CN103553709B - Preparation method of POSS (polyhedral oligomeric silsesquioxane) based high-emissivity nano coating - Google Patents
Preparation method of POSS (polyhedral oligomeric silsesquioxane) based high-emissivity nano coating Download PDFInfo
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- 239000002103 nanocoating Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 54
- 239000011248 coating agent Substances 0.000 claims abstract description 53
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- 238000010792 warming Methods 0.000 claims description 36
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 26
- 229960004756 ethanol Drugs 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000011819 refractory material Substances 0.000 claims description 15
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 13
- 235000019253 formic acid Nutrition 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 238000012423 maintenance Methods 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 9
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001238 wet grinding Methods 0.000 claims description 8
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- 229910021343 molybdenum disilicide Inorganic materials 0.000 claims description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 abstract description 10
- 238000001035 drying Methods 0.000 abstract 1
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- 238000009413 insulation Methods 0.000 description 14
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- 230000000694 effects Effects 0.000 description 4
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical group [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
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- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a preparation method of a POSS (polyhedral oligomeric silsesquioxane) based high-emissivity nano coating, relating to a preparation method of an infrared high-emissivity nano coating. The invention aims to solve the technical problems that the existing infrared coating is poor in film-forming property and a film layer is cracked easily. The preparation method comprises the steps of mixing a POSS sol and an ethanol solution of boric acid, then adding a high-temperature resistant base material and an additive subjected to ball milling, and uniformly mixing to obtain a coating material; coating a boric acid-POSS solution on the surface of a fireproof material matrix, then drying to obtain a transition layer, then coating the coating material on the transition layer, and performing heat treatment to obtain the POSS based high-emissivity nano coating. The POSS sol can be easily coated into a film and has self-healing performance after micro-crack thermal cycle, the emissivity of the nano coating to infrared rays of which the wavelength is 11-18 microns is more than 0.9, and the emissivity value to infrared rays of which the wavelength is 15 microns reaches 0.95, so that the POSS based high-emissivity nano coating can be used in an industrial kiln.
Description
Technical field
The present invention relates to the preparation method of infrared high emissivity coating.
Background technology
Infrared coating, as a kind of novel energy-saving material, industrial furnace, domestic burners has extraordinary energy-saving effect.From the angle of radiative transfer, due to the emissivity of infrared coating high (more than 0.80), the heat that the overwhelming majority absorbs by infrared coating is radiated on heated object with ultrared form, substantially increases thermo-efficiency.So High Radiation Ability Far-infrared Coating has broad application prospects.
Infrared radiant material refers to the material within the scope of infrared band with high emissivity or characteristic emission rate.The ir radiation of material produces because its particle vibration causes moment of dipole to change, and during the particle vibration of material inside, symmetry is lower, and moment of dipole changes greatly, and its infrared intensity is also stronger.Due to the material of the macromolecular structure that stupalith is mostly made up of polyion, the symmetry of polyion malleable molecule in vibration processes and moment of dipole is changed, therefore most stupalith has higher radiant ratio.Existing infrared radiation coating, with inorganic adhesive preparation, the film-forming properties of coating is poor, and rete is easy to crack.
Summary of the invention
The present invention is that will to solve existing infrared coating film-forming properties poor, the technical problem that rete is easy to crack, and provides a kind of preparation method of POSS base high emissivity nano coating.
The preparation method of a kind of POSS base high emissivity nano coating of the present invention, carries out according to the following steps:
One, 10 parts of silane coupling agent JH-50, the ethanol of 9 ~ 10 parts and the acetic acid of 3 ~ 4 parts and 1 ~ 2 part of formic acid is taken by weight; First ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, then add formic acid, after stirring, sealing, being placed on temperature is hydrolysis reaction 7 ~ 8 days in the water-bath of 30 ~ 35 DEG C, obtains POSS colloidal sol;
This POSS colloidal sol is the vitreosol with certain viscosity.
Two, take ethanol as the ethanolic soln that boric acid prepared by solvent, the mass percentage concentration of its mesoboric acid is 10% ~ 15%; Be that the ethanolic soln of boric acid mixes with POSS colloidal sol by 18 ~ 20:1 by the ethanolic soln of boric acid and the mass ratio of POSS colloidal sol again, obtain boric acid-POSS solution;
Three, take the high temperature resistant base-material of 10 parts and the additive of 2 ~ 4 parts by weight, wherein high temperature resistant base-material is molybdenum disilicide (MoSi
2), a kind of or wherein several combination in silicon carbide (SiC), zirconium white (ZrO), silicon oxide, additive is aluminum oxide, after mixing, obtains powder;
Four, powder and dehydrated alcohol to be added in planetary ball mill wet-milling 8 ~ 10 hours, obtain nano pulp;
During wet-milling, the add-on of ethanol there was not the rotor of ball mill, and the mobility of base-material during to ensure ball milling, after ball milling, the granularity of powder is nano level.
Five, be that the nano pulp that step 4 obtains by 8 ~ 10:1 mixes with the boric acid-POSS solution that step 2 obtains by nano pulp and the mass ratio of boric acid-POSS solution, obtain coating;
Six, boric acid-POSS solution refractory material matrix surface coating step two obtained, dry 30 ~ 40min under the condition of 20 ~ 30 DEG C, be warming up to 70 ~ 80 DEG C again and keep 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min, obtain transition layer;
Seven, the coating that coating step five obtains on the transition layer of refractory material matrix, dry 30 ~ 40min at 40 ~ 50 DEG C, then be warming up to 70 ~ 80 DEG C of maintenance 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min;
Eight, the refractory material matrix through step 7 process is put into retort furnace, after temperature is 300 ~ 320 DEG C of maintenance 30 ~ 40min, be warming up to 500 ~ 520 DEG C again and keep 50 ~ 60min, be finally warming up to 650 ~ 700 DEG C and keep 30 ~ 60min, obtain POSS base high emissivity nano coating.
The present invention's employing sol-gel method, adopt formic acid as the vitreosol of catalyzer synthesis thickness, i.e. POSS colloidal sol, after POSS colloidal sol mixes with the ethanolic soln of boric acid, obtains boric acid-POSS solution; Mix after the nano particle ball milling of high temperature resistant base-material and additive with boric acid-POSS solution, make coating; Refractory material matrix surface is coated with boric acid-POSS solution as transition layer, then by paint on transition layer, high temperature sintering obtains POSS base high emissivity nano coating.
The silicon boron glass produced in high temperature resistant base-material, additive and sintering process in coating of the present invention is nano level, and under sintering condition of the present invention, in coating, microcrystalline growth is controlled, the crystal grain obtained is tiny and be evenly distributed, this all significantly reduces the scattering coefficient of radiation paint, improve the infrared radiation property of coating, make infrared radiation coating kiln at relatively high temperatures plays excellent effect.
Have employed POSS colloidal sol in coating preparation process of the present invention, POSS colloidal sol easily applies film forming, and can not form solid breeze during POSS colloidal sol pyrolytic decomposition, but forms one deck SiO
2ceramic protective layer or melts, product after organic constituent high temperature carbonization more can be conducive to the high emissivity improving coating, the corresponding physical and mechanical properties of POSS hybrid material under hot conditions will be caused the adding of suitable type is high temperature resistant base-material and additive, rheological property, heat physical properties and other performance change, under raw material of the present invention and preparation condition, by POSS bulk effect, the migration of resultant and the filling to crackle, the self-healing after tiny crack thermal cycling can be realized, therefore by the introducing of POSS, and adjust kind and the dosage of high temperature resistant base-material and additive in slurry, realize the raising to material thermal emissivity rate, the POSS base high temperature thermal insulation coating of final acquisition performance optimization.
First the present invention selects the Al that emittance is high
2o
3, MoSi
2, SiC, ZrO be as high radiation agent material, then obtain by ball milling method the good slurry that is uniformly dispersed, select POSS colloidal sol as binding agent, and adopt multiple material Composite, enable the radiation characteristic of various material in the wave band of differing temps scope and different wave length complementary and mutually strengthen, and then improve coatings emissivity.POSS base high emissivity nano coating of the present invention is that the ultrared emittance of 11 μm ~ 18 μm is all higher to wavelength, substantially remains on more than 0.9, reaches 0.95, can be used in Industrial Stoves in the ultrared emittance value to wavelength being 15 μm.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the POSS base high emissivity nano coating that test 1 obtains on thermal insulation tile;
Fig. 2 is the emittance curve of the POSS base high emissivity nano coating that test 1 obtains on thermal insulation tile.
Fig. 3 is that to be placed on temperature be respectively burn 30min in the stove of 800 DEG C and 1100 DEG C for prepared by test 1 thermal insulation tile scribbling high emission coating, and simulation scribbles the situation of thermal insulation tile in kiln of high emission coating, takes out to do X-ray diffraction and test after burning, the XRD spectra obtained; Wherein a is the X-ray diffraction spectrogram of the high emission coating under 1100 DEG C of conditions after sintering processes, and b is the X-ray diffraction spectrogram of the high emission coating under 800 DEG C of conditions after sintering processes.
Embodiment
Embodiment one: the preparation method of a kind of POSS base high emissivity nano coating of present embodiment, carry out according to the following steps:
One, 10 parts of silane coupling agent JH-50, the ethanol of 9 ~ 10 parts and the acetic acid of 3 ~ 4 parts and 1 ~ 2 part of formic acid is taken by weight; First ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, then add formic acid, after stirring, sealing, being placed on temperature is hydrolysis reaction 7 ~ 8 days in the water-bath of 30 ~ 35 DEG C, obtains POSS colloidal sol;
This POSS colloidal sol is the vitreosol with certain viscosity.
Two, take ethanol as the ethanolic soln that boric acid prepared by solvent, the mass percentage concentration of its mesoboric acid is 10% ~ 15%; Be that the ethanolic soln of boric acid mixes with POSS colloidal sol by 18 ~ 20:1 by the ethanolic soln of boric acid and the mass ratio of POSS colloidal sol again, obtain boric acid-POSS solution;
Three, take the high temperature resistant base-material of 10 parts and the additive of 2 ~ 4 parts by weight, wherein high temperature resistant base-material is molybdenum disilicide (MoSi
2), a kind of or wherein several combination in silicon carbide (SiC), zirconium white (ZrO), silicon oxide, additive is aluminum oxide, after mixing, obtains powder;
Four, powder and dehydrated alcohol to be added in planetary ball mill wet-milling 8 ~ 10 hours, obtain nano pulp;
During wet-milling, the add-on of ethanol there was not the rotor of ball mill, the mobility of base-material during to ensure ball milling, and after ball milling, the granularity of powder is nano level;
Five, be that the nano pulp that step 4 obtains by 8 ~ 10:1 mixes with the boric acid-POSS solution that step 2 obtains by nano pulp and the mass ratio of boric acid-POSS solution, obtain coating;
Six, boric acid-POSS solution refractory material matrix surface coating step two obtained, dry 30 ~ 40min under the condition of 20 ~ 30 DEG C, be warming up to 70 ~ 80 DEG C again and keep 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min, obtain transition layer;
Seven, the coating that coating step five obtains on the transition layer of refractory material matrix, dry 30 ~ 40min at 40 ~ 50 DEG C, then be warming up to 70 ~ 80 DEG C of maintenance 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min;
Eight, the refractory material matrix through step 7 process is put into retort furnace, after temperature is 300 ~ 320 DEG C of maintenance 30 ~ 40min, be warming up to 500 ~ 520 DEG C again and keep 50 ~ 60min, be finally warming up to 650 ~ 700 DEG C and keep 30 ~ 60min, obtain POSS base high emissivity nano coating.
This enforcement, the migration of mode by POSS bulk effect, resultant and the filling to crackle can realize the self-healing after tiny crack thermal cycling, the POSS base high emissivity nano coating of present embodiment is applicable to various matrix, to the strong adhesion of matrix, be applicable to reaction atmosphere, long-term durability is good, heat shock resistance ability to bear is strong, can thermo-efficiency be improved, reduce substrate temperature, improve the work-ing life of matrix.
Embodiment two: present embodiment and embodiment one are unlike taking 10 parts of silane coupling agent JH-50, the ethanol of 9.5 parts and the acetic acid of 3.5 parts and 1.5 parts of formic acid in step one by weight, first ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, add formic acid again, after stirring, sealing, being placed on temperature is hydrolysis reaction 7.5 days in the water-bath of 32 DEG C, obtains POSS colloidal sol; Other are identical with embodiment one.
This POSS colloidal sol is the vitreosol with certain viscosity.
Embodiment three: present embodiment and embodiment one or two are (18.5 ~ 19.5) unlike the ethanolic soln of step 2 mesoboric acid and the mass ratio of POSS colloidal sol: 1.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are the molybdenum disilicide (MoSi combined by any mass ratio unlike base-material high temperature resistant in step 3
2), silicon carbide (SiC) and zirconium white (ZrO).Other are identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to three are the molybdenum disilicide (MoSi combined by any mass ratio unlike base-material high temperature resistant in step 3
2), silicon carbide (SiC) and silicon oxide (SiO
2).Other are identical with one of embodiment one to three.
Embodiment six: one of present embodiment and embodiment one to five are unlike in step 4, powder and dehydrated alcohol being added in planetary ball mill wet-milling 9 hours.Other are identical with one of embodiment one to five.
During wet-milling, the add-on of ethanol there was not the rotor of ball mill, and the mobility of base-material during to ensure ball milling, after ball milling, the granularity of powder is nano level.
Embodiment seven: one of present embodiment and embodiment one to six are 9:1 unlike the mass ratio of nano pulp in step 5 and boric acid-POSS solution.Other are identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike in step 6 under the condition of 25 DEG C dry 35min, then be warming up to 75 DEG C keep 110min, be then warming up to 115 DEG C keep 35min.Other are identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike after applying coating in step 7 on the transition layer of refractory material matrix, dry 35min at 45 DEG C, be warming up to 75 DEG C again and keep 110min, be then warming up to 115 DEG C and keep 35min.Other are identical with one of embodiment one to eight.
Embodiment ten: the refractory material matrix through step 7 process is put into retort furnace unlike in step 8 by one of present embodiment and embodiment one to nine, after temperature is 310 DEG C of maintenance 35min, be warming up to 510 DEG C again and keep 55min, finally be warming up to 670 DEG C and keep 40min, obtain POSS base high emissivity nano coating.Other are identical with one of embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten are metal unlike the refractory material matrix described in step 6 is pottery.Other are identical with one of embodiment one to ten.
With following verification experimental verification beneficial effect of the present invention:
Test 1: the preparation method of the POSS base high emissivity nano coating of this test, carry out according to the following steps:
One, 10 parts of silane coupling agent JH-50, the ethanol of 10 parts and the acetic acid of 3 parts and 2 parts of formic acid are taken by ratio of weight and the number of copies, first ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, add formic acid again, after stirring, sealing, being placed on temperature is hydrolysis reaction 7 days in the water-bath of 30 DEG C, obtain POSS colloidal sol, this POSS colloidal sol is vitreosol;
Two, take ethanol as the ethanolic soln that boric acid prepared by solvent, the mass percentage concentration of its mesoboric acid is 15%; Be that the ethanolic soln of boric acid mixes with POSS colloidal sol by 20:1 by the ethanolic soln of boric acid and the mass ratio of POSS colloidal sol again, obtain boric acid-POSS solution;
Three, take the high temperature resistant base-material of 10 parts and the additive of 3.3 parts by weight, wherein high temperature resistant base-material by mass percentage by 44.5% molybdenum silicide powder (MoSi
2), the carborundum powder (SiC) of 33.3%, the cobalt oxide powder (Co of 22.2%
2o
3) composition, additive is aluminum oxide, after mixing, obtains powder, and wherein the particle diameter of molybdenum silicide powder, carborundum powder, cobalt oxide powder is 80 ~ 120nm;
Four, powder and dehydrated alcohol to be added in planetary ball mill ball milling 8 hours, obtain slurry; Wherein the add-on of dehydrated alcohol there was not the rotor of ball mill;
Five, be that the slurry that step 4 obtains by 10:1 mixes with the boric acid-POSS solution that step 2 obtains by slurry and the mass ratio of boric acid-POSS solution, obtain coating;
Six, thermal insulation tile cuts into the square of 3cmx3cmx0.5cm, it is the sand papering smooth of 800 by surface fineness, clean rear dry with ethanol purge again, then at the boric acid-POSS solution that thermal insulation tile surface coating step two obtains, dry 30min under the condition of 30 DEG C, be warming up to 80 DEG C again and keep 120min, be then warming up to 120 DEG C and keep 30min, obtain transition layer;
Seven, the coating that coating step five obtains on the transition layer of thermal insulation tile, dry 30min at 50 DEG C, then be warming up to 80 DEG C of maintenance 120min, be then warming up to 120 DEG C and keep 30min;
Eight, the thermal insulation tile through step 7 process is put into retort furnace, be after keeping 30min under the condition of 300 DEG C in temperature, first be warming up to 500 DEG C again with the heat-up rate of 10 DEG C/min again and keep 60min, then be warming up to 700 DEG C of maintenance 30min, obtain POSS base high emissivity nano coating.
As shown in Figure 1, as can be seen from Figure 1, coating is smooth for the stereoscan photograph of the POSS base high emissivity nano coating that this test 1 obtains on thermal insulation tile, and without obvious bubbling, efflorescence, the phenomenon of cracking, this can improve the work-ing life of rete greatly.This test adopts boric acid-POSS solution as binding agent, forms external phase, wherein the metal crystal conversion of crystal, enhances the free carrier of material and the transition of electron radiation mechanism of impurity level, improve the full wave infrared radiation property of material.
The emittance curve of the POSS base high emissivity nano coating that this test 1 obtains on thermal insulation tile as shown in Figure 2, as can be seen from Figure 2, within the scope of 2.5 ~ 11 μm, the trend of emittance change raises along with the increase of wavelength, increasing degree is larger, 11 μm time, reach maximum value 0.90.To in 11 μm ~ 18 μm processes, emittance value is all higher, substantially remains on more than 0.9, and 15 μm time, reach maximum 0.95, after 18 μm, emittance slightly declines, and afterwards again in increase tendency, fluctuates larger.According to the data of Fig. 2, the coating thermal emissivity rate of this test preparation is high, can improve thermo-efficiency.
The thermal insulation tile scribbling high emission coating prepared by this test 1 being placed on respectively temperature is burn 30min in the stove of 800 DEG C and 1100 DEG C, simulation scribbles the situation of thermal insulation tile in kiln of high emission coating, take out after burning and do X-ray diffraction test, as shown in Figure 3, wherein a is the X-ray diffraction spectrogram of the high emission coating under 1100 DEG C of conditions after sintering processes to the XRD spectra obtained; B is the X-ray diffraction spectrogram of the high emission coating under 800 DEG C of conditions after sintering processes.Can see from spectrogram 3, in the spectrogram of the coating sintered under 1100 DEG C of conditions, dominant is ZrSiO mutually
4, i.e. zircon structure is the ZrSiO of 06-0266 with card number in PDF card
4correspondence, three strongest ones' peak crystal face is respectively (200), (112) and (312), crystal face diffraction angle 2 θ and 26.980 °, 35.626 ° and 53.478 ° corresponding.Meanwhile, Mo (SiAl) is also had
2thing phase and SiO
2generate, be conducive to improving the antioxidant property of coating when high temperature.Its dominant is zircon ZrSiO mutually
4, this structure has good resistance to elevated temperatures.In addition, this structure, because its lattice vibration easily changes, also has good radiance, and namely the generation of this thing phase is conducive to the emittance improving coated material.In the coating that 800 DEG C of sintering obtain, also create zircon, compared with just sinter with 1100 DEG C, zircon structural generation slightly few, compares with standard card, corresponding good when too late 1100 DEG C.Be that the surface scribbling the thermal insulation tile of high emission coating after burning 30min in the stove of 800 DEG C and 1100 DEG C does not all have crackle to occur in temperature.
Claims (10)
1. a preparation method for POSS base high emissivity nano coating, is characterized in that the method is carried out according to the following steps:
One, 10 parts of silane coupling agent JH-50, the ethanol of 9 ~ 10 parts and the acetic acid of 3 ~ 4 parts and 1 ~ 2 part of formic acid is taken by weight; First ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, then add formic acid, after stirring, sealing, being placed on temperature is hydrolysis reaction 7 ~ 8 days in the water-bath of 30 ~ 35 DEG C, obtains POSS colloidal sol;
Two, take ethanol as the ethanolic soln that boric acid prepared by solvent, the mass percentage concentration of its mesoboric acid is 10% ~ 15%; Be that the ethanolic soln of boric acid mixes with POSS colloidal sol by 18 ~ 20:1 by the ethanolic soln of boric acid and the mass ratio of POSS colloidal sol again, obtain boric acid-POSS solution;
Three, the high temperature resistant base-material of 10 parts and the additive of 2 ~ 4 parts is taken by weight, wherein high temperature resistant base-material is a kind of or wherein several combination in molybdenum disilicide, silicon carbide, zirconium white, silicon oxide, additive is aluminum oxide, after mixing, obtains powder;
Four, powder and dehydrated alcohol to be added in planetary ball mill wet-milling 8 ~ 10 hours, obtain nano pulp;
Five, be that the nano pulp that step 4 obtains by 8 ~ 10:1 mixes with the boric acid-POSS solution that step 2 obtains by nano pulp and the mass ratio of boric acid-POSS solution, obtain coating;
Six, boric acid-POSS solution refractory material matrix surface coating step two obtained, dry 30 ~ 40min under the condition of 20 ~ 30 DEG C, be warming up to 70 ~ 80 DEG C again and keep 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min, obtain transition layer;
Seven, the coating that coating step five obtains on the transition layer of refractory material matrix, dry 30 ~ 40min at 40 ~ 50 DEG C, then be warming up to 70 ~ 80 DEG C of maintenance 100 ~ 120min, be then warming up to 110 ~ 120 DEG C and keep 30 ~ 40min;
Eight, the refractory material matrix through step 7 process is put into retort furnace, after temperature is 300 ~ 320 DEG C of maintenance 30 ~ 40min, be warming up to 500 ~ 520 DEG C again and keep 50 ~ 60min, be finally warming up to 650 ~ 700 DEG C and keep 30 ~ 60min, obtain POSS base high emissivity nano coating.
2. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1, it is characterized in that in step one, taking 10 parts of silane coupling agent JH-50, the ethanol of 9.5 parts and the acetic acid of 3.5 parts and 1.5 parts of formic acid by weight, first ethanol and acetic acid are mixed, then join in silane coupling agent JH-50, add formic acid again, after stirring, sealing, being placed on temperature is hydrolysis reaction 7.5 days in the water-bath of 32 DEG C, obtains POSS colloidal sol.
3. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, is characterized in that the ethanolic soln of step 2 mesoboric acid and the mass ratio of POSS colloidal sol are (18.5 ~ 19.5): 1.
4. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, is characterized in that in step 3, high temperature resistant base-material is the molybdenum disilicide, silicon carbide and the zirconium white that combine by any mass ratio.
5. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, is characterized in that in step 3, high temperature resistant base-material is the molybdenum disilicide, silicon carbide and the silicon oxide that combine by any mass ratio.
6. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, to is characterized in that powder and dehydrated alcohol being added in step 4 in planetary ball mill wet-milling 9 hours.
7. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, is characterized in that the mass ratio of nano pulp and boric acid-POSS solution in step 5 is 9:1.
8. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, to is characterized in that in step 6 dry 35min under the condition of 25 DEG C, then is warming up to 75 DEG C and keeps 110min, is then warming up to 115 DEG C and keeps 35min.
9. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, after it is characterized in that applying coating in step 7 on the transition layer of refractory material matrix, dry 35min at 45 DEG C, be warming up to 75 DEG C again and keep 110min, be then warming up to 115 DEG C and keep 35min.
10. the preparation method of a kind of POSS base high emissivity nano coating according to claim 1 and 2, it is characterized in that, in step 8, the refractory material matrix through step 7 process is put into retort furnace, after temperature is 310 DEG C of maintenance 35min, be warming up to 510 DEG C again and keep 55min, finally be warming up to 670 DEG C and keep 40min, obtain POSS base high emissivity nano coating.
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| CN111533563A (en) * | 2020-05-20 | 2020-08-14 | 国装新材料技术(江苏)有限公司 | POSS (polyhedral oligomeric silsesquioxane) functionalized alumina ceramic fiber and sol-gel spinning preparation method thereof |
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