat treatment, obtains the yttrium silicate aerogel composite.
8, the preparation method according to technical solution 7 carries out the solvent displacement using ethyl alcohol, and displacement number is 4-8
Secondary, each interval time is 12-24 hours.
9, the preparation method according to technical solution 7, is dried using supercritical drying.
10, a kind of yttrium silicate Aerogel Nanocomposites material, using the described in any item preparation methods of technical solution 1 to 9
It is made.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
(1) yttrium silicate aerogel composite of the invention, the good characteristics of yttrium silicate and aeroge are combined, and are obtained
Be a kind of not only to have low-density, high porosity (89%-93%), lower thermal conductivity (0.02-0.04W/m-1·K-1), nanometer
The characteristic that kernel structure and nano aperture structure combine, there are also heat-insulated good, anti-oxidant, high temperature resistant, dystectic performance it is compound
Material.
(2) high-temperature stability of yttrium silicate Aerogel Nanocomposites material made from preparation method of the present invention greatly improves,
The high temperature action more than 1500 DEG C can be resisted in aerobic environment and can stablize military service.
(3) heat-proof quality of yttrium silicate Aerogel Nanocomposites material made from preparation method of the present invention greatly improves, by
Hot face is in high temperature environment (1200-1500 DEG C), and heat-insulating efficiency is up to 80% or more.
(4) yttrium silicate Aerogel Nanocomposites material made from preparation method of the present invention, passes through simple sol-gel
Method, supercritical drying are available, prepare raw material and are easy to get, and technique is repeatable.
Detailed description of the invention
Fig. 1 is the outside drawing of yttrium silicate Aerogel Nanocomposites material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of yttrium silicate Aerogel Nanocomposites material prepared by the embodiment of the present invention 2；
Fig. 3 is the heat insulation figure of yttrium silicate Aerogel Nanocomposites material prepared by the embodiment of the present invention 4.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of preparation method of yttrium silicate Aerogel Nanocomposites material, the preparation component of use includes
The presoma of silicon, soluble yttrium salt, ethanol water and gel auxiliary agent, the preparation component is made up of sol-gel method
Wet gel, wet gel replaces through solvent, is dried to obtain aeroge, then aeroge is carried out high-temperature heat treatment, obtains yttrium silicate gas
Gel nanocomposites；Wherein, high-temperature heat treatment includes:
First stage: it is warming up to the first temperature from room temperature according to the heating rate of 2-4 DEG C/min, and is protected at the first temperature
1-2 hours warm, the first temperature is 400-600 DEG C；
Second stage: it is warming up to second temperature from the first temperature according to the heating rate of 3-5 DEG C/min, and in second temperature
Lower heat preservation 1-2 hours, second temperature are 800-1200 DEG C.
Specifically, the preparation method includes the following steps:
(1) presoma of silicon, soluble yttrium salt, ethanol water are mixed, obtains preliminary solution；
The presoma of silicon can be any one or more of selected from ethyl orthosilicate, methyltrimethoxysilane, waterglass；
Soluble yttrium salt can be any one or more of selected from yttrium chloride, yttrium nitrate, yttrium sulfate, and dosage can refer to
The dosage of the presoma of silicon is determined according to following condition: the mole of soluble yttrium salt is the 1- of the presoma mole of silicon
6 times；
Ethanol water is the mixed solution that second alcohol and water is formulated, its dosage is not particularly limited in the present invention, right
The proportion of second alcohol and water is also not particularly limited；
(2) gel auxiliary agent is added into preliminary solution, is uniformly dispersed, obtain colloidal sol, stood, obtain wet gel；Gel
Auxiliary agent can be any one or more of selected from propylene oxide, methyloxetane, ethylene oxide, epoxychloropropane, dosage
Can be with reference to the dosage of soluble yttrium salt, more appropriately, the mole of gel auxiliary agent is the soluble yttrium salt mole
6-8 times；
(3) wet gel is subjected to solvent displacement, is then dried, obtains aeroge；
When carrying out solvent displacement, wet gel can be put into ethyl alcohol and carry out the solvent displacement, displacement number is preferably
4-8 times, each interval time is preferably 12-24 hours；
Drying means is preferably supercritical drying, the wet gel after displacement is put into dry in supercritical drying device
To aeroge；
(4) aeroge is subjected to high-temperature heat treatment, obtains the yttrium silicate aerogel composite；High-temperature heat treatment packet
It includes:
First stage: it is warming up to the first temperature from room temperature according to the heating rate of 2-4 DEG C/min, and is protected at the first temperature
1-2 hours warm, the first temperature is 400-600 DEG C, for example, can be 400 DEG C, 500 DEG C, 600 DEG C；
Second stage: it is warming up to second temperature from the first temperature according to the heating rate of 3-5 DEG C/min, and in second temperature
Lower heat preservation 1-2 hours, second temperature is 800-1200 DEG C, for example, can be 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200
℃。
The present invention also provides a kind of yttrium silicate Aerogel Nanocomposites material, using preparation method system provided by the invention
?.The excellent hot spot of yttrium silicate and aeroge is combined using this composite material made from this method, and there is low-density, low-heat
The characteristic that conductance, high porosity, nanoparticle structure and nano aperture structure combine also has heat-insulated good, anti-oxidant, resistance to height
Warm, dystectic performance.It, can using the heat-insulating efficiency of this composite material made from preparation method provided by the invention through detecting
Up to 80% or more (heating surface is in 1200-1500 environment), show that its heat-proof quality greatly improves；It can be in aerobic environment
It resists the high temperature action more than 1500 DEG C and military service can be stablized, show that its high-temperature stability greatly improves.
It is the embodiment that the present invention enumerates below.
Embodiment 1
4.15g ethyl orthosilicate is mixed to 41.50gEtOH/H2In O solution, wherein H2O is the 30% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 8 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 800 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 500 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 800 DEG C by 500 DEG C, and heating rate is 2 DEG C/min, then the soaking time 2h at 800 DEG C, is made
Yttrium silicate Aerogel Nanocomposites material, outside drawing Fig. 1.
Through detecting, the density of material made from the embodiment is 0.15g/cm3, thermal conductivity 0.024W/m-1·K-1, hole
Rate is 92%, intensity 0.64Mpa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
80%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 4.8%.
Embodiment 2
4.15g ethyl orthosilicate is mixed to 27.67gEtOH/H2In O solution, wherein H2O is the 15% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 7 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, solution of every 12h replacement, one
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 800 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 500 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 800 DEG C by 500 DEG C, and heating rate is 2 DEG C/min, then the soaking time 2h at 800 DEG C, is made
Yttrium silicate Aerogel Nanocomposites material, SEM figure are shown in Fig. 2.
Through detecting, the density of material made from the embodiment is 0.12g/cm3, thermal conductivity 0.022W/m-1·K-1, hole
Rate is 93%, intensity 0.60Mpa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
82%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 4.4%.
Embodiment 3
4.15g ethyl orthosilicate is mixed to 41.50gEtOH/H2In O solution, wherein H2O is the 20% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 8 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 6 times altogether.Then wet gel is put into supercritical drying kettle and is dried, the aeroge after drying is heat-treated,
Processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 600 DEG C；After heat preservation after
Temperature of continuing rising rises to 1000 DEG C by 600 DEG C, and heating rate is 2 DEG C/min, then the soaking time 2h at 1000 DEG C, and silicic acid is made
Yttrium Aerogel Nanocomposites material.
Through detecting, the density of material made from the embodiment is 0.19g/cm3, thermal conductivity 0.028W/m-1·K-1, hole
Rate is 91%, intensity 0.70Mpa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
79%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 4.5%.
Embodiment 4
6.04g ethyl orthosilicate is mixed to 50.58gEtOH/H2In O solution, wherein H2O is the 10% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 1 times of ethyl orthosilicate are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 6 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1000 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 5 DEG C/min, then keeps the temperature 2h at 600 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 1000 DEG C by 600 DEG C, and heating rate is 4 DEG C/min, then the soaking time 2h at 1000 DEG C, system
Yttrium silicate Aerogel Nanocomposites material is obtained, heat insulation is shown in Fig. 3.
Through detecting, the density of material made from the embodiment is 0.22g/cm3, thermal conductivity 0.031W/m-1·K-1, hole
Rate is 90%, intensity 0.69Mpa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
79%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 4.0%.
Embodiment 5
6.04g ethyl orthosilicate is mixed to 40.46gEtOH/H2In O solution, wherein H2O is the 40% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 1 times of ethyl orthosilicate are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 6 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1100 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 4 DEG C/min, then keeps the temperature 2h at 600 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 1100 DEG C by 600 DEG C, and heating rate is 2 DEG C/min, then the soaking time 2h at 1100 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, the density of material made from the embodiment is 0.20g/cm3, thermal conductivity 0.029W/m-1·K-1, hole
Rate is 91%, and 1200 DEG C of heat-insulating efficiencies are 81%, intensity 0.68Mpa, is tested and is surveyed by the back temperature of 1000s under 1200 DEG C of environment
It obtains material heat-insulating efficiency and is greater than 81%, heat treatment 1000s measures the contraction of material overall linear and is less than in 1500 DEG C of environment
3.8%.
Embodiment 6
6.04g ethyl orthosilicate is mixed to 40.46gEtOH/H2In O solution, wherein H2O is the 20% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 1 times of ethyl orthosilicate are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 6 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, solution of every 12h replacement, one
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1200 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 2 DEG C/min, then keeps the temperature 1h at 600 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 1200 DEG C by 600 DEG C, and heating rate is 3 DEG C/min, then the soaking time 2h at 1200 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, the density of material made from the embodiment is 0.18g/cm3, thermal conductivity 0.026W/m-1·K-1, hole
Rate is 91%, intensity 0.62MPa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
79%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 3.2%.
Embodiment 7
2.77g ethyl orthosilicate is mixed to 55.40gEtOH/H2In O solution, wherein H2O is the 30% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 3 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 7 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 4 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1200 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 5 DEG C/min, then keeps the temperature 2h at 600 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 1200 DEG C by 600 DEG C, and heating rate is 3 DEG C/min, then the soaking time 2h at 1200 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, the density of material made from the embodiment is 0.23g/cm3, thermal conductivity 0.033W/m-1·K-1, hole
Rate is 89%, intensity 0.75MPa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
82%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 3.3%.
Embodiment 8
2.77g ethyl orthosilicate is mixed to 55.40gEtOH/H2In O solution, wherein H2O is the 20% of EtOH mass, is stirred
1h is mixed, six water yttrium chlorides of the mole of 3 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Again to solution
The propylene oxide of the middle mole for instilling 6 times of six water yttrium chloride, stirs 10min, then pours into sol solution in mold, quiet
It postpones to obtain wet gel.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours, one
It replaces 6 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1100 DEG C of heat are carried out to the aeroge after drying
Processing, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 4 DEG C/min, then keeps the temperature 2h at 600 DEG C；Heat preservation knot
Shu Houji temperature of continuing rising rises to 1100 DEG C by 600 DEG C, and heating rate is 2 DEG C/min, then the soaking time 2h at 1100 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, the density of material made from the embodiment is 0.20g/cm3, thermal conductivity 0.027W/m-1·K-1, hole
Rate is 91%, intensity 0.70Mpa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
82%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 3.9%.
Embodiment 9
4.15g ethyl orthosilicate is mixed to 41.50g EtOH/H2In O solution, wherein H2O is the 30% of EtOH mass,
1h is stirred, the yttrium nitrate hexahydrate of the mole of 2 times of ethyl orthosilicates is then added, stirring 2h is complete to its hydrolysis.Xiang Rong again
The methyloxetane that the mole of 8 times of yttrium nitrate hexahydrates is instilled in liquid, stirs 10min, sol solution is then poured into mould
In tool, wet gel is obtained after standing.Wet gel is put into EtOH environment and carries out aging and solvent replacement, it is primary per replacement for 24 hours
Solution is replaced 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, the aeroge after drying is carried out
800 DEG C of heat treatments, processing step are as follows: rise to 500 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；
Continue to heat up after heat preservation, rises to 800 DEG C by 500 DEG C, heating rate is 2 DEG C/min, then the soaking time at 800 DEG C
Yttrium silicate Aerogel Nanocomposites material is made in 2h.
Through detecting, the density of material made from the embodiment is 0.16g/cm3, thermal conductivity 0.023W/m-1·K-1, hole
Rate is 92%, intensity 0.61MPa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
81%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 5.0%.
Embodiment 10
4.15g ethyl orthosilicate is mixed to 41.50g EtOH/H2In O solution, wherein H2O is the 30% of EtOH mass,
1h is stirred, eight water yttrium sulfates of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Xiang Rong again
The epoxychloropropane that the mole of 8 times of eight water yttrium sulfate is instilled in liquid, stirs 10min, sol solution is then poured into mold
In, wet gel is obtained after standing.Wet gel is put into EtOH environment and carries out aging and solvent replacement, it is primary molten per replacement for 24 hours
Liquid is replaced 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 800 are carried out to the aeroge after drying
DEG C heat treatment, processing step are as follows: rise to 500 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；It protects
Continuing to heat up after temperature, rises to 800 DEG C by 500 DEG C, heating rate is 2 DEG C/min, then the soaking time 2h at 800 DEG C,
Yttrium silicate Aerogel Nanocomposites material is made.
Through detecting, the density of material made from the embodiment is 0.13g/cm3, thermal conductivity 0.021W/m-1·K-1, hole
Rate is 93%, intensity 0.55MPa, measures material heat-insulating efficiency by the back temperature of 1000s under 1200 DEG C of environment and is greater than
82%, it is heat-treated 1000s in 1500 DEG C of environment and measures the contraction of material overall linear less than 5.4%.
Embodiment 11
4.15g ethyl orthosilicate is mixed to 41.50g EtOH/H2In O solution, wherein H2O is the 30% of EtOH mass,
1h is stirred, six water yttrium chlorides of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Xiang Rong again
The propylene oxide that the mole of 8 times of six water yttrium chloride is instilled in liquid, stirs 10min, then pours into sol solution in mold,
Wet gel is obtained after standing.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours,
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 700 DEG C are carried out to the aeroge after drying
Heat treatment, processing step are as follows: rise to 400 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；Heat preservation
After continue to heat up, rise to 700 DEG C by 400 DEG C, heating rate is 2 DEG C/min, then the soaking time 2h at 800 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, which makes aeroge fail to complete the phase transition process of material since heat treatment temperature is too low,
Material obtained is the yttrium silicate Aerogel Nanocomposites material of moiety content.
Embodiment 12
4.15g ethyl orthosilicate is mixed to 41.50g EtOH/H2In O solution, wherein H2O is the 30% of EtOH mass,
1h is stirred, six water yttrium chlorides of the mole of 2 times of ethyl orthosilicates are then added, stirring 2h is complete to its hydrolysis.Xiang Rong again
The propylene oxide that the mole of 8 times of six water yttrium chloride is instilled in liquid, stirs 10min, then pours into sol solution in mold,
Wet gel is obtained after standing.Wet gel is put into EtOH environment and carries out aging and solvent replacement, per solution of replacement for 24 hours,
It replaces 8 times altogether.Then wet gel is put into supercritical drying kettle and is dried, 1300 DEG C are carried out to the aeroge after drying
Heat treatment, processing step are as follows: rise to 600 DEG C by room temperature, heating rate is 3 DEG C/min, then keeps the temperature 1h at 500 DEG C；Heat preservation
After continue to heat up, rise to 1300 DEG C by 600 DEG C, heating rate is 2 DEG C/min, then the soaking time 2h at 800 DEG C, system
Obtain yttrium silicate Aerogel Nanocomposites material.
Through detecting, the embodiment is obtained since heat treatment temperature is excessively high so that aeroge has obvious contraction
Material is bigger with respect to other embodiments density and has the tendency that densification is affected so as to cause aeroge performance.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of yttrium silicate Aerogel Nanocomposites material, which is characterized in that the preparation group of the preparation method
The siliceous presoma of subpackage, soluble yttrium salt, ethanol water and gel auxiliary agent, by sol-gel method by the preparation group
Divide and wet gel is made, wet gel replaces through solvent, is dried to obtain aeroge, then aeroge is carried out high-temperature heat treatment, obtains silicon
Sour yttrium Aerogel Nanocomposites material；Wherein, high-temperature heat treatment includes:
First stage: it is warming up to the first temperature from room temperature according to the heating rate of 2-4 DEG C/min, and keeps the temperature 1- at the first temperature
2 hours, the first temperature was 400-600 DEG C；
Second stage: it is warming up to second temperature from the first temperature according to the heating rate of 3-5 DEG C/min, and is protected at the second temperature
1-2 hours warm, second temperature is 800-1200 DEG C.
2. preparation method according to claim 1, which is characterized in that the presoma of the silicon is selected from ethyl orthosilicate, first
Base trimethoxy silane, waterglass are any one or more of.
3. preparation method according to claim 1, which is characterized in that it is described solubility yttrium salt be selected from yttrium chloride, yttrium nitrate,
Yttrium sulfate is any one or more of.
4. preparation method according to claim 3, which is characterized in that the mole of the solubility yttrium salt is the silicon
1-6 times of presoma mole.
5. preparation method according to claim 1, which is characterized in that the gel auxiliary agent is selected from propylene oxide, methyl ring
Ethylene Oxide, ethylene oxide, epoxychloropropane are any one or more of.
6. preparation method according to claim 5, which is characterized in that the mole of the gel auxiliary agent is the solubility
6-8 times of yttrium salt mole.
7. preparation method according to any one of claims 1 to 6, which is characterized in that the preparation method includes following step
It is rapid:
(1) presoma of silicon, soluble yttrium salt, ethanol water are mixed, obtains preliminary solution；
(2) gel auxiliary agent is added into preliminary solution, is uniformly dispersed, obtain colloidal sol, stood, obtain wet gel；
(3) wet gel is subjected to solvent displacement, is then dried, obtains aeroge；
(4) aeroge is subjected to high-temperature heat treatment, obtains the yttrium silicate aerogel composite.
8. preparation method according to claim 7, which is characterized in that carry out the solvent displacement, displacement time using ethyl alcohol
Number is 4-8 times, and each interval time is 12-24 hours.
9. preparation method according to claim 7, which is characterized in that be dried using supercritical drying.
10. a kind of yttrium silicate Aerogel Nanocomposites material, which is characterized in that use the described in any item systems of claim 1 to 9
Preparation Method is made.
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| CN115872732A (en) * | 2023-02-23 | 2023-03-31 | 中国人民解放军国防科技大学 | Porous yttrium silicate-aluminum oxide complex phase wave-transmitting ceramic and preparation method thereof |
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