CN107399969A - A kind of method that curtain coating in situ prepares zirconia ceramics piece - Google Patents
A kind of method that curtain coating in situ prepares zirconia ceramics piece Download PDFInfo
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- CN107399969A CN107399969A CN201610332306.6A CN201610332306A CN107399969A CN 107399969 A CN107399969 A CN 107399969A CN 201610332306 A CN201610332306 A CN 201610332306A CN 107399969 A CN107399969 A CN 107399969A
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Abstract
The invention discloses a kind of method that method of curtain coating in situ prepares zirconia ceramics body, its process includes mixing Zirconium powder and doping phase oxide using high-energy ball milling, it is dispersion liquid that well mixed powder is added into solvent, dispersant and levelling agent ball milling mixing again, and it is casting slurry that binding agent and plasticizer ball milling mixing are then added in dispersion liquid.Casting slurry is left a message on casting machine after drying, then cut and be sintered to doped zirconia ceramics lamellar body.Zirconia ceramics preparation of the present invention, the cost of raw material is relatively low, and sintering character is good, easily realizes extensive prepare.
Description
Technical field
This technology is related to a kind of preparation method of zirconia ceramics, especially relates to the tape casting in situ and prepares zirconium oxide
The preparation method of potsherd.
Background technology
Zirconia material is because having high rigidity, high intensity, high tenacity, high wearability and higher and pure oxonium ion
The premium properties such as electric conductivity, obtained in each field such as ceramics, refractory material, machinery, electronics, optics, Aero-Space, biology, chemistry
Obtained and be widely applied.Be present three kinds of crystal formations in pure zirconia, and can mutually convert：It is monoclinic system less than 950 DEG C, 1200
It is tetragonal structure to more than 2370 DEG C, in 2370 DEG C of cubics formed above.Due to the zirconia material in high and low temperature shift
Phase transformation larger Volume Changes be present, cause material to be easy to ftracture during sintering is use, crush and intensity step-down,
So using when be typically necessary and be doped phase with stabilizing zirconia with other elements, it is not produced in temperature change
The destruction of material.By controlling stably-doped dose of content to obtain the different zirconium oxide of phase composition, if making part Tetragonal
It is metastable to arrive room temperature, just obtain PSZ PSZ；If make Tetragonal all it is metastable to room temperature if obtain containing only single-phase polycrystalline
Tetragonal zircite TZP；If making cube is metastable to arrive room temperature, it is fully stabilized zirconia FSZ to obtain single-phase cubic phase material.Stabilizer
A variety of it can also be used in combination with single use, it is also different to zirconia stabilized effect.At present for doped zirconia
Moulding process be essentially all have followed first into phase reshaping technical process, such as CN103951421A, CN100519475C
Etc. the method that patent all discloses preparing zirconium oxide ceramic by curtain coating, i.e., prepare the powder of doped zirconia first, then by powder
Sinter molding is prepared as device.The method is typically all to prepare doped zirconia using wet chemistry method, it is necessary to costly
Zirconates presoma, and substantial amounts of organic solvent and other organic matters are needed in preparation process, seriously polluted and cost is high, mixes
Miscellaneous zirconium oxide preparation process is required for sintering phase into, and high temperature can cause the sintering activity of zirconium oxide to substantially reduce, walked after making into
The increase of type sintering temperature, sintered density reduce.
The content of the invention
In view of problem present in current zirconia ceramics forming process, the invention reside in provide one kind to be cast using in situ
Method prepare doped zirconia ceramics lamella, its raw material is zirconium oxide and doping powder, using the tape casting by material into
Mutually completed with forming process by a step, reduce material preparation process, reduce the cost of product.
For achieving the above object, present invention employs following technical scheme：
（1）Zirconium oxide and doping phase oxide powder are mixed using ball milling in proportion；
（2）The use of ball milling mixing is uniformly dispersion liquid by mixed uniformly powder, solvent, dispersant, levelling agent.Dispersion liquid quality
Than for：Powder 20% ~ 50%, solvent 10% ~ 50%, dispersant 1% ~ 10%, levelling agent 0 ~ 3%.The ball milling mixing time was at 30 minutes to 6
Between individual hour, ball mill tank rotating speed is between 30 revs/min to 100 revs/min, and the mass ratio of ball and powder is 30:1 arrives
2:Between 1；
（3）It is uniformly zirconia slurry that binding agent, plasticizer, defrother are added into dispersion liquid using ball milling mixing.The matter of slurry
Measuring ratio is：Dispersion liquid 70% ~ 95%, binding agent 5% ~ 25%, plasticizer 1% ~ 5%, defrother 0.5% ~ 2%.The ball milling mixing time is 30
Minute, ball mill tank rotating speed was between 10 revs/min ~ 30 revs/min, and the mass ratio of ball and powder is 20 to 4 hours:1
To 2:Between 1；
（4）De-bubble processing is carried out to zirconia slurry using the method for being stirred under vacuum deaeration；
（5）Slurry after de-bubble is cast, dried, is sintered and is obtained zirconia ceramics piece.
Among a typical embodiments, the method that the curtain coating in situ prepares zirconia ceramics piece includes：
（1）Zirconium oxide and doping phase oxide powder are mixed using ball milling in proportion.2 hours of ball milling mixing time,
Ball mill tank rotating speed is 800 revs/min, and the mass ratio of ball and powder is 15:1；
（2）The use of ball milling mixing is uniformly dispersion liquid by mixed uniformly powder, solvent, dispersant, levelling agent.Dispersion liquid quality
Than for：Powder 45%, solvent are ethanol and butanone mixture 50%, dispersant triethanolamine 3%, levelling agent cyclohexanone 2%.Ball milling mixes
Close 4 hours, 80 revs/min of ball mill tank rotating speed, the mass ratio of ball and powder is 20:1；
（3）It is uniformly zirconia slurry that binding agent, plasticizer, defrother are added into dispersion liquid using ball milling mixing.The matter of slurry
Measuring ratio is：Dispersion liquid 80%, binding agent polyvinyl butyral resin 15%, polyethylene glycol 400 account for 4.5%, defrother isooctanol 0.5%.
The ball milling mixing time, ball mill tank rotating speed was at 20 revs/min, and the mass ratio of ball and powder is 20 in 4 hours:1；
5th, froth in vacuum method will be prepared, vacuum 4KPa, mixing speed is 10 revs/min, and inclined heated plate was at 30 minutes.It is de-
Slurry viscosity after bubble is 20000mPa.s；
6th, it is stirred under vacuum the slurry after deaeration and drying is cast on casting machine, drying temperature is 25 DEG C；Drying time is 12 hours；
Thickness is 5 millimeters；The green compact that curtain coating obtains after drying heat up for -500 DEG C in room temperature by 1 DEG C/min of speed, and in 500 degree of guarantors
Temperature dumping processing in 4 hours, then heats up, between maximum temperature is 1450 DEG C, insulation is mixed after 3 hours by 3 DEG C/min of speed
Miscellaneous zirconia ceramics piece.
Compared with the prior art, the positive effect of the present invention includes：
1st, compared with the prior art, present invention omits doped zirconia ceramic powder into phase process, using into phase-shaping one
Step process is completed, and is saved the process time, is reduced process costs；
2nd, the present invention will complete into phase-a be molded over step so that material sintering activity strengthens, and can partly reduce the sintering of material
Temperature, the sintered density of material is improved, be readily available high-performance, highdensity doped zirconia ceramic material；
3rd, the present invention using the tape casting in situ prepare doped zirconia ceramics, technique is flexible, can prepare various complicated shapes or
The ceramic material of person's sandwich construction, it can very easily realize that different elements, various concentrations are mixed using the method for reaction in-situ
It is miscellaneous, avoid ceramic powder into phase preparation process.
Brief description of the drawings：
Fig. 1 is the process chart of the present invention.
Embodiment
As it was previously stated, in view of many defects of prior art, inventor is through studying for a long period of time and putting into practice, it is proposed that a kind of 0
Curtain coating in situ prepares the preparation method of doped zirconia potsherd, and nationality is to realize inexpensive, the big rule of doped zirconia potsherd
Mould and high performance production.Illustrate as follows.
The invention provides a kind of method that method using curtain coating in situ prepares doped zirconia potsherd, it is utilized just
Beginning material be Zirconium powder and doping phase oxide powder, using flow casting molding method by doped zirconia ceramics shaping
Completed with into phase process in a step.
The preparation method can include：
（1）Zirconium oxide and doping phase oxide powder are mixed using ball milling in proportion.
（2）The use of ball milling mixing is uniformly dispersion liquid by mixed uniformly powder, solvent, dispersant, levelling agent.
（3）It is uniformly zirconia slurry that binding agent, plasticizer, defrother are added into dispersion liquid using ball milling mixing.
（4）De-bubble processing is carried out to zirconia slurry using the method for being stirred under vacuum deaeration.
（5）Slurry after de-bubble is cast, dried, is sintered and is obtained zirconia ceramics piece
Further, the Zirconium powder used in the present invention is monoclinic phase Zirconium powder, and diameter of particle D50 arrives at 100 nanometers
Between 500 microns, purity is more than 99.9%, the monoclinic phase zirconia powder that more preferably particle diameter is 5 microns, purity is 99.9%
Body.Doping is mutually aluminum oxide, yittrium oxide, cerium oxide, scandium oxide, erbium oxide, niobium oxide, ytterbium oxide, gadolinium oxide, molybdenum oxide, oxygen
Change one or more kinds of mixing and dopings in lanthanum, praseodymium oxide, samarium oxide, magnesia, calcium oxide, barium monoxide, preferred doping
Thing is yittrium oxide, aluminum oxide, calcium oxide, scandium oxide.The particle diameter D50 of above oxide powder 100 nanometers to 500 microns it
Between, purity is more than 99.9%, and more preferably particle diameter is 5 microns, and purity is 99.95% oxide powder.
Further, the ball milling mixing time of zirconium oxide and doping oxide of the present invention is small at 30 minutes to 3
When between, more preferably 1 ~ 2 hour；Ball mill tank rotating speed is between 100 revs/min to 1000 revs/min, more preferably
400 revs/min to 800 revs/min；The mass ratio of ball and powder is 20:1 to 10:Between 5, more preferably 15:1 to 3:1 it
Between.
Further, solvent of the present invention is that described solvent is water, ethanol, propyl alcohol, isopropanol, butanol, isobutyl
Alcohol, the tert-butyl alcohol, acetone, butanone, toluene, n-hexane, isohexane, neohexane, pentane, isopentane, neopentane, N- methylpyrroles
One or several kinds of mixtures in alkanone, tetrahydrofuran, more preferably water, ethanol/acetone mixture, N- crassitudes
Ketone；The mass fraction that solvent accounts for dispersion liquid is 10% ~ 50%, more preferably 20% ~ 45%；Described dispersant can be fat
The more second polyamines of amine, diethanol amine, triethanolamine, N-alkyl Diethylenetriamine, N-alkyl, 2-alkyl imidazoline, 2-alkyl ammonia
Base ethyl imidazol(e) quinoline, OTAC, hexadecyltrimethylammonium chloride, distearyl hydroxyethyl methyl sulfuric acid
Formicester ammonium, distearyl hydroxyethyl methyl sulfuric acid formicester ammonium, cetearyl alcohol alcohol ether -2, cetearyl alcohol alcohol ether -21, cetearyl alcohol
Base ether -20, lauryl glucoside polyglycereol, rilanit special, APEO phosphotriester, polyoxyethylene sorbitan
Monolaurate, sodium alkyl benzene sulfonate, sodium alkyl sulfate, pareth sulfate, sodium soap, alkyl polyoxyethylene
Ether carboxylic acid sodium, sodium alkyl sulfonate, sodium methylene bis-naphthalene sulfonate, glycerin monostearate, polyalcohol sucrose ester, aliphatic acid sorb
It is smooth, one or more kinds of mixtures in polysorbate, more preferably diethanol amine, triethanolamine, octadecyl trimethyl
Ammonium chloride, hexadecyltrimethylammonium chloride, the mass fraction that described dispersant accounts for dispersion liquid are 1% ~ 10%, more preferably
2%~6%。
Further, the dispersion liquid ball milling mixing time of the present invention between 30 minutes to 6 hours, more preferably
Time is between 2 hours to 5 hours；Ball mill tank rotating speed is between 30 revs/min to 100 revs/min, more preferably 40
Rev/min between 90 revs/min；The mass ratio of ball and powder is 30:1 to 10:Between 5, more preferably 20:1 to 3:1 it
Between.
Further binding agent of the present invention be polyvinyl alcohol, polyvinyl butyral resin, polyacrylic acid, polyurethane,
One in epoxy resin, methylcellulose, ethyl cellulose, carboxymethyl cellulose, carboxyethyl cellulose, polyvinylpyrrolidone
Kind or a variety of mixing, more preferably polyvinyl alcohol, polyvinyl butyral resin, polyvinylpyrrolidone, described binding agent
The mass ratio for accounting for slurry is 5% ~ 25%, with being preferably 10% ~ 20%；Plasticizer of the present invention is to face the fourth of phthalic acid two
Ester, diisooctyl phthalate, diisooctyl phthalate, diisooctyl phthalate, two different nonyl of phthalic acid
Ester, dibutyl phthalate, diisobutyl phthalate, BBP(Butyl Benzyl Phthalate, repefral, adjacent benzene
Dicarboxylate, dicyclohexyl phthalate, DOTP, dioctyl adipate, diisodecyl adipate,
One or more in dioctyl azelate, the butyric acid of decanedioic acid two, polyethylene glycol 400, Macrogol 600, polyethylene glycol-800
Mixing, more preferably repefral, diethyl phthalate, dicyclohexyl phthalate, polyethylene glycol
400th, Macrogol 600, polyethylene glycol-800, described plasticizer account for slurry mass ratio be 1% ~ 5%, more preferably 2% ~
4%;Defrother of the present invention is octanol, 2-Ethylhexyl Alcohol, propane diols, stearic acid, palmitic acid, fatty acid ester, tricresyl phosphate fourth
One or more kinds of mixtures in ester, sorbitan fatty acid ester, more preferably octanol, fatty acid ester, propane diols, it is described
De-bubble dosage account for slurry mass ratio be 0.5% ~ 2%, more preferably 0.5% ~ 1%.
Further froth in vacuum method of the present invention, vacuum more preferably exist between 6KPa to 2KPa
Between 5KPa to 3KPa；Mixing speed is between 5rpm to 15rpm, more preferably between 7rpm to 10rpm；Inclined heated plate exists
Between 15 minutes to 1 hour more preferably between 30 minutes to 1 hour.
It is stirred under vacuum the slurry after deaeration and drying is cast on casting machine, drying temperature is 20 DEG C -60 DEG C；Drying time is
- 24 hours 0.5 hour；Thickness is 0.1 millimeter -10 millimeters；After curtain coating is dried obtained green compact in -500 DEG C of room temperature by 1 DEG C/min
Speed is heated up, and the processing of 1-6 hours dumping is incubated at 500 degree, is then heated up by 3 DEG C/min speed, maximum temperature 1200
Between DEG C -1500 DEG C, 1-4 hours are incubated.Its optimize parameter can with environment, application scenario, dopant difference and
It is fixed.
Below in conjunction with some preferred embodiments the technical solution of the present invention is further explained explanation.
Embodiment 1,
100 grams of Zirconium powder and 15 grams of yttrium oxide powder are mixed using ball milling.2 hours of ball milling, ball mill
Tank body rotating speed is at 800 revs/min, and the mass ratio of ball and powder is 10:1；Then 45 grams of ethanol, 55 grams of acetone, 4 gram of three second are added
Between hydramine, 4 hours of 2 grams of cyclohexanone ball milling mixings, ball mill tank rotating speed is 80rpm, and the mass ratio of ball and powder is 20:
1；By the ball milling mixing time in 40 grams of polyvinyl butyral resins, 8.8 grams of polyethylene glycol 400s, 2 grams of octanols addition dispersion liquids at 4
Hour, ball mill tank rotating speed is 20 revs/min, and the mass ratio of ball and powder is 20:1；The slurry viscosity of preparation is at 25 DEG C
For 10000mPa.s.The slurry of preparation is poured into deaeration in vacuum degasing machine, deaeration vacuum is 4KPa, mixing speed 10
Rev/min, inclined heated plate is 15 minutes.Slurry after de-bubble is cast, dried, and curtain coating is that edge height is adjusted to 5 millimeters, stream
After prolonging end, green compact are dried 12 hours at 25 DEG C.Curtain coating green compact are placed on load bearing board of zirconia and are put into Muffle furnace, 1 DEG C/min
Speed is warming up to 500 DEG C, is incubated 4 hour dumping processing, and then 3 DEG C/min speed is warming up to 1450 DEG C, is incubated 3 small doping
Zirconia ceramics piece.Zirconia ceramics piece density prepared by the method is 6.2g/cc, bending strength 780MPa, 800 DEG C of conductances
Rate is 0.02S/cm, and thermal conductivity is 2.0W/mk at 20 DEG C.
Embodiment 2,
100 grams of Zirconium powder, 15 grams of yittrium oxide, 2 grams of alumina powders are mixed using ball milling.Ball milling is 2 small
When, ball mill tank rotating speed is at 800 revs/min, and the mass ratio of ball and powder is 10:1；Then add 45 grams of ethanol, 55 gram third
Ketone, 3.5 grams of triethanolamines, between 4 hours of 1.6 grams of cyclohexanone ball milling mixings, ball mill tank rotating speed be 80 revs/min, ball
Mass ratio with powder is 20:1；40 grams of polyvinyl butyral resins, 8.8 grams of polyethylene glycol 400s, 2 grams of octanols are added into dispersion liquid
The middle ball milling mixing time, ball mill tank rotating speed was 20 revs/min in 4 hours, and the mass ratio of ball and powder is 20:1；Prepare
Slurry viscosity be 15000mPa.s at 25 DEG C.The slurry of preparation is poured into deaeration in vacuum degasing machine, deaeration vacuum is
4KPa, mixing speed 10rpm, inclined heated plate are 15 minutes.Slurry after de-bubble is cast, dried, and curtain coating is edge of a knife height
Degree is adjusted to 5 millimeters, after curtain coating terminates, and green compact are dried 12 hours at 25 DEG C.Curtain coating green compact are placed on load bearing board of zirconia and are put into
Muffle furnace, 1 DEG C/min speed are warming up to 500 DEG C, are incubated 4 hour dumping processing, then 3 DEG C/min speed is warming up to 1450
DEG C, it is incubated 3 small doped zirconia potsherd.Zirconia ceramics piece density prepared by the method is 6.3g/cc, and bending strength is
900MPa, 800 DEG C of electrical conductivity are 0.002S/cm, and thermal conductivity is 2.5W/mk at 20 DEG C.
Claims (9)
1. a kind of method that curtain coating in situ prepares zirconia ceramics piece, its process include：
（1）Zirconium oxide and doping phase oxide powder are mixed using high-energy ball milling in proportion；
The ball milling mixing time, ball mill tank rotating speed was at 300 revs/min to 3000 revs/min between 30 minutes to 3 hours
Between, the mass ratio of ball and powder is 20:1 to 2:Between 1；
（2）Will（1）Powder that step obtains, solvent, dispersant, levelling agent are uniformly dispersion liquid using ball milling mixing；
Dispersion liquid composition is：Powder 20% ~ 50%, solvent 10% ~ 50%, dispersant 1% ~ 10%, levelling agent 0 ~ 3%；
The ball milling mixing time between 30 minutes to 6 hours, ball mill tank rotating speed 30 revs/min to 100 revs/min it
Between, the mass ratio of ball and powder is 30:1 to 2:Between 1；
（3）It using ball milling mixing is uniformly zirconia slurry that binding agent, plasticizer, defrother, which are added in dispersion liquid,；
The composition of slurry is：Dispersion liquid 70% ~ 95%, binding agent 5% ~ 25%, plasticizer 1% ~ 5%, defrother 0.5% ~ 2%；
The ball milling mixing time between 30 minutes to 6 hours, ball mill tank rotating speed 10 revs/min to 30 revs/min it
Between, the mass ratio of ball and powder is 30:1 to 2:Between 1；
（4）De-bubble processing is carried out to zirconia slurry using the method for being stirred under vacuum deaeration；
（5）Slurry after de-bubble is cast, dried, is sintered and is obtained zirconia ceramics piece.
2. Zirconium powder as claimed in claim 1 is monocline phase zircite, diameter of particle D50 is at 100 nanometers to 500 microns
Between, between zirconia content is 99% to 99.99%；Doping mutually for aluminum oxide, yittrium oxide, cerium oxide, scandium oxide, erbium oxide,
One kind in niobium oxide, ytterbium oxide, gadolinium oxide, molybdenum oxide, lanthana, praseodymium oxide, samarium oxide, magnesia, calcium oxide, barium monoxide
Or a variety of mixing and dopings, between 100 nanometers to 500 microns, purity arrives the particle diameter D50 of above oxide powder for 99%
Between 99.99%.
3. powder as claimed in claim 1 is zirconium oxide and doping oxide through the uniform powder of ball milling mixing；Described
Solvent is water, ethanol, propyl alcohol, isopropanol, butanol, isobutanol, the tert-butyl alcohol, acetone, butanone, toluene, n-hexane, isohexane, new
One or several kinds of mixtures in hexane, pentane, isopentane, neopentane, 1-METHYLPYRROLIDONE, tetrahydrofuran.
4. dispersant as claimed in claim 1 is fatty amine, diethanol amine, triethanolamine, N-alkyl diethyl triamine,
2-alkyl imidazoline, 2-alkylaminoethyl imidazoline, OTAC, cetyl trimethyl chlorination
Ammonium, distearyl hydroxyethyl methyl sulfuric acid formicester ammonium, distearyl hydroxyethyl methyl sulfuric acid formicester ammonium, cetearyl alcohol alcohol ether -2,
Cetearyl alcohol alcohol ether -21, cetearyl ether -20, lauryl glucoside polyglycereol, rilanit special, APEO phosphorus
Sour three esters, polyoxyethylene 20 sorbitan monolaurate, sodium alkyl benzene sulfonate, sodium alkyl sulfate, alkyl polyoxyethylene ether sulphur
Sour sodium, sodium soap, Alkyl ethoxy carboxylate acid sodium, sodium alkyl sulfonate, sodium methylene bis-naphthalene sulfonate, glycerol monostearate
One or more kinds of mixtures in ester, fatty acid sorbitan, polysorbate；
Levelling agent is cyclohexanone.
5. binding agent as claimed in claim 1 is polyvinyl alcohol, polyvinyl butyral resin, polyacrylic acid, polyurethane, asphalt mixtures modified by epoxy resin
One kind in fat, methylcellulose, ethyl cellulose, carboxymethyl cellulose, carboxyethyl cellulose, polyvinylpyrrolidone or
A variety of mixing.
6. plasticizer as claimed in claim 1 is to face dibatyl phithalate, dioctyl phthalate, phthalic acid
Di-isooctyl, diisooctyl phthalate, diisononyl phthalate, dibutyl phthalate, phthalic acid two
Isobutyl ester, BBP(Butyl Benzyl Phthalate, repefral, diethyl phthalate, dicyclohexyl phthalate,
DOTP, dioctyl adipate, diisodecyl adipate, dioctyl azelate, the butyric acid of decanedioic acid two, poly- second two
One or more kinds of mixing in alcohol 400, Macrogol 600, polyethylene glycol-800；
Defrother is octanol, 2-Ethylhexyl Alcohol, propane diols, stearic acid, palmitic acid, fatty acid ester, tributyl phosphate, Sorbitan
One or more kinds of mixtures in alcohol fatty acid ester.
7. froth in vacuum method as claimed in claim 1, vacuum is between 6KPa to 2KPa, and mixing speed is at 5 revs/min
To between 15 revs/min, inclined heated plate is between 15 minutes to 1 hour；
Slurry viscosity after deaeration is 8000mPa.s ~ 40000mPa.s.
8. the slurry as claimed in claim 1, being stirred under vacuum after deaeration is cast drying on casting machine；
Drying temperature is 20 DEG C ~ 60 DEG C；Drying time is 0.5 hour ~ 24 hours；Thickness is 0.1 millimeter ~ 10 millimeters；Curtain coating is dry
The green compact obtained after dry heat up in room temperature ~ 500 DEG C by 1 DEG C/min speed, and are handled in 500 degree of insulations, 1 ~ 6 hour dumping, so
Heated up afterwards by 3 DEG C/min speed, between maximum temperature is 1200 DEG C ~ 1500 DEG C, be incubated 1 ~ 4 hour.
9. the method that curtain coating in situ as claimed in claim 1 prepares zirconia ceramics piece, its process include：Starting powder processing
Process, dispersion liquid preparation process, slurry preparation process, it is cast drying process, sinters porcelain process into.
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| CN112876245A (en) * | 2021-01-28 | 2021-06-01 | 深圳陶陶科技有限公司 | Preparation method of zirconia ceramic |
| CN113087523A (en) * | 2021-04-07 | 2021-07-09 | 盐城工学院 | Zirconia ceramic doped with rare earth/transition metal oxide and preparation method thereof |
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| CN116283244B (en) * | 2023-05-17 | 2023-07-21 | 湖南大学 | Method for preparing alumina ceramic flake by casting |
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