CN104860717A - Rigid ceramic thermal-insulation tile surface coating preparation method - Google Patents
Rigid ceramic thermal-insulation tile surface coating preparation method Download PDFInfo
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Abstract
The invention relates to a rigid ceramic thermal-insulation tile surface coating preparation method, and relates to a ceramic thermal-insulation tile surface coating preparation method. The invention aims at solving technical problems of high water absorption, low oxidation resistance and low thermal radiation coefficient of rigid porous ceramic thermal-insulation tiles. The method comprises the steps of 1, raw material powder preparation; 2, mixed material preparation; 3, spray coating; and 4, sintering. With the method provided by the invention, the microstructure of the coating has a gradual gradient feature. The coating at a porous substrate side is porous, and the surface coating is smooth and compact. With the existence of the porous transition layer, a coating and substrate expansion mismatch characteristic can be coordinated. The method provided by the invention is used for preparing the rigid ceramic thermal-insulation tile surface coating.
Description
Technical field
The present invention relates to the preparation method of ceramic insulation watt top coat.
Background technology
Near space hypersonic aircraft needs to fly thousands of second under aerobic and hot environment, compared to the high-speed aircraft (only tens seconds) passing through near space region, its active time under oxidation and hot environment grows (large two orders of magnitude) especially.The part of air to the damping merit of aircraft finally shows as the Aerodynamic Heating being transmitted to aircraft surface, thus causes the sharply rising of surface temperature.Long Aerodynamic Heating makes the surface temperature of head and flange portions more than 2000 DEG C, and simultaneously for keeping high liftdrag and good aerodynamic configuration, these position outside surfaces do not allow to produce obvious ablation.In addition, along with the flight velocity of aircraft strides forward to more High Mach number, more harsh requirement is proposed to aircraft surface thermal protection.Because high emissivity coatings significantly can improve the ability of Step atmospheric layers vehicle outwardly radiations heat energy, aircraft surface temperature can being reduced in the mode of heat radiation, therefore providing a new approach for solving the protection of Step atmospheric layers vehicle surface heat.Ceramic insulation watt is the thermally protective materials that colonial uses in space shuttle windward side, and be a kind of fibrous type rigidity lagging material, its main component is silica fiber, boron sikicate aluminum fiber or sapphire whisker.After high temperature sintering, between fiber, mutual " overlap joint " forms vesicular structure (porosity 80-95%), gives ceramic insulation watt good heat-proof quality and mechanical property.The high radiation coating technology matched with ceramic insulation watt also achieves obvious progress.Due to height friction, high temperature, the special environment for use such as oxidizable, this type coating majority is made up of resistant to elevated temperatures ceramic phase material, minority is contained to the coating of organic composition, is then generally applied in inside the relatively low empennage of temperature and upper surface place.According to the difference of preparation technology, the main method preparing supercoat on ceramic fiber thermal insulation tile surface has spraying method, spread coating and chemical Vapor deposition process etc.RCG (Reaction CuredGlass) is a kind of rigid ceramic surface high emissivity coating that colonial uses on the thermal insulation tile of shuttle Columbia surface, and emittance is between 0.9-0.93.The features such as coating has heat shock resistance, and thermal expansivity is low, waterproof, and chemical stability is good, the highlyest can use at 1100 DEG C, can keep good mechanical property under high temperature.But, due to the existence of organic binder bond methylcellulose gum, easily form the uneven phenomenon of volatilization in the coating after sintering, cause coating to become fragile.TUFI (Toughened Unipiece Fibrous Insulation) coating strengthens application on ceramic tile AETB at adiabatic watt of s-generation rigidity thermal insulation tile refractory fibre matrix material FRCI and aluminum oxide.With air spray finishing by glass bond and high radiation agent MoSi
2mixture be applied on porous-substrates, to improve watt a top density, its ability of resisting destruction improves several times than reaction solidified coating RCG, and has good weather resistance.
Summary of the invention
The present invention will solve Rigid Porous ceramic insulation watt easily water suction, oxidation-resistance and the low technical problem of heat emissivity coefficient, and provides a kind of preparation method of rigid ceramic thermal insulation tile top coat.
A preparation method for rigid ceramic thermal insulation tile top coat, specifically carries out according to following steps:
One, by borosilicate glass powder and melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1, by borosilicate glass powder in mass fraction raw material powder 1 40 ~ 60 parts, melt of si O
2powder is 40 ~ 60 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder and SiB
4powder Homogeneous phase mixing, obtains raw material powder 2, is 30 ~ 40 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 2
2powder is 30 ~ 40 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder, SiB
4powder and ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3, is 20 ~ 30 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 3
2powder is 20 ~ 30 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts, ZrB
2powder is 10 ~ 15 parts;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 1; By mass fraction raw material powder 1 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 300 parts;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 2; By mass fraction raw material powder 2 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 3; By mass fraction raw material powder 3 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Wherein binding agent is tetraethoxy, and agglutinant is norbide;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays three ~ tetra-layers; Spray compound 2 again, spray at least three layers; Spray compound 3 again, spray at least three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, then put into retort furnace, carry out coating sintering, then furnace cooling, obtain rigid ceramic thermal insulation tile top coat.
Described tetraethoxy and norbide are that chemical analysis is pure, and quality purity is 99%.
The present invention is filled a prescription by optimized coatings and controls coating sintering temperature, there is at porous ceramics watt surface construction and base material the composite ceramic coat of close thermal expansivity, this functional coating can meet working condition harsh when hypersonic aircraft reenters, and possesses Aerodynamic Heating to extraradial ability.
The invention has the beneficial effects as follows: the coating microstrueture adopting the present invention to prepare has the Gradient Features of gradual change, and the coating of porous matrix side is vesicular, and top coat is smooth compact shape.The existence of Porous transition layer can coordinate the expansion not matching properties of coating and matrix.Coating of the present invention has lower thermal expansivity 0.8 ~ 3.0 × 10
-6k
-1, the high radiation agent in coating plays the effect of high radiation, and the radiation coefficient of As-deposited state coating is not less than 0.90.According to the experiment needs of Substrate State and working condition, regulate the proportioning of three kinds of mixed slurries, obtain the optimum coating with Matrix Match.
The present invention is for the preparation of rigid ceramic thermal insulation tile top coat.
Accompanying drawing explanation
Fig. 1 is the thermal expansivity graphic representation of rigid ceramic thermal insulation tile top coat prepared by embodiment one ~ tetra-, wherein 1 represents ceramic tile untreatment surface, 2 and represents embodiment one, 3 and represent embodiment two, 4 and represent embodiment three, 5 and represent embodiment four;
Fig. 2 is the cross section electronic scanning figure of rigid ceramic thermal insulation tile top coat prepared by embodiment one;
Fig. 3 is the radiation coefficient graphic representation of rigid ceramic thermal insulation tile top coat after different thermal shock circulation prepared by embodiment two.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of rigid ceramic thermal insulation tile of present embodiment top coat, specifically carry out according to following steps:
One, by borosilicate glass powder and melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1, by borosilicate glass powder in mass fraction raw material powder 1 40 ~ 60 parts, melt of si O
2powder is 40 ~ 60 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder and SiB
4powder Homogeneous phase mixing, obtains raw material powder 2, is 30 ~ 40 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 2
2powder is 30 ~ 40 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder, SiB
4powder and ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3, is 20 ~ 30 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 3
2powder is 20 ~ 30 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts, ZrB
2powder is 10 ~ 15 parts;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 1; By mass fraction raw material powder 1 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 300 parts;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 2; By mass fraction raw material powder 2 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 3; By mass fraction raw material powder 3 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Wherein binding agent is tetraethoxy, and agglutinant is norbide;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays three ~ tetra-layers; Spray compound 2 again, spray at least three layers; Spray compound 3 again, spray at least three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, then put into retort furnace, carry out coating sintering, then furnace cooling, obtain rigid ceramic thermal insulation tile top coat.
Embodiment two: present embodiment and embodiment one unlike: in step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, and wherein boron oxide weight content is 10 ~ 20%.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: in step one, borosilicate glass powder median size is 2 ~ 10 μm; Melt of si O
2siO in powder
2mass content is greater than 98%, and median size is 2 ~ 10 μm; MoSi
2the median size of powder is 1 ~ 4 μm; SiB
4the median size of powder is 10 ~ 50 μm; ZrB
2the median size of powder is 20 ~ 50 μm.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: in step 2, ball material weight ratio is (3 ~ 4): 1.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: in step 2, dispersion agent is pure water.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: the processing parameter of air spray finishing described in step 3 is: air pressure 0.1 ~ 0.3MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 5 ~ 10 centimetres.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one unlike: controlling drying temperature time dry in step 4 is 70 ~ 90 DEG C, and humidity is 40 ~ 50%.Other is identical with embodiment one.
Embodiment eight: present embodiment and embodiment seven unlike: controlling drying temperature time dry in step 4 is 80 DEG C.Other is identical with embodiment seven.
Embodiment nine: present embodiment and embodiment one unlike: described in step 4, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 900 ~ 1100 DEG C of conditions, be incubated 0.5h ~ 1h, controlling temperature rise rate is 5 DEG C/min.Other is identical with embodiment one.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of rigid ceramic thermal insulation tile of the present embodiment top coat, specifically carries out according to following steps:
One, by 50g borosilicate glass powder and 50g melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1;
By 40g borosilicate glass powder, 40g melt of si O
2powder, 10g MoSi
2powder and 10g SiB
4powder Homogeneous phase mixing, obtains raw material powder 2;
By 30g borosilicate glass powder, 30g melt of si O
2powder, 15g MoSi
2powder, 15g SiB
4powder and 10g ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3;
In step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, and wherein boron oxide weight content is 10%;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 1; Raw material powder 1 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1g, dispersion agent is pure water 200g;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 2; Raw material powder 2 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.6g, dispersion agent is pure water 200g;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 3; Raw material powder 3 is 100g, binding agent is tetraethoxy 3g, agglutinant is norbide 0.6g, dispersion agent is pure water 200g;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays three layers; Spray compound 2 again, spray three layers; Spray compound 3 again, spray three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, controlling drying temperature is 80 DEG C, and humidity is 40%, then puts into retort furnace, carry out coating sintering, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 1000 DEG C of conditions, is incubated 1h, and controlling temperature rise rate is 5 DEG C/min, furnace cooling again, obtains rigid ceramic thermal insulation tile top coat;
The processing parameter of air spray finishing described in step 3 is: air pressure 0.2MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 8 centimetres.
Embodiment two:
The preparation method of a kind of rigid ceramic thermal insulation tile of the present embodiment top coat, specifically carries out according to following steps:
One, by 60g borosilicate glass powder and 40g melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1;
By 40g borosilicate glass powder, 30g melt of si O
2powder, 15g MoSi
2powder and 15g SiB
4powder Homogeneous phase mixing, obtains raw material powder 2;
By 40g borosilicate glass powder, 20g melt of si O
2powder, 15g MoSi
2powder, 15g SiB
4powder and 10g ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3;
In step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, and wherein boron oxide weight content is 15%;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 1; Raw material powder 1 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.2g, dispersion agent is pure water 300g;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 2; Raw material powder 2 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.6g, dispersion agent is pure water 220g;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 3; Raw material powder 3 is 100g, binding agent is tetraethoxy 3g, agglutinant is norbide 0.6g, dispersion agent is pure water 220g;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays four layers; Spray compound 2 again, spray four layers; Spray compound 3 again, spray four layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, controlling drying temperature is 90 DEG C, and humidity is 40%, then puts into retort furnace, carry out coating sintering, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 1000 DEG C of conditions, is incubated 1h, and controlling temperature rise rate is 5 DEG C/min, furnace cooling again, obtains rigid ceramic thermal insulation tile top coat;
The processing parameter of air spray finishing described in step 3 is: air pressure 0.2MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 8 centimetres.
Embodiment three:
The preparation method of a kind of rigid ceramic thermal insulation tile of the present embodiment top coat, specifically carries out according to following steps:
One, by 40g borosilicate glass powder and 60g melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1;
By 40g borosilicate glass powder, 30g melt of si O
2powder, 20g MoSi
2powder and 10g SiB
4powder Homogeneous phase mixing, obtains raw material powder 2;
By 40g borosilicate glass powder, 20g melt of si O
2powder, 10g MoSi
2powder, 15g SiB
4powder and 15g ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3;
In step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, and wherein boron oxide weight content is 20%;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 1; Raw material powder 1 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.2g, dispersion agent is pure water 250g;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 2; Raw material powder 2 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.6g, dispersion agent is pure water 220g;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 3; Raw material powder 3 is 100g, binding agent is tetraethoxy 3g, agglutinant is norbide 0.6g, dispersion agent is pure water 220g;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays four layers; Spray compound 2 again, spray four layers; Spray compound 3 again, spray three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, controlling drying temperature is 90 DEG C, and humidity is 50%, then puts into retort furnace, carry out coating sintering, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 1000 DEG C of conditions, is incubated 1h, and controlling temperature rise rate is 5 DEG C/min, furnace cooling again, obtains rigid ceramic thermal insulation tile top coat;
The processing parameter of air spray finishing described in step 3 is: air pressure 0.2MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 8 centimetres.
Embodiment four:
The preparation method of a kind of rigid ceramic thermal insulation tile of the present embodiment top coat, specifically carries out according to following steps:
One, by 55g borosilicate glass powder and 45g melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1;
By 30g borosilicate glass powder, 40g melt of si O
2powder, 20g MoSi
2powder and 10g SiB
4powder Homogeneous phase mixing, obtains raw material powder 2;
By 30g borosilicate glass powder, 30g melt of si O
2powder, 10g MoSi
2powder, 15g SiB
4powder and 15g ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3;
In step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, and wherein boron oxide weight content is 20%;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 1; Raw material powder 1 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.2g, dispersion agent is pure water 250g;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 2; Raw material powder 2 is 100g, binding agent is tetraethoxy 5g, agglutinant is norbide 1.6g, dispersion agent is pure water 220g;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 20min, obtain compound 3; Raw material powder 3 is 100g, binding agent is tetraethoxy 3g, agglutinant is norbide 0.8g, dispersion agent is pure water 220g;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays three layers; Spray compound 2 again, spray four layers; Spray compound 3 again, spray three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, controlling drying temperature is 90 DEG C, and humidity is 40%, then puts into retort furnace, carry out coating sintering, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 1000 DEG C of conditions, is incubated 1h, and controlling temperature rise rate is 5 DEG C/min, furnace cooling again, obtains rigid ceramic thermal insulation tile top coat;
The processing parameter of air spray finishing described in step 3 is: air pressure 0.2MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 8 centimetres.
As shown in Figure 1, wherein 1 untreatment surface, 2 representing ceramic insulation watt represents embodiment one, 3 and represents embodiment two, 4 and represent embodiment three, 5 and represent embodiment four the thermal expansivity graphic representation of rigid ceramic thermal insulation tile top coat prepared by embodiment one ~ tetra-.
The cross section electronic scanning figure of rigid ceramic thermal insulation tile top coat prepared by embodiment one as shown in Figure 2.
The radiation coefficient graphic representation of the rigid ceramic thermal insulation tile top coat prepared of embodiment two after different thermal shock circulation as shown in Figure 3.
From accompanying drawing, adopting the air spraying method of low cost can obtain on rigid ceramic thermal insulation tile surface, thermal expansivity is low, thermal shock resistance good and have the high radiation coating of porous microstructure characteristic.
Claims (9)
1. a preparation method for rigid ceramic thermal insulation tile top coat, is characterized in that what the method was specifically carried out according to following steps:
One, by borosilicate glass powder and melt of si O
2powder Homogeneous phase mixing, obtains raw material powder 1, by borosilicate glass powder in mass fraction raw material powder 1 40 ~ 60 parts, melt of si O
2powder is 40 ~ 60 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder and SiB
4powder Homogeneous phase mixing, obtains raw material powder 2, is 30 ~ 40 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 2
2powder is 30 ~ 40 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts;
By borosilicate glass powder, melt of si O
2powder, MoSi
2powder, SiB
4powder and ZrB
2powder Homogeneous phase mixing, obtains raw material powder 3, is 20 ~ 30 parts, melt of si O by borosilicate glass powder in mass fraction raw material powder 3
2powder is 20 ~ 30 parts, MoSi
2powder is 10 ~ 20 parts, SiB
4powder is 10 ~ 20 parts, ZrB
2powder is 10 ~ 15 parts;
Two, put into ball grinder after the raw material powder 1 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 1; By mass fraction raw material powder 1 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 300 parts;
Put into ball grinder after the raw material powder 2 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 2; By mass fraction raw material powder 2 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Put into ball grinder after the raw material powder 3 step one obtained, binding agent, agglutinant and dispersion agent Homogeneous phase mixing, ball milling 10 ~ 30min, obtain compound 3; By mass fraction raw material powder 3 be 100 parts, binding agent is 1 ~ 5 part, agglutinant is 0.5 ~ 1 part, dispersion agent is 150 ~ 250 parts;
Wherein binding agent is tetraethoxy, and agglutinant is norbide;
Three, pre-treatment is carried out on ceramic insulation watt surface, compound 1 even application then adopting air spray finishing step 2 to be obtained, on ceramic insulation watt surface, sprays three ~ tetra-layers; Spray compound 2 again, spray at least three layers; Spray compound 3 again, spray at least three layers, obtain the coating of uniform ground on ceramic insulation watt surface;
Four, the ceramic insulation of step 3 process watt is put into climatic chamber, carry out drying, then put into retort furnace, carry out coating sintering, then furnace cooling, obtain rigid ceramic thermal insulation tile top coat.
2. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, it is characterized in that in step one, borosilicate glass powder is synthesized through high temperature 1100 DEG C of meltings by silicon oxide and boron oxide, wherein boron oxide weight content is 10 ~ 20%.
3. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, is characterized in that in step one, borosilicate glass powder median size is 2 ~ 10 μm; Melt of si O
2siO in powder
2mass content is greater than 98%, and median size is 2 ~ 10 μm; MoSi
2the median size of powder is 1 ~ 4 μm; SiB
4the median size of powder is 10 ~ 50 μm; ZrB
2the median size of powder is 20 ~ 50 μm.
4. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, is characterized in that in step 2, ball material weight ratio is (3 ~ 4): 1.
5. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, is characterized in that in step 2, dispersion agent is pure water.
6. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, it is characterized in that the processing parameter of air spray finishing described in step 3 is: air pressure 0.1 ~ 0.3MPa, nozzle perpendicular to by sprayed surface, gun slot distance sprayed surface 5 ~ 10 centimetres.
7. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, controlling drying temperature when it is characterized in that dry in step 4 is 70 ~ 90 DEG C, and humidity is 40 ~ 50%.
8. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 7, controlling drying temperature when it is characterized in that dry in step 4 is 80 DEG C.
9. the preparation method of a kind of rigid ceramic thermal insulation tile top coat according to claim 1, it is characterized in that described in step 4, coating sintering process is: under temperature is 200 DEG C of conditions, be incubated 0.5h, then under temperature is 900 ~ 1100 DEG C of conditions, be incubated 0.5h ~ 1h, controlling temperature rise rate is 5 DEG C/min.
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| CN201510178042.9A CN104860717B (en) | 2015-04-15 | 2015-04-15 | A kind of preparation method of rigid ceramic thermal insulation tile face coat |
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| CN105198480A (en) * | 2015-10-29 | 2015-12-30 | 中原工学院 | Preparation method of molybdenum disilicide/silicon carbide composite porous ceramic |
| CN105502946A (en) * | 2015-09-30 | 2016-04-20 | 航天特种材料及工艺技术研究所 | High-emissivity glass glaze and method for preparation of high-emissivity coating from high-emissivity glass glaze |
| CN106083115A (en) * | 2016-06-12 | 2016-11-09 | 山东工业陶瓷研究设计院有限公司 | Thermal insulation tile coating of resistance to 1500 DEG C of high temperature and preparation method thereof |
| CN106380205A (en) * | 2016-08-29 | 2017-02-08 | 天津大学 | BAS-based high temperature-resistant emission coating and preparation method thereof |
| CN107556885A (en) * | 2017-10-26 | 2018-01-09 | 中国科学院理化技术研究所 | Near-infrared radiation ceramic coating for ethylene cracking furnace and preparation method and application thereof |
| CN107603286A (en) * | 2017-09-11 | 2018-01-19 | 山东工业陶瓷研究设计院有限公司 | Rigid thermal insulation tile coating of unburned 1500 DEG C of heatproof and preparation method thereof |
| CN108658626A (en) * | 2018-05-25 | 2018-10-16 | 莱芜亚赛陶瓷技术有限公司 | MoSi2-SiO2Borosilicate coating with thermostability and high emissivity and the preparation method and application thereof |
| CN110342916A (en) * | 2019-08-20 | 2019-10-18 | 北京电子工程总体研究所 | The powder of high temperature resistant height radiation, includes its coating paste, coating and application at its preparation |
| CN113024280A (en) * | 2021-02-26 | 2021-06-25 | 天津大学 | Preparation method of double-layer silicon-oxygen-carbon composite ceramic coating for porous ceramic heat insulation matrix |
| CN113307659A (en) * | 2021-06-10 | 2021-08-27 | 航天特种材料及工艺技术研究所 | Preparation method for forming high-emissivity coating on heat insulation tile |
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| CN105502946A (en) * | 2015-09-30 | 2016-04-20 | 航天特种材料及工艺技术研究所 | High-emissivity glass glaze and method for preparation of high-emissivity coating from high-emissivity glass glaze |
| CN105502946B (en) * | 2015-09-30 | 2017-11-10 | 航天特种材料及工艺技术研究所 | A kind of high emissivity glass glaze and the method that high emissivity coating is prepared by the glaze |
| CN105198480A (en) * | 2015-10-29 | 2015-12-30 | 中原工学院 | Preparation method of molybdenum disilicide/silicon carbide composite porous ceramic |
| CN106083115A (en) * | 2016-06-12 | 2016-11-09 | 山东工业陶瓷研究设计院有限公司 | Thermal insulation tile coating of resistance to 1500 DEG C of high temperature and preparation method thereof |
| CN106083115B (en) * | 2016-06-12 | 2019-07-02 | 山东工业陶瓷研究设计院有限公司 | The thermal insulation tile coating and preparation method thereof of resistance to 1500 DEG C of high temperature |
| CN106380205A (en) * | 2016-08-29 | 2017-02-08 | 天津大学 | BAS-based high temperature-resistant emission coating and preparation method thereof |
| CN107603286A (en) * | 2017-09-11 | 2018-01-19 | 山东工业陶瓷研究设计院有限公司 | Rigid thermal insulation tile coating of unburned 1500 DEG C of heatproof and preparation method thereof |
| CN107603286B (en) * | 2017-09-11 | 2019-08-09 | 山东工业陶瓷研究设计院有限公司 | Rigid thermal insulation tile coating of 1500 DEG C of unburned heatproof and preparation method thereof |
| CN107556885A (en) * | 2017-10-26 | 2018-01-09 | 中国科学院理化技术研究所 | Near-infrared radiation ceramic coating for ethylene cracking furnace and preparation method and application thereof |
| CN108658626A (en) * | 2018-05-25 | 2018-10-16 | 莱芜亚赛陶瓷技术有限公司 | MoSi2-SiO2Borosilicate coating with thermostability and high emissivity and the preparation method and application thereof |
| CN110342916A (en) * | 2019-08-20 | 2019-10-18 | 北京电子工程总体研究所 | The powder of high temperature resistant height radiation, includes its coating paste, coating and application at its preparation |
| CN110342916B (en) * | 2019-08-20 | 2021-11-30 | 北京电子工程总体研究所 | High-temperature-resistant and high-radiation-resistant powder, preparation thereof, coating slurry containing same, coating and application |
| CN113024280A (en) * | 2021-02-26 | 2021-06-25 | 天津大学 | Preparation method of double-layer silicon-oxygen-carbon composite ceramic coating for porous ceramic heat insulation matrix |
| CN113307659A (en) * | 2021-06-10 | 2021-08-27 | 航天特种材料及工艺技术研究所 | Preparation method for forming high-emissivity coating on heat insulation tile |
| CN113307659B (en) * | 2021-06-10 | 2022-04-08 | 航天特种材料及工艺技术研究所 | Preparation method for forming high-emissivity coating on heat insulation tile |
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