CN104909729B - Preparation method of lightweight rigid heat insulation material - Google Patents
Preparation method of lightweight rigid heat insulation material Download PDFInfo
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- CN104909729B CN104909729B CN201510251197.0A CN201510251197A CN104909729B CN 104909729 B CN104909729 B CN 104909729B CN 201510251197 A CN201510251197 A CN 201510251197A CN 104909729 B CN104909729 B CN 104909729B
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Abstract
The present invention belongs to the inorganic composite material technical field, and specifically relates to a preparation method of a lightweight rigid heat insulation material, and the preparation method comprises lightweight rigid heat insulation material fiber pretreatment, heat insulation substrate forming slurry preparation, slurry dispersion, suction filter forming, heat treatment, TiO2 sol preparation, vacuum impregnation, insulation substrate compositing TiO2 gel, and supercritical drying. The preparation method has the advantages of being scientific and reasonable, easy to implement, short in production cycle, and low in cost of investment, and the lightweight rigid heat insulation material prepared by the method has high mechanical properties and excellent heat insulation effect on the premise of guaranteeing of high porosity, and also has good thermal shock resistance.
Description
Technical field
The invention belongs to inorganic composite materials technical field, and in particular to a kind of preparation side of light rigidity heat-barrier material
Method.
Background technology
, in endoatmosphere flying for long time, aerodynamic force, thermal environment are very harsh for hypersonic aircraft, material and thermal protection
Technology is one of key technology.Rigid heat-barrier material porosity is high, and unit weight is low, at high temperature with stable shape and certain
Intensity, while the effect with excellent heat loss through radiation, heat-insulated, antiscour and holding aerodynamic configuration.Rigid heat-barrier material is in height
Have carrying and insulative effectiveness in supersonic aircraft concurrently.Insulative effectiveness is one of critical function of heat-barrier material, is flown with new
The local temperature of row device is more than 1000 DEG C, therefore heat-barrier material is put forward higher requirement.Research and the high property of preparation high temperature resistant
Energy heat-barrier material is the important directions of Future Development.
Under high temperature in heat-barrier material gas phase heat conduction and radiation heat conduction in the highest flight, wherein the radiation ratio that accounts for of heat conduction is more than
Gas phase heat conduction.Research shows that the ratio of more than 500 DEG C infra-red radiations accounts for 50%, under 1000 DEG C and 1300 DEG C of hot conditionss, heat-insulated
The emittance for having 76% and 85% respectively in material concentrates on infrared band.Therefore, under hot environment, reduce infrared band spoke
It is the effective way for reducing heat-barrier material thermal conductivity to penetrate, and the excellent fire-resistant high-performance heat-barrier material of processability is important
Method.TiO2Also referred to as titanium dioxide, its refraction coefficient are maximum in presently used filler, thus its reflectance is very high,
It is the first-selection of heat insulating function filler.Spectrogrph test finds that its reflectance in visible region is close to 100%, can in near-infrared
Up to more than 85%, the absorbance in the near ultraviolet band of 200-400nm has reached more than 85% to the emissivity in Jian Guang areas.There is research people
Member is with Ti (SO4)2Chemical deposition mode is adopted to coat a layer thickness in hollow glass micropearl outer wall for raw material sharp for 0.5 μm
Titanium ore type TiO2, gained thermal insulating filling is to visible ray and near infrared reflectance respectively 86% and 81%.There is research worker ratio
Cladding TiO is analyzed relatively2Glass microballoon and TiO2Glass microballoon mix the thermal insulating filling of both various combination modes every
Hot property, finds cladding TiO2Glass microballoon coating temperature compared with TiO2The coating that glass microballoon is mixed is in the outdoor sun
Under light irradiation, temperature is low by 0.8.Therefore by TiO2It is added in heat-barrier material as infrared shielding agent, height can be effectively reduced
The infra-red radiation of temperature area, so as to reduce thermal conductivity and improve heat-barrier material heat resistance the characteristics of.
The content of the invention
It is an object of the invention to provide a kind of preparation method of light rigidity heat-barrier material, the heat-barrier material of preparation is in guarantee
There is higher mechanical property, with good heat-insulated and scour resistance on the premise of high porosity.
The preparation method of light rigidity heat-barrier material of the present invention, step are as follows：
(1) pretreatment of light rigidity heat-barrier material fiber：The process that is chopped is carried out to quartz fibre, be chopped fiber after processing
Length is in 30-150um；The process that is chopped is carried out to alumina fibre, the alumina fibre length after process is in 50-250um；
(2) prepared by heat-insulated matrix molding slip：To be chopped obtained in step (1) quartz fibre and chopped alumina fibre,
Ludox, binding agent and deionized water are mixed, and obtain me fibrous slurry；
(3) mud dispersivity：With the pH value of me fibrous slurry in sour regulating step (2), it is stirred in V-type agitator；
(4) sucking filtration molding：The slip that step (3) is obtained carries out sucking filtration molding under vacuum, and the demoulding afterwards moves to perseverance
Warm drying baker is dried；
(5) heat treatment：By material obtained in step (4) loaded on heat treatment being carried out in kiln, obtain heat-insulated matrix；
(6)TiO2It is prepared by colloidal sol：Tetrabutyl titanate and tetraethyl orthosilicate are mixed, TiO is prepared2Colloidal sol；
(7) vacuum impregnation：Heat-insulated matrix in step (5) is put in vacuum tank, evacuation, will be molten in step (6)
Glue is impregnated in heat-insulated matrix；
(8) heat-insulated matrix composite Ti O2Gel：In the heat-insulated matrix that hydrolyzed solution is poured in step (7), whole process exists
Carry out on vibromill, until TiO2Colloidal sol is all changed into gel, obtains composite Ti O2The heat-barrier material matrix of gel；
(9) supercritical drying：The heat-barrier material matrix that step (8) is obtained is carried out into supercritical drying in autoclave
It is dry, obtain final product.
A diameter of 1-3um of the quartz fibre described in step (1), a diameter of 1-5um of alumina fibre.
The proportioning of Ludox, binding agent and deionized water described in step (2) is 75-125:1-4:3000-5000, silicon
, in terms of g, in terms of g, deionized water is in terms of ml for binding agent for colloidal sol.
Binding agent described in step (2) is BN powder, and the quality of binding agent is quartz fibre and the chopped aluminium oxide fibre of being chopped
The 1-4% of dimension gross mass；The quality of chopped alumina fibre is the 10- of chopped quartz fibre and chopped alumina fibre gross mass
40%；Ludox is acidic silicasol, and SiO2The content of effective ingredient is 20%.
PH value described in step (3) is 3-4.
Acid described in step (3) the preferably hydrochloric acid of 0.5mol/l.
In vacuum condition described in step (4), vacuum is -0.01--0.1MPa；Drying condition is to do at 70 DEG C
Dry 12h, is dried 4h afterwards at a temperature of 140 DEG C.
The sucking filtration time described in step (4) is 5-10min.
Heat treatment temperature described in step (5) is 1200-1240 DEG C, and heat treatment time is 1-2h.
Kiln described in step (5) is conventional radiation heating kiln, such as Si-Mo rod high temperature furnace, resistance wire high temperature furnace etc..
The volume ratio of tetraethyl orthosilicate and tetrabutyl titanate described in step (6) is 1:4-10.
Pumpdown time described in step (7) is 0.5-2h.
In step (7) using siphon principle by the sol impregnation in step (6) in heat-barrier material matrix.
Hydrolyzed solution described in step (8) is by TEOS, HAc and H2O mix homogeneously, stirs 10-30min；TEOS、HAc
And H2The volume ratio of O is 1:0.75:0.5-2.
Dried medium described in step (9) is ethanol, and drying pressure is 8.0-10MPa, and baking temperature is 270-300
DEG C, drying time is 4-8h.
Condition drying nano TiO of the step (9) using supercritical drying2。
Described infrared shielding agent TiO2It is to be prepared using sol-gel process, and TiO2Size be below 100nm.
Development scientific and technological in recent years it is also proposed the higher operating temperature of new requirement, more to the performance of rigid heat-barrier material
Low heat conductivity and higher mechanical property, therefore a kind of addition nano-TiO2The quartz fibre of infrared shielding agent and oxidation
Aluminum fiber prepares the new technology of porous heat insulation material and also just arises at the historic moment.It mainly uses the weaving feature or very thin shape of fiber
State, is formed the heat-barrier material matrix that the mutual frame of node constitutes porous between the fibers by binding agent, is drawn by sol-gel process
Enter nano-TiO2.Chopped fiber is dispersed in material from chopped quartz fibre and alumina fibre as reinforcement by the present invention
In slurry, then by operations such as slime vacuum sucking filtration molding, dry solidification and heat treatments, the light rigidity for making function admirable is more
The heat-barrier material matrix in hole.By colloidal sol Vacuum infusion techniques, TiO is prepared using sol-gel process2Colloidal sol, by nano-TiO2It is molten
Glue is impregnated into heat-barrier material matrix.Finally by aging and supercritical drying treatment process, the addition for preparing excellent performance is received
Rice TiO2The rigid heat-barrier material of infrared shielding agent.
Heat-barrier material matrix and TiO2Traditional kiln is used in the heat-barrier material Technology for Heating Processing link of immersing hydrogels
With autoclave as Equipment for Heating Processing, asking for heat-insulated matrix material porosity is controlled by the ratio of fiber and binding agent
Topic, adjusts ageing time and supercritical drying time control nano-TiO2Gel granular size and distribution feelings in heat-insulated matrix
Condition.Additionally, the present invention is easy to operate, the mass and through engineering approaches production of large scale product is facilitated implementation.
The present invention compared with prior art, has the advantages that：
The present invention utilizes nano-TiO2The characteristics of to the heat high-selenium corn high emission of region of ultra-red, can have as screening agent
The reduction radiant heat transfer of effect, using ultra-fine, high-strength, high temperature resistant and good stability quartz fibre and alumina fibre as skeleton,
It is aided with the heat-barrier material matrix that binding agent prepares effectively insulating, the characteristics of by heat-insulated matrix porosity, by sol-gel
Method is by the TiO of nanometer2It is incorporated in the hole of heat-insulated matrix.The present invention has scientific and reasonable, the easy to implement, production cycle
The low advantage of short, cost of investment, has on the premise of high porosity is ensured using light rigidity heat-barrier material prepared by the method
Higher mechanical property and excellent effect of heat insulation, while also having good thermal shock resistance.
Specific embodiment
With reference to embodiments the present invention is described further.
Raw material specification used in embodiment is as follows：
Quartz fibre：Cellucotton, diameter 1-3um, SiO2Content >=99%；
Alumina fibre：Cellucotton, diameter 1-7um, Al2O3Content >=71%；
Ludox：Pure, the SiO of chemistry2Content is no less than 20%；
Binding agent：Analyze pure, BN >=99%；
Tetrabutyl titanate (TBT)：Analysis is pure；
Tetraethyl orthosilicate (TEOS)：Analysis is pure；
HAc：Analysis is pure；
Ethanol：Analysis is pure.
Embodiment 1
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 30um, alumina fibre average length is 65um.
(2) quartz fibre 80g, alumina fibre 20g in weighing step (1), weighing 2g BN powder, 75g Ludox, fiber,
BN powder and Ludox are added in 3000ml deionized waters, make me fibrous slurry.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1220 DEG C, 2h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:240ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:0.5 (volume ratio) mix homogeneously, stirs 10min.It is slow to add
It is soaked with entering step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolysis
Liquid is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
Embodiment 2
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 30um, alumina fibre average length is 250um.
(2) quartz fibre 60g, alumina fibre 40g in step (1) is weighed, weighs 2g BN powder, 100g Ludox, it is fine
During dimension, BN powder and Ludox add 4000ml deionized waters, me fibrous slurry is made.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1200 DEG C, 2h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:400ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:0.5 (volume ratio) mix homogeneously, stirs 10min.It is slow to add
It is soaked with entering step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolysis
Liquid is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
Embodiment 3
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 65um, alumina fibre average length is 125um.
(2) quartz fibre 70g, alumina fibre 30g in step (1) is weighed, weighs 2g BN powder, 125g Ludox, it is fine
During dimension, BN powder and Ludox add 5000ml deionized waters, me fibrous slurry is made.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1200 DEG C, 1h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:320ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:1 (volume ratio) mix homogeneously, stirs 10min.It is slowly added to
It is soaked with step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolyzed solution
It is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
Embodiment 4
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 100um, alumina fibre average length is 65um.
(2) quartz fibre 80g, alumina fibre 20g in step (1) is weighed, weighs 2g BN powder, 100g Ludox, it is fine
During dimension, BN powder and Ludox add 4000ml deionized waters, me fibrous slurry is made.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1200 DEG C, 2h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:240ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:2 (volume ratio) mix homogeneously, stirs 10min.It is slowly added to
It is soaked with step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolyzed solution
It is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
Embodiment 5
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 150um, alumina fibre average length is 65um.
(2) quartz fibre 80g, alumina fibre 20g in step (1) is weighed, weighs 2g BN powder, 125g Ludox, it is fine
During dimension, BN powder and Ludox add 3000ml deionized waters, me fibrous slurry is made.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1220 DEG C, 2h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:240ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:2 (volume ratio) mix homogeneously, stirs 10min.It is slowly added to
It is soaked with step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolyzed solution
It is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
Embodiment 6
(1) process that is chopped, quartz fibre average length after process are carried out to ultra-fine quartz fibre cotton and alumina fibre cotton
For 150um, alumina fibre average length is 65um.
(2) quartz fibre 80g, alumina fibre 20g in step (1) is weighed, weighs 2g BN powder, 125g Ludox, it is fine
During dimension, BN powder and Ludox add 5000ml deionized waters, me fibrous slurry is made.
(3) pH value of slip is adjusted with acid, is made PH=3-4,30min is stirred in V-type agitator, makes fiber complete
It is dispersed in slip.
(4) vacuum for adjusting vacuum tank is -0.1MPa, and vacuum filtration process time is 10 minutes, sucking filtration molding, system
Into wet base.Wet base is put in thermostatic drying chamber and is dried, and drying condition is that 12h is dried at 70 DEG C, afterwards at a temperature of 140 DEG C
It is dried 4h.
(5) the wet base after being dried is loaded under normal pressure in kiln, in 1220 DEG C, 2h carries out heat treatment.
(6) tetrabutyl titanate (TBT) and tetraethyl orthosilicate (TEOS) are mixed, TEOS:40ml, TBT:320ml, mixing
Uniformly, 5min is stirred, prepares TiO2Colloidal sol.
(7) heat-barrier material matrix 100 × 100 × 30mm of size is put in vacuum tank, evacuation 30 minutes, vacuum
For -0.1MPa, using the principle of siphon by the sol impregnation in step (6) in heat-insulated matrix, make matrix be completely immersed in colloidal sol
In solution.
(8) by hydrolyzed solution TEOS:HAc:H2O=1:0.75:2 (volume ratio) mix homogeneously, stirs 10min.It is slowly added to
It is soaked with step (7) in the sol solution of heat-insulated matrix, whole process is carried out on vibromill, it is ensured that TiO2Colloidal sol and hydrolyzed solution
It is sufficiently mixed, until TiO2Colloidal sol is all changed into gel.
(9) heat-barrier material of step (8) is carried out into supercritical drying in autoclave.Dry condition：It is dried and is situated between
Matter is ethanol, pressure 8.0MPa, 270 DEG C of baking temperature, drying time 4h.
In embodiment 1-6, raw material and process conditions are shown in Table 1, table 2, and the parameter measured by obtained material is shown in Table 3.
With embodiment 1, raw material and process conditions are shown in Table 1, table 2 to embodiment 7-24 preparation method, measured by obtained material
Parameter be shown in Table 3.
Raw material and its ratio and other process conditions that each embodiment of 1 heat-insulated matrix of table is adopted
2 composite Ti O of table2Raw material and its ratio and other process conditions that each embodiment of nanometer infrared shielding agent is adopted
Note：TEOS in table 2:Ratios of the TBT for colloidal sol, TEOS:HAc:H2Ratios of the O for hydrolyzed solution, between the two
The not direct relations of TEOS.
Parameter of the table 3 by obtained in each embodiment measured by material
Claims (6)
1. a kind of preparation method of light rigidity heat-barrier material, it is characterised in that step is as follows：
（1）The pretreatment of light rigidity heat-barrier material fiber：The process that is chopped is carried out to quartz fibre, be chopped fibre length after processing
In 30-150um；The process that is chopped is carried out to alumina fibre, the alumina fibre length after process is in 50-250um；
（2）It is prepared by heat-insulated matrix molding slip：By step（1）Obtained chopped quartz fibre and chopped alumina fibre, silicon are molten
Glue, binding agent and deionized water are mixed, and obtain me fibrous slurry；
（3）Mud dispersivity：Use sour regulating step（2）The pH value of middle me fibrous slurry, is stirred in V-type agitator；
（4）Sucking filtration molding：Step（3）The slip for obtaining carries out sucking filtration molding under vacuum, and the demoulding afterwards moves to constant temperature and does
Dry case is dried；
（5）Heat treatment：By step（4）Obtained material obtains heat-insulated matrix loaded on heat treatment is carried out in kiln；
（6）TiO2It is prepared by colloidal sol：Tetrabutyl titanate and tetraethyl orthosilicate are mixed, TiO is prepared2Colloidal sol；
（7）Vacuum impregnation：By step（5）In heat-insulated matrix be put in vacuum tank, evacuation, by step（6）In colloidal sol leaching
Stain is in heat-insulated matrix；
（8）Heat-insulated matrix composite Ti O2Gel：Pour hydrolyzed solution into step（7）In heat-insulated matrix in, whole process is in vibromill
On carry out, until TiO2Colloidal sol is all changed into gel, obtains composite Ti O2The heat-barrier material matrix of gel；
（9）Supercritical drying：By step in autoclave（8）The heat-barrier material matrix for obtaining carries out supercritical drying, i.e.,
；
Step（1）Described in quartz fibre a diameter of 1-3um, a diameter of 1-5um of alumina fibre；
Step（2）Described in Ludox, binding agent and deionized water proportioning be 75-125:1-4:3000-5000, Ludox
In terms of g, in terms of g, deionized water is in terms of mL for binding agent；
Step（2）Described in binding agent be BN powder, the quality of binding agent for be chopped quartz fibre and chopped alumina fibre it is total
The 1-4% of quality；The quality of chopped alumina fibre is the 10-40% of chopped quartz fibre and chopped alumina fibre gross mass；
Step（4）Described in vacuum condition in vacuum be -0.01--0.1MPa；Drying condition is to be dried at 70 DEG C
12h, is dried 4h afterwards at a temperature of 140 DEG C；
Step（8）Described in hydrolyzed solution be by TEOS, HAc and H2O mix homogeneously, stirs 10-30min；TEOS, HAc and H2O
Volume ratio be 1:0.75:0.5-2.
2. the preparation method of light rigidity heat-barrier material according to claim 1, it is characterised in that step（2）Described in
Ludox is acidic silicasol, and SiO2The content of effective ingredient is 20%.
3. the preparation method of light rigidity heat-barrier material according to claim 1, it is characterised in that step（3）Described in
PH value is 3-4.
4. the preparation method of light rigidity heat-barrier material according to claim 1, it is characterised in that step（5）Described in
Heat treatment temperature is 1200-1240 DEG C, and heat treatment time is 1-2h.
5. the preparation method of light rigidity heat-barrier material according to claim 1, it is characterised in that step（6）Described in
The volume ratio of tetraethyl orthosilicate and tetrabutyl titanate is 1:4-10.
6. the preparation method of light rigidity heat-barrier material according to claim 1, it is characterised in that step（9）Described in
Dried medium is ethanol, and drying pressure is 8.0-10MPa, and baking temperature is 270-300 DEG C, and drying time is 4-8h.
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| CN104909729B true CN104909729B (en) | 2017-05-03 |
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| CN109996604A (en) * | 2016-11-30 | 2019-07-09 | 松下知识产权经营株式会社 | Filter, gas absorption device and vacuum insulation part using filter |
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| CN107142715B (en) * | 2017-04-11 | 2019-10-29 | 南京工业大学 | Light flexible reusable heat-insulation-prevention integrated material and preparation method thereof |
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| CN108793984B (en) * | 2018-07-13 | 2021-02-09 | 航天材料及工艺研究所 | High-temperature-resistant heat-insulation wave-transparent function integrated composite material and preparation method thereof |
| CN116854494A (en) * | 2023-06-02 | 2023-10-10 | 山东工业陶瓷研究设计院有限公司 | Rigid heat insulation material and preparation method thereof |
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