CN108558443A - A kind of preparation method and application method of nano modification mullite ceramic coating - Google Patents
A kind of preparation method and application method of nano modification mullite ceramic coating Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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Abstract
The present invention relates to a kind of preparation method and application method of nano modification mullite ceramic coating, wherein preparation method is：Lithium tetraborate, Sodium azide and metal magnesium powder are reacted in Muffle furnace high temperature, obtained product is reacted with salt acid soak, and obtained product is dried to obtain nano modifier；Mullite precursor is prepared using sol-gal process；Nano modifier is added after mullite precursor dispersant is disperseed to be modified.Application method is：Ceramic matrix is coated using Best-Effort request device in nano modification mullite ceramic coating first, then the ceramic matrix after coating is sintered.The defects of preparation method of the nano modification mullite ceramic coating of the present invention, the mullite ceramic coating prepared coating when applying is less prone to crackle and cavity, improves barrier propterty and the protection service life of coating；The application method of the nano modification mullite ceramic coating of the present invention, easy to operate, use cost is cheap, and coating works well, and coating is hardly damaged.
Description
Technical field
The present invention relates to paint field more particularly to a kind of hexagonal phase boron nitride two-dimensional nano piece modification mullite ceramic are anti-
The preparation method of oxidation coating.
Background technology
High-temperature oxidation resistant coating is the effective technical way for solving material at high temperature problem of oxidation, in aerospace, metallurgy, energy
The fields such as source and chemical industry have wide application.
Since mullite ceramic has high temperature phase stability good, excellent in mechanical performance, anti-thermal shock/thermal cycling capability is strong, resistance to
The series of advantages such as corrosive environment become a kind of ideal antioxidant coating material system.Currently, occurred one
The technical solution of a little coatings that ceramic matrix is served as using mullite ceramic coating.
But mullite ceramic coating make coating because of the intrinsic brittleness of mullite itself, in practical application, coating
It is easy to the defects of cracked and empty, the antioxygenic property of ceramic coating and thermal shock resistance is caused to be difficult to meet and prevent for a long time
The demand of shield.
In addition, mainly using making for plasma spraying and impregnating slurry using more universal mullite ceramic coating at present
Use mode.Plasma spray coating process equipment is complicated, and cost is higher；Impregnating slurry then there is long preparation period and coating effect it is poor
The shortcomings of causing coating fragile.
Invention content
Existing defect for the above-mentioned prior art, the object of the present invention is to provide a kind of nano modification mullite ceramics
The defects of preparation method of coating, the mullite ceramic coating prepared coating when applying is less prone to crackle and cavity,
Improve barrier propterty and the protection service life of coating.
To achieve the goals above, the technical scheme is that：
A kind of preparation method of nano modification mullite ceramic coating comprising following step：
(1) modifying agent is prepared：
1. dispensing：Lithium tetraborate, Sodium azide and metal magnesium powder are pressed 1~1.5 successively：3~5：4~7 molar ratio ingredient
Mixing is placed in reaction kettle；
2. reacting：It is put into Muffle furnace after the reaction kettle is sealed, the Muffle furnace is set by 5~10 DEG C/minute of clock rates
After rate is warming up to 500~600 DEG C, heat preservation 16~for 24 hours, obtain the first product；
3. pickling：First reactant is put into hydrochloric acid solution after impregnating and stirring 4~6h and is separated by solid-liquid separation, obtained
Solid second product；
4. drying：Second product is dried in vacuo 8~10h at 80~100 DEG C, obtains six sides of white powder
Phase boron nitride two-dimensional nano piece；
(2) precalcining porzite powder is prepared：
1. preparing the first gel：Using aluminum soluble salt, esters of silicon acis as raw material, by Al：Si：H2O：Organic solvent：Catalyst
=(2~3)：(1~1.5)：(5~8)：(20~30)：The molar ratio of (0.3~0.5), which is matched, takes raw material, organic solvent and catalyst
Back flow reaction is carried out later, obtains the first gel；
2. preparing precalcining porzite powder：By first gel after drying with 1200~1350 DEG C of temperature in sky
It is calcined in gas, obtains precalcining porzite powder；
(3) mullite precursor is prepared：
1. preparing the second gel：Using aluminum acetate, esters of silicon acis as raw material, by Al：Si：Organic solvent：Catalyst=(2~3)：
(1~1.5)：(5~8)：(20~30)：The molar ratio of (0.3~0.5), which is matched, takes raw material, organic solvent and catalyst later in 60-
2~4h of back flow reaction at a temperature of 85 DEG C, obtains the second gel；
2. gel water reacts：Al is pressed into second gel：H2O=1：1~2 molar ratio is slowly dropped into deionization
Water, then be warming up to 80~85 DEG C and react 4~6 hours, obtain intermediate；
3. slurrying defibrination：According to intermediate：Precalcining mullite powder=(4~6)：1 mass ratio adds into the intermediate
Enter the precalcining porzite powder, at the same be added 0.3~1wt% of slurry gross mass coalescents and slurry gross mass 5~
The drying retarder of 8wt%, 4~6h of ball milling, obtains mullite precursor；
(4) dispersion and nano modification：
1. disperseing：By the hexagonal phase boron nitride two-dimensional nano piece of 0.2~1wt% of the mullite precursor gross mass
It is mixed into the dispersant of a concentration of 0.01~0.05mol/L, 30~60min of ultrasonic disperse obtains suspension；
2. being modified：By the suspension be added the rotating speed ball milling 20 in the mullite precursor with 120~160rpm~
30min obtains the nano modification mullite ceramic coating.
In some specific embodiments, the pickling the step of in, the volume ratio 1 of the hydrochloric acid solution：1；Institute
In the step of stating pickling, monitors the concentration of the hydrochloric acid solution in real time and the hydrochloric acid solution is replenished in time.
In some specific embodiments, the pickling the step of in, it is described to be separated by solid-liquid separation using by the way of suction filtration.
In some specific embodiments, the reaction the step of and the step of the pickling between, by described first
Absolute ethyl alcohol and deionized water is used alternately to clean again after product natural cooling.
In some specific embodiments, the pickling the step of and between the step of the drying, by described second
Product washes of absolute alcohol.
In some specific embodiments, the aluminum soluble salt is in aluminum nitrate, anhydrous Aluminum chloride and aluminium isopropoxide
It is one or more of；The esters of silicon acis is selected from least one of ethyl orthosilicate, methyl orthosilicate and positive silicic acid propyl ester；It is described to have
Solvent is at least one of absolute ethyl alcohol and absolute methanol；The catalyst is at least one in glacial acetic acid and hydrofluoric acid
Kind；The drying retarder is at least one of oxalic acid and glycerine；The coalescents are polyvinylpyrrolidone and gather
At least one of vinyl butyral；The dispersant is at least one of carboxymethyl cellulose and poly amic acid.
The preparation method of the nano modification mullite ceramic coating of the present invention has beneficial skill below compared with the prior art
Art effect：
Hexagonal phase boron nitride two-dimensional nano piece thermostabilization is good, good with the preparation process compatibility of mullite bonded.Six
Square phase boron nitride is chemically inert material, has good resistance to mild oxidation resistance and lubricity, uses hexagonal phase nitrogen
Change modifying agent of the boron two-dimensional nano piece as coating, in conjunction with its two-dimensional nanostructure so that boron nitride gives full play in coating
Its excellent performance so that mullite ceramic coating is less prone to the defects of crackle and cavity in application, promotes ceramic coating
Barrier propterty and protection service life.
The present invention also provides a kind of application methods of nano modification mullite ceramic coating comprising following steps：
(1) it coats：Ceramic matrix is immersed in the nano modification mullite ceramic coating, using Best-Effort request device into
Row coating obtains coating matrix；
(2) it is sintered：The coating matrix is sintered.
In some specific embodiments, in the coating step, lifting parameter is：The rate of pulling is less than 1mm/min,
40~60 DEG C of temperature is lifted, relative humidity is less than 30%RH, and it is 0.8~1.5L/min to lift the nitrogen flow rate in kettle.
In some specific embodiments, in the sintering step, by the coating matrix with 1500 DEG C of temperature,
It is sintered 3~4 hours under air environment.
The application method of the nano modification mullite ceramic coating of the present invention has skill beneficial below compared with the prior art
Art effect：
Coating coating is carried out by the way of Best-Effort request, is then sintered, simple for process quick and of low cost, shape
At paint coatings coat excellent effect, be hardly damaged.
The present invention is further elaborated With reference to embodiment.
Specific implementation mode
Embodiment 1
Prepare hexagonal phase boron nitride two-dimensional nano piece：First by the lithium tetraborate (Li of 33.80g2B4O7), 39.00g it is folded
Nitrogen sodium (NaN3) and 19.20g 400 mesh metal magnesium powder (Mg) ball milling mixings be uniformly placed on 500mL stainless steel high temperature reaction
It in kettle, is put into Muffle furnace after being sealed, after being warming up to 500 DEG C with 10 DEG C/min of rate, keeps the temperature 18 hours, wait having reacted
Cheng Hou, cooled to room temperature.The product in pyroreaction kettle is taken out successively after absolute ethyl alcohol and deionized water clean 4 times,
It is 1 with volume ratio：1 hydrochloric acid solution is impregnated and is stirred 4 hours, during which should monitor concentration of hydrochloric acid, hydrochloric acid solution is replenished in time.It waits for anti-
Should completely after, filter product and with washes of absolute alcohol 3 times.Finally, the product after cleaning up is placed in vacuum drying chamber
After being dried 10 hours at 80 DEG C, the hexagonal phase boron nitride two-dimensional nano piece of white powder is obtained.
Sol-gel method prepares hexagonal phase boron nitride two-dimensional nano piece and is modified mullite coating：
1) by 10.4165g ethyl orthosilicates and with 56.247gAl (NO3)3·9H2O is dissolved in 14mL ethyl alcohol, is added
It is warming up to 80 DEG C of reaction 12h after 1.800g glacial acetic acid after back flow reaction 4h again under 60 DEG C of heating water baths, will then be obtained by the reaction
Gel drying after to be put into Muffle furnace after 250rpm rotating speed ball millings 2h, after heating rate 5 DEG C/min, 1200 DEG C of heat preservation 2h with
Stove is cooled to room temperature, and precalcining porzite powder is made.
2) after 6.1233g aluminium acetates and 2.4165g ethyl orthosilicates being dissolved in 50mL absolute ethyl alcohols, 1.2g ice vinegar is added
Acid adds in the case where completely cutting off moisture content environment in 60 DEG C of water-baths as being stirred after catalyst after solid reagent is dissolved completely in absolute ethyl alcohol
It is slowly added dropwise again into 3.042g deionized waters after the lower back flow reaction 4h of heat, after then raising temperature to 80 DEG C of reaction 4h, by the nothing of 35mL
The acetone of water-ethanol and 15mL after mixing, are added 0.19g polyvinylpyrrolidones (PVP) and stir to being completely dissolved, then
The oxalic acid of 15g precalcinings porzite powder and 2.5mL is added, it is molten after ball milling 4h to obtain mullite precursor under 250rpm rotating speeds
Glue.
3) take 0.11g hexagonal phase boron nitride two-dimensional nano pieces that ultrasound in the cmc soln of 0.02mol/L is added
After disperseing 30min, it is added in mullite precursor colloidal sol obtained by step 2), is received after ball milling 25min under 150rpm rotating speeds
The modified mullite ceramic coating of rice.
4) in the nano modification mullite ceramic coating for obtaining SiC ceramic matrix immersion step 3), Best-Effort request is utilized
Technology carries out slurry coating, rate of pulling 1mm/min, and lifting environment temperature is 45 DEG C, relative humidity 20%RH, is lifted in kettle
Nitrogen flow rate be 1.5L/min.Hexagonal phase boron nitride two dimension is obtained after being sintered 4h in tube furnace 1500 DEG C after the completion of coating
Nanometer sheet is modified the SiC ceramic material sample of mullite antioxidant coating cladding.
Embodiment 2
Prepare hexagonal phase boron nitride two-dimensional nano piece：First by the lithium tetraborate (Li of 33.80g2B4O7), 63.50g it is folded
Nitrogen sodium (NaN3) and 32.86g 400 mesh metal magnesium powder (Mg) ball milling mixings be uniformly placed on 500mL stainless steel high temperature reaction
It in kettle, is put into Muffle furnace after being sealed, after being warming up to 600 DEG C with 5 DEG C/min of rate, keeps the temperature 24 hours, wait for that reaction is completed
Afterwards, cooled to room temperature.The product in pyroreaction kettle is taken out successively after absolute ethyl alcohol and deionized water clean 4 times, use
Volume ratio is 1：1 hydrochloric acid solution is impregnated and is stirred 4 hours, during which should monitor concentration of hydrochloric acid, hydrochloric acid solution is replenished in time.It waits reacting
After completely, product is filtered and with washes of absolute alcohol 3 times.Finally, the product after cleaning up is placed in vacuum drying chamber
After being dried 8 hours at 80 DEG C, the hexagonal phase boron nitride two-dimensional nano piece of white powder is obtained.
Sol-gel method prepares the crystal whisker toughened mullite external coatings of SiC：
1) by 41.666g ethyl orthosilicates and with 224.988gAl (NO3)3·9H2O is dissolved in 200mL ethyl alcohol, and 30g is added
80 DEG C of reaction 12h are warming up to after glacial acetic acid after back flow reaction 4h again under 60 DEG C of heating water baths, then by gel obtained by the reaction
To be put into Muffle furnace after 250rpm rotating speed ball millings 2h after drying, furnace cooling after heating rate 5 DEG C/min, 1200 DEG C of heat preservation 2h
To room temperature, precalcining porzite powder is made.
2) after 30.6930g aluminium acetates and 8.0852g ethyl orthosilicates being dissolved in 200mL absolute ethyl alcohols, 20g ice is added
Acetic acid after catalyst as stirring, in the case where completely cutting off moisture content environment in 60 DEG C of water-baths after solid reagent is dissolved completely in absolute ethyl alcohol
It is slowly added dropwise again into 8.400g deionized waters after the lower back flow reaction 4h of heating, after then raising temperature to 80 DEG C of reaction 3.5h, by 65mL
Absolute ethyl alcohol and 25mL acetone after mixing, be added 1g polyvinylpyrrolidones (PVP) stir to being completely dissolved, then
27g precalcinings porzite powder is added and obtains mullite precursor colloidal sol after ball milling 4h under 250rpm rotating speeds.
3) take 0.715g hexagonal phase boron nitride two-dimensional nano pieces that ultrasound in the cmc soln of 0.03mol/L is added
After disperseing 30min, it is added in mullite precursor colloidal sol obtained by step 2), is received after ball milling 25min under 150rpm rotating speeds
The modified mullite ceramic coating of rice.
4) nanometer that carbon fibre reinforced silicon carbide (C/SiC) ceramic composite matrix sample immersion step 3) obtains is changed
Property mullite ceramic coating in, utilize Best-Effort request technology carry out slurry coating, rate of pulling 0.8mm/min, lift environment
Temperature is 55 DEG C, relative humidity 10%RH, and it is 1.0L/min to lift the nitrogen flow rate in kettle.In in tube furnace after the completion of coating
The C/SiC potteries that hexagonal phase boron nitride two-dimensional nano piece is modified mullite antioxidant coating cladding are obtained after being sintered 4.5h at 1500 DEG C
Porcelain composite sample.
The above described is only a preferred embodiment of the present invention, limitation in any form not is done to the present invention, therefore
All contents without departing from technical solution of the present invention, it is made to the above embodiment according to the technical essence of the invention any simply to repair
Change, equivalent variations and modification, in the range of still falling within technical solution of the present invention.
Claims (9)
1. a kind of preparation method of nano modification mullite ceramic coating, which is characterized in that include the following steps：
(1) modifying agent is prepared：
1. dispensing：Lithium tetraborate, Sodium azide and metal magnesium powder are pressed 1~1.5 successively：3~5：4~7 molar ratio ingredient mixing
It is placed in reaction kettle；
2. reacting：It is put into Muffle furnace after the reaction kettle is sealed, the Muffle furnace is set by 5~10 DEG C/min of rate liters
Temperature is to after 500~600 DEG C, and heat preservation 16~for 24 hours obtains the first product；
3. pickling：First reactant is put into hydrochloric acid solution after impregnating and stirring 4~6h and is separated by solid-liquid separation, obtains solid-state
The second product；
4. drying：Second product is dried in vacuo 8~10h at 80~100 DEG C, obtains the hexagonal phase nitrogen of white powder
Change boron two-dimensional nano piece；
(2) precalcining porzite powder is prepared：
1. preparing the first gel：Using aluminum soluble salt, esters of silicon acis as raw material, by Al：Si：H2O：Organic solvent：Catalyst=(2
~3)：(1~1.5)：(5~8)：(20~30)：The molar ratio of (0.3~0.5) is with after taking raw material, organic solvent and catalyst
Back flow reaction is carried out, the first gel is obtained；
2. preparing precalcining porzite powder：By first gel after drying with 1200~1350 DEG C of temperature in air
Calcining, obtains precalcining porzite powder；
(3) mullite precursor is prepared：
1. preparing the second gel：Using aluminum acetate, esters of silicon acis as raw material, by Al：Si：Organic solvent：Catalyst=(2~3)：(1~
1.5)：(5~8)：(20~30)：The molar ratio of (0.3~0.5), which is matched, takes raw material, organic solvent and catalyst later at 60-85 DEG C
At a temperature of 2~4h of back flow reaction, obtain the second gel；
2. gel water reacts：Al is pressed into second gel：H2O=1：1~2 molar ratio is slowly dropped into deionized water, then rises
Temperature to 80~85 DEG C react 4~6 hours, obtain intermediate；
3. slurrying defibrination：According to intermediate：Precalcining mullite powder=(4~6)：Institute is added into the intermediate for 1 mass ratio
Precalcining porzite powder is stated, while 5~8wt% of coalescents and slurry gross mass of 0.3~1wt% of slurry gross mass is added
Drying retarder, 4~6h of ball milling obtains mullite precursor；
(4) dispersion and nano modification：
1. disperseing：The hexagonal phase boron nitride two-dimensional nano piece of 0.2~1wt% of the mullite precursor gross mass is mixed into
In the dispersant of a concentration of 0.01~0.05mol/L, 30~60min of ultrasonic disperse obtains suspension；
2. being modified：By the suspension be added the rotating speed ball milling 20 in the mullite precursor with 120~160rpm~
30min obtains the nano modification mullite ceramic coating.
2. the preparation method of nano modification mullite ceramic coating according to claim 1, it is characterised in that：
In the pickling the step of, the volume ratio 1 of the hydrochloric acid solution：1；
In the pickling the step of, monitors the concentration of the hydrochloric acid solution in real time and the hydrochloric acid solution is replenished in time.
3. the preparation method of nano modification mullite ceramic coating according to claim 1, it is characterised in that：
It is described to be separated by solid-liquid separation using by the way of suction filtration in the pickling the step of.
4. the preparation method of nano modification mullite ceramic coating according to claim 1, it is characterised in that：
Between the reaction the step of and the step of the pickling, by after the first product natural cooling again with anhydrous second
Alcohol and deionized water are alternately cleaned.
5. the preparation method of nano modification mullite ceramic coating according to claim 1, it is characterised in that：
The pickling the step of and between the step of the drying, by the second product washes of absolute alcohol.
6. the preparation method of nano modification mullite ceramic coating according to claim 1, it is characterised in that：
The aluminum soluble salt is one or more of aluminum nitrate, anhydrous Aluminum chloride and aluminium isopropoxide；
The esters of silicon acis is selected from least one of ethyl orthosilicate, methyl orthosilicate and positive silicic acid propyl ester；
The organic solvent is at least one of absolute ethyl alcohol and absolute methanol；
The catalyst is at least one of glacial acetic acid and hydrofluoric acid；
The drying retarder is at least one of oxalic acid and glycerine；
The coalescents are at least one of polyvinylpyrrolidone and polyvinyl butyral；
The dispersant is at least one of carboxymethyl cellulose and poly amic acid.
7. the application method of the nano modification mullite ceramic coating described in a kind of any one of claim 1-6, feature
It is, includes the following steps：
(1) it coats：Ceramic matrix is immersed in the nano modification mullite ceramic coating, is applied using Best-Effort request device
It covers, obtains coating matrix；
(2) it is sintered：The coating matrix is sintered.
8. the application method of nano modification mullite ceramic coating according to claim 7, it is characterised in that：
In the coating step, lifting parameter is：The rate of pulling is no more than 1mm/min, lifts 40~60 DEG C of temperature, relatively wet
Degree is less than 30%RH, and it is 0.8~1.5L/min to lift the nitrogen flow rate in kettle.
9. the application method of nano modification mullite ceramic coating according to claim 7, it is characterised in that：
In the sintering step, by the coating matrix with 1500 DEG C of temperature, it is sintered 3~4 hours under air environment.
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| CN112048203A (en) * | 2020-09-16 | 2020-12-08 | 天津达盈材料科技有限公司 | Water-based high-temperature-resistant flexible ceramic coating material and preparation and use methods thereof |
| CN115124976A (en) * | 2022-07-19 | 2022-09-30 | 淄博众晓新材料科技有限公司 | Composite phase-change gel heat-preservation energy-storage material and preparation method thereof |
| EP4173820A1 (en) * | 2021-10-26 | 2023-05-03 | The Boeing Company | Method for producing high-temperature-resistant coatings and structures |
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