CN112456979A - Preparation method of zirconia toughened alumina powder and ceramic - Google Patents
Preparation method of zirconia toughened alumina powder and ceramic Download PDFInfo
- Publication number
- CN112456979A CN112456979A CN202011437485.2A CN202011437485A CN112456979A CN 112456979 A CN112456979 A CN 112456979A CN 202011437485 A CN202011437485 A CN 202011437485A CN 112456979 A CN112456979 A CN 112456979A
- Authority
- CN
- China
- Prior art keywords
- toughened alumina
- alumina powder
- zirconia
- zirconia toughened
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 196
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000000843 powder Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 title abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 62
- 238000001556 precipitation Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 25
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 230000032683 aging Effects 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 24
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000007921 spray Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 30
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 22
- 238000003760 magnetic stirring Methods 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002131 composite material Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 235000015895 biscuits Nutrition 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000009694 cold isostatic pressing Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of zirconia toughened alumina powder, which comprises the following steps: and S1, mixing the aluminum nitrate solution and the zirconium nitrate solution, adding a surfactant, and stirring to obtain a first solution. And S2, adding an alkaline aqueous solution into the first solution, carrying out precipitation aging treatment, and carrying out suction filtration on the reacted first solution to collect the lower-layer precipitate to obtain a precipitate mixture. And S3, calcining the precipitation mixture, and then performing spray granulation on the calcined precipitation mixture to obtain the zirconia toughened alumina powder. Also provides a preparation method of the zirconia toughened alumina ceramic, which comprises the preparation method of the zirconia toughened alumina powder, a step of preparing a forming body and a sintering step. The zirconia toughened alumina powder and the ceramics prepared by the method have uniform grain size, good sintering performance, uniform components and excellent mechanical properties.
Description
Technical Field
The invention relates to the technical field of ceramic preparation, in particular to zirconia toughened alumina powder and a preparation method of ceramic.
Background
The alumina ceramic has the advantages of corrosion resistance, high temperature resistance, wear resistance, light weight, low cost and the like, and is an industrial ceramic material with the largest production and the widest application range in the world at present. The material has wide application prospect in the technical field of defense and protection such as aerospace and the like and the general industrial fields such as machinery, metallurgy, chemical industry and the like, but the most fatal mechanical weakness is the brittleness of the material, which is determined by the structural characteristics of the material. Chemical bonds in the ceramic material are mainly covalent bonds and ionic bonds, and both the chemical bonds have strong directionality and high bonding strength, so that remarkable dislocation movement in the structure is difficult to occur. Thus limiting the further spread of its practical application range. Therefore, toughening of ceramics, particularly alumina ceramics, has become a central issue in the recent research of structural ceramic materials.
In the prior art, zirconia powder and alumina powder are often prepared respectively and then compounded to prepare zirconia toughened alumina powder. The method is difficult to realize the consistency and stability of the composite condition, so that the particle size or components are deviated and uneven phenomena occur, the sintering performance of the powder is poor, and the prepared ceramic has uneven components and poor mechanical properties.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the zirconia toughened alumina powder and the preparation method of the ceramic.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of zirconia toughened alumina powder comprises the following steps:
s1, mixing the aluminum nitrate solution and the zirconium nitrate solution, stirring for the first time, adding the surfactant, and stirring for the second time at the temperature of 70-90 ℃ to obtain a first solution;
s2, adding an alkaline aqueous solution into the first solution prepared in the step S1, carrying out precipitation aging treatment, and carrying out suction filtration on the reacted first solution to collect lower-layer precipitates to obtain a precipitate mixture;
and S3, calcining the precipitation mixture to obtain zirconia-toughened alumina composite powder, and performing spray granulation on the composite powder to obtain the zirconia-toughened alumina powder.
The further improvement of the technical scheme is as follows:
in the step S1, the first stirring and the second stirring are both magnetic stirring, and the time is 20-30 min.
The alkaline aqueous solution in the step S2 is an ammonia aqueous solution with the concentration of 20-30 wt%.
And in the step S2, repeatedly washing the lower-layer precipitate with deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, and stopping washing.
The method also comprises the following steps after the step S2: and repeatedly washing the precipitate mixture by using absolute ethyl alcohol, and drying.
The calcination temperature in the step S3 is 900-1100 ℃, and the calcination time is 3-5 h.
The zirconia toughening alumina powder contains 15-25 parts by mass of zirconia and 85-92 parts by mass of alumina.
The invention also provides a preparation method of the zirconia toughened alumina ceramic, which comprises the preparation method of the zirconia toughened alumina powder and also comprises the following steps:
and S4, carrying out dry pressing molding on the zirconia toughened alumina powder to obtain a molded body.
Or further comprising:
s5, mixing the zirconia toughened alumina powder with a dispersant and a binder to prepare slurry, preparing the slurry into a green body, and heating and discharging the green body to obtain a formed body.
The further improvement of the technical proposal of the preparation method of the zirconia toughened alumina ceramic also comprises the following steps:
and S6, sintering the formed body in an air atmosphere to obtain the zirconia toughened alumina ceramic.
According to the technical scheme, the aluminum nitrate solution and the zirconium nitrate solution are used as the sources of the alumina and the zirconia, and after precipitation and aging treatment, the crystal form is more complete and the grain size is more uniform. After being washed by absolute ethyl alcohol, the zirconium oxide can be effectively prevented from agglomerating, the zirconium oxide is uniformly dispersed in aluminum oxide, and the obtained composite powder has round surface, high sphericity, strong fluidity and good sintering performance through spray granulation. The zirconia toughened alumina ceramic prepared by the zirconia toughened alumina powder prepared by the method has uniform components, uniform crystal grain size and good mechanical property.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing zirconia toughened alumina powder according to an embodiment of the present invention.
FIG. 2 is a schematic flow chart of a preparation method of zirconia toughened alumina ceramic according to an embodiment of the present invention.
FIG. 3 is a D50 particle size distribution chart for example 4 of the present invention.
FIG. 4 is a graph of the D50 particle size distribution for a comparative example of example 4 of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
As shown in FIG. 1 and FIG. 2, the flow chart of the preparation method of the zirconia toughened alumina powder and the ceramics of the invention is shown.
Example 1, as shown in fig. 1, the method for preparing a zirconia toughened alumina powder of this example comprises the steps of:
s1, respectively adding an aluminum nitrate solution and a zirconium nitrate solution into the reaction kettle, performing first magnetic stirring for 20min, adding a citric acid surfactant into the reaction kettle, heating to 70-80 ℃, performing second magnetic stirring for 20min, and uniformly mixing the solutions to obtain a first solution.
S2, adding an alkaline aqueous solution into the first solution prepared in the step S1, wherein the alkaline aqueous solution is an ammonia water solution with the concentration of 20 wt%, the dropping speed of the ammonia water solution is 10ml/min, carrying out precipitation aging treatment at the temperature of 60-70 ℃, the time of deep precipitation aging is 8h, the pH value of the solution during precipitation is 7-10, after the upper layer liquid is clarified, carrying out suction filtration on the upper layer liquid to collect the lower layer precipitate, repeatedly washing the lower layer precipitate with deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, and stopping washing to obtain a precipitation mixture.
S2.1, repeatedly washing the precipitation mixture prepared in the step S2 with absolute ethyl alcohol for at least two times, and then placing the mixture in an oven for drying, wherein the drying temperature is 90-100 ℃, and the drying time is 6 h.
And S3, calcining the precipitation mixture treated in the step S2.1 to obtain the zirconia toughened alumina composite powder. The calcination temperature is 900-950 ℃, the calcination time is 5h, and the temperature rise speed is 5 ℃/min. The temperature of the drying air is 200 ℃, the rotating speed of the spray head is 4000rpm, the air pressure difference is 150Pa, and the air outlet temperature is 100 ℃. And then sending the composite powder into a spray drying tower for spray drying granulation to obtain the zirconia toughened alumina powder. The zirconia toughened alumina powder prepared by the method comprises 15 parts by mass of zirconia and 92 parts by mass of alumina.
Example 2 as shown in fig. 1, the method for preparing the zirconia toughened alumina powder of this example substantially corresponds to the steps of example 1, except that:
and S1, performing magnetic stirring for the first time for 30min, and performing magnetic stirring for the second time for 30min at the temperature of 80-90 ℃.
S2, the concentration of the ammonia water solution is 30 wt%, the dropping speed of the ammonia water solution is 15ml/min, and the precipitation aging treatment is carried out at the temperature of 80-90 ℃, and the time of deep precipitation aging is 10 h.
S2.1, drying for 8 h.
S3, the calcining temperature is 1050-. The temperature of the drying air is 300 ℃, the rotating speed of the spray head is 6000rpm, the air pressure difference is 200Pa, and the air outlet temperature is 150 ℃. The zirconia toughened alumina powder prepared by the method comprises 25 parts by mass of zirconia and 85 parts by mass of alumina.
Example 3, as shown in fig. 1, the method for preparing the zirconia toughened alumina powder of this example is substantially the same as the steps of example 1 except that:
and S1, performing the first magnetic stirring for 25min, and performing the second magnetic stirring at the temperature of 75-85 ℃ for 25 min.
S2, the concentration of the ammonia water solution is 25 wt%, the dropping speed of the ammonia water solution is 20ml/min, and the precipitation aging treatment is carried out at the temperature of 70-80 ℃, and the time of deep precipitation aging is 9 h.
S2.1, drying for 7 h.
S3, the calcining temperature is 980-. The temperature of the drying air is 250 ℃, the rotating speed of the spray head is 5000rpm, the air pressure difference is 180Pa, and the air outlet temperature is 120 ℃. The zirconia toughened alumina powder prepared by the method comprises 20 parts by mass of zirconia and 88 parts by mass of alumina.
The zirconia toughened alumina powder prepared by the invention has the advantages that zirconia and alumina are generated simultaneously, so that the phenomenon that the prepared particle size and components are uneven due to difficulty in realizing the consistency and stability of compounding conditions in the process of respectively preparing the zirconia and the alumina and then compounding in the prior art is avoided, the particle size of the zirconia toughened alumina powder is ensured to be uniform, and the sintering performance of the zirconia toughened alumina powder is better. Experiments prove that the grain size of the zirconia toughened alumina powder prepared by the invention is not more than 4D 90/D50, the components are uniform after sintering, the crystal grain size is uniform, and the mechanical property is excellent.
Example 4, as shown in fig. 2, the method for preparing zirconia toughened alumina ceramic of this example includes the following steps:
s1, respectively adding an aluminum nitrate solution and a zirconium nitrate solution into the reaction kettle, stirring for 20min after the first magnetic stirring, adding a citric acid surfactant into the reaction kettle, heating to 70-80 ℃, and performing the second magnetic stirring for 20min to uniformly mix the solutions to obtain a first solution.
S2, adding an alkaline aqueous solution into the first solution prepared in the step S1, wherein the alkaline aqueous solution is an ammonia water solution with the concentration of 20 wt%, the dropping speed of the ammonia water solution is 10ml/min, carrying out precipitation aging treatment at the temperature of 60-70 ℃, the time of deep precipitation aging is 8h, the pH value of the solution during precipitation is 7-10, after the upper layer liquid is clarified, carrying out suction filtration on the upper layer liquid to collect the lower layer precipitate, repeatedly washing the lower layer precipitate with deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, and stopping washing to obtain a precipitation mixture.
S2.1, repeatedly washing the precipitation mixture prepared in the step S2 with absolute ethyl alcohol for at least two times, and then placing the mixture in an oven for drying, wherein the drying temperature is 90-100 ℃, and the drying time is 6 h.
And S3, calcining the precipitation mixture treated in the step S2.1 to obtain the zirconia toughened alumina composite powder. The calcination temperature is 900-950 ℃, the calcination time is 5h, and the temperature rise speed is 5 ℃/min. The temperature of the drying air is 200 ℃, the rotating speed of the spray head is 4000rpm, the air pressure difference is 150Pa, and the air outlet temperature is 100 ℃. And then sending the composite powder into a spray drying tower for spray drying granulation to obtain the zirconia toughened alumina powder. The zirconia toughened alumina powder prepared by the method comprises 15 parts by mass of zirconia and 92 parts by mass of alumina.
S4, dry-pressing the zirconia toughened alumina powder prepared in the step S3 to obtain a molded body: firstly, pressurizing the zirconia toughened alumina powder by using a press with the pressure of 20MPa for 5min to obtain a biscuit with the density of 2.8-3.0g/cm3Then the biscuit is subjected to cold isostatic pressing treatment under the pressure of 150MPa for 5min, and the density of the obtained formed body is 3.2-3.5g/cm3。
And S6, sintering the molded body prepared in the step S4 in the air atmosphere, wherein the sintering temperature is 1430-1440 ℃, the sintering time is 8h, the heating rate is 5 ℃/min during heating, and the zirconia toughened alumina ceramic is obtained after sintering.
Example 5, as shown in fig. 2, the preparation method of the zirconia toughened alumina ceramic of this example is substantially the same as the steps of example 4, except that:
and S1, performing magnetic stirring for the first time for 30min, and performing magnetic stirring for the second time for 30min at the temperature of 80-90 ℃.
S2, the concentration of the ammonia water solution is 30 wt%, the dropping speed of the ammonia water solution is 15ml/min, and the precipitation aging treatment is carried out at the temperature of 80-90 ℃, and the time of deep precipitation aging is 10 h.
S2.1, drying for 8 h.
S3, the calcining temperature is 1050-. The temperature of the drying air is 300 ℃, the rotating speed of the spray head is 6000rpm, the air pressure difference is 200Pa, and the air outlet temperature is 150 ℃. The zirconia toughened alumina powder prepared by the method comprises 25 parts by mass of zirconia and 85 parts by mass of alumina.
And S4, firstly, pressurizing the zirconia toughened alumina powder by using a press with the pressure of 30MPa for 2min to obtain a biscuit, and then carrying out cold isostatic pressing on the biscuit with the pressure of 200MPa for 3 min.
S6, the sintering temperature is 1460-1470 ℃, the sintering time is 5h, and the heating speed is 10 ℃/min during heating.
Example 6, as shown in fig. 2, the preparation method of the zirconia toughened alumina ceramic of this example is substantially the same as the steps of example 4, except that:
and S1, performing the first magnetic stirring for 25min, and performing the second magnetic stirring at the temperature of 75-85 ℃ for 25 min.
S2, the concentration of the ammonia water solution is 25 wt%, the dropping speed of the ammonia water solution is 20ml/min, and the precipitation aging treatment is carried out at the temperature of 70-80 ℃, and the time of deep precipitation aging is 9 h.
S2.1, drying for 7 h.
S3, the calcining temperature is 980-. The temperature of the drying air is 250 ℃, the rotating speed of the spray head is 5000rpm, the air pressure difference is 180Pa, and the air outlet temperature is 120 ℃. The zirconia toughened alumina powder prepared by the method comprises 20 parts by mass of zirconia and 88 parts by mass of alumina.
And S4, firstly, pressurizing the zirconia toughened alumina powder by using a press with the pressure of 25MPa for 4min to obtain a biscuit, and then carrying out cold isostatic pressing on the biscuit with the pressure of 180MPa for 4 min.
S6, the sintering temperature is 1450-.
Example 7, as shown in fig. 2, the method for preparing zirconia toughened alumina ceramic of this example includes the following steps:
s1, respectively adding an aluminum nitrate solution and a zirconium nitrate solution into a reaction kettle, stirring for 20min after first magnetic stirring, adding a citric acid surfactant into the reaction kettle, heating to 70-80 ℃, and performing second magnetic stirring for 20min to uniformly mix the solutions to obtain a first solution;
s2, adding an alkaline aqueous solution into the first solution prepared in the step S1, wherein the alkaline aqueous solution is an ammonia water solution with the concentration of 20 wt%, the dropping speed of the ammonia water solution is 10ml/min, carrying out precipitation aging treatment at the temperature of 60-70 ℃, the time of deep precipitation aging is 8h, the pH value of the solution during precipitation is 7-10, after the upper layer liquid is clarified, carrying out suction filtration on the upper layer liquid to collect the lower layer precipitate, repeatedly washing the lower layer precipitate with deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, and stopping washing to obtain a precipitation mixture.
S2.1, repeatedly washing the precipitation mixture prepared in the step S2 with absolute ethyl alcohol for at least two times, and then placing the mixture in an oven for drying, wherein the drying temperature is 90-100 ℃, and the drying time is 6 h.
And S3, calcining the precipitation mixture treated in the step S2.1 to obtain the zirconia toughened alumina composite powder. The calcination temperature is 900-950 ℃, the calcination time is 5h, and the temperature rise speed is 5 ℃/min. And (3) feeding the composite powder into a spray drying tower for spray drying granulation to obtain the zirconia toughened alumina powder, wherein the temperature of the drying air is 200 ℃, the rotating speed of a spray head is 4000rpm, the air pressure difference is 150Pa, and the air outlet temperature is 100 ℃. The zirconia toughened alumina powder prepared by the method comprises 15 parts by mass of zirconia and 92 parts by mass of alumina.
S5, mixing the zirconia toughened alumina powder prepared in the step S3 with a carboxylic acid-based dispersant, a wax-based binder and other solvents to prepare slurry. The prepared slurry contains 55 parts by mass of zirconia toughened alumina powder, 1 part by mass of a dispersant, 10 parts by mass of a binder and the balance of a solvent. The dispersing agent is triethanolamine, phosphate or castor oil, the binder is PVB, and the solvent is water, absolute ethyl alcohol, propanol or isopropanol. And preparing the slurry into a green body, heating the green body to discharge the glue, and removing the auxiliary agent in the green body to obtain a formed body.
And S6, sintering the molded body prepared in the step S4 in the air atmosphere, wherein the sintering temperature is 1430-1440 ℃, the sintering time is 8h, the heating rate is 5 ℃/min during heating, and the zirconia toughened alumina ceramic is obtained after sintering.
Example 8, as shown in fig. 2, the preparation method of the zirconia toughened alumina ceramic of this example is substantially the same as the steps of example 7, except that:
and S1, performing magnetic stirring for the first time for 30min, and performing magnetic stirring for the second time for 30min at the temperature of 80-90 ℃.
S2, the concentration of the ammonia water solution is 30 wt%, the dropping speed of the ammonia water solution is 15ml/min, and the precipitation aging treatment is carried out at the temperature of 80-90 ℃, and the time of deep precipitation aging is 10 h.
S2.1, drying for 8 h.
S3, the calcining temperature is 1050-. The temperature of the drying air is 300 ℃, the rotating speed of the spray head is 6000rpm, the air pressure difference is 200Pa, and the air outlet temperature is 150 ℃. The zirconia toughened alumina powder prepared by the method comprises 25 parts by mass of zirconia and 85 parts by mass of alumina.
S5, in the prepared slurry, 77 parts by mass of zirconia toughened alumina powder, 3 parts by mass of a dispersant, 30 parts by mass of a binder and the balance of a solvent.
S6, the sintering temperature is 1460-1470 ℃, the sintering time is 5h, and the heating speed is 10 ℃/min during heating.
Example 9, as shown in fig. 2, the preparation method of the zirconia toughened alumina ceramic of this example is substantially the same as the steps of example 7, except that:
and S1, performing the first magnetic stirring for 25min, and performing the second magnetic stirring at the temperature of 75-85 ℃ for 25 min.
S2, the concentration of the ammonia water solution is 25 wt%, the dropping speed of the ammonia water solution is 20ml/min, and the precipitation aging treatment is carried out at the temperature of 70-80 ℃, and the time of deep precipitation aging is 9 h.
S2.1, drying for 7 h.
S3, the calcining temperature is 980-. The temperature of the drying air is 250 ℃, the rotating speed of the spray head is 5000rpm, the air pressure difference is 180Pa, and the air outlet temperature is 120 ℃. The zirconia toughened alumina powder prepared by the method comprises 20 parts by mass of zirconia and 88 parts by mass of alumina.
S5, in the prepared slurry, 66 parts by mass of zirconia toughened alumina powder, 2 parts by mass of a dispersant, 20 parts by mass of a binder and the balance of a solvent.
S6, the sintering temperature is 1450-.
In order to prove the component uniformity and excellent mechanical properties of the zirconia toughened alumina ceramic prepared by the method of the invention, the following experiment is specially carried out to compare with the experiment of example 4.
Comparative example to example 4:
respectively adding an aluminum nitrate solution and a zirconium nitrate solution into a reaction kettle A and a reaction kettle B, wherein the reaction kettle A and the reaction kettle B have the same experimental procedure steps and the specific steps are as follows:
and S1, respectively carrying out first magnetic stirring on the solutions in the reaction kettle A and the reaction kettle B for 20min, respectively adding citric acid surfactant into the reaction kettles, and carrying out second magnetic stirring at the temperature of 70-80 ℃ for 20min to uniformly mix the solutions to respectively obtain first solutions.
S2, respectively adding an alkaline aqueous solution into the first solution prepared in the step S1, wherein the alkaline aqueous solution is an ammonia water solution with the concentration of 20 wt%, the dropping speed of the ammonia water solution is 10ml/min, precipitation aging treatment is carried out at the temperature of 60-70 ℃, the time of deep precipitation aging is 8h, the pH value of the solution during precipitation is 7-10, after the upper layer liquid is clarified, suction filtration is carried out on the upper layer liquid to collect the lower layer precipitate, the lower layer precipitate is repeatedly washed by deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, washing is stopped, and the precipitate A and the precipitate B are obtained in the reaction kettle A and the reaction kettle B respectively.
S2.1, repeatedly washing the precipitate A and the precipitate B prepared in the step S2 with absolute ethyl alcohol for at least two times, and then placing the precipitates in an oven for drying, wherein the drying temperature is 90-100 ℃, and the drying time is 6 h.
And S3, calcining the precipitate A and the precipitate B treated in the step S2.1 to respectively obtain alumina powder and zirconia powder. The calcination temperature is 900-950 ℃, the calcination time is 5h, and the temperature rise speed is 5 ℃/min. The temperature of the drying air is 200 ℃, the rotating speed of the spray head is 4000rpm, the air pressure difference is 150Pa, and the air outlet temperature is 100 ℃. Respectively weighing 15 parts by mass of zirconia and 92 parts by mass of alumina, mixing, and then sending into a spray drying tower for spray drying granulation to obtain zirconia and alumina mixed powder.
S4, dry-pressing the mixed powder obtained in the step S3 to obtain a molded body: firstly, pressurizing the zirconia toughened alumina powder by using a press with the pressure of 20MPa for 5min to obtain a biscuit with the density of 2.8-3.0g/cm3And then carrying out cold isostatic pressing treatment on the biscuit, wherein the pressure is 150MPa and the time is 5 min.
And S6, sintering the molded body prepared in the step S4 in the air atmosphere, wherein the sintering temperature is 1430-1440 ℃, the sintering time is 8h, the heating rate is 5 ℃/min during heating, and the zirconia toughened alumina ceramic is obtained after sintering.
As shown in FIGS. 3 and 4, the particle size distribution of example 4, which is measured to have an average D50 particle size of 0.722 μm, the particle size distribution of comparative example, which is measured to have an average D50 particle size of 0.757 μm, shows only a single peak in the particle size distribution of FIG. 3, and shows that the particle size distribution of example 4 is relatively uniform.
The ceramics obtained in example 4 and comparative example were measured for particle size, flexural strength and hardness, respectively, and the results are shown in table 1. The ceramics obtained in example 4 were tested nine times, and the test results are shown as numbers 1 to 9, and it can be seen from the test results that the ceramics obtained in example 4 of the present invention have uniform particle size distribution, high bending strength, high hardness, and excellent comprehensive mechanical properties. The ceramic prepared by the method of the comparative example has obviously larger grain diameter and much poorer mechanical property than that of the example 4.
TABLE 1
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the zirconia toughened alumina powder is characterized by comprising the following steps:
s1, mixing the aluminum nitrate solution and the zirconium nitrate solution, stirring for the first time, adding the surfactant, and stirring for the second time at the temperature of 70-90 ℃ to obtain a first solution;
s2, adding an alkaline aqueous solution into the first solution prepared in the step S1, carrying out precipitation aging treatment, and carrying out suction filtration on the reacted first solution to collect lower-layer precipitates to obtain a precipitate mixture;
and S3, calcining the precipitation mixture to obtain zirconia-toughened alumina composite powder, and performing spray granulation on the composite powder to obtain the zirconia-toughened alumina powder.
2. The method of producing zirconia toughened alumina powder of claim 1, wherein: in the step S1, the first stirring and the second stirring are both magnetic stirring, and the time is 20-30 min.
3. The method of producing zirconia toughened alumina powder of claim 1, wherein: the alkaline aqueous solution in the step S2 is an ammonia aqueous solution with the concentration of 20-30 wt%.
4. The method of producing zirconia toughened alumina powder of claim 1, wherein: and in the step S2, repeatedly washing the lower-layer precipitate with deionized water until the conductivity of the deionized water is less than or equal to 2.0 mu S/cm, and stopping washing.
5. The method of producing zirconia toughened alumina powder of claim 1, wherein: the method also comprises the following steps after the step S2:
and repeatedly washing the precipitate mixture by using absolute ethyl alcohol, and drying.
6. The method of producing zirconia toughened alumina powder of claim 1, wherein: the calcination temperature in the step S3 is 900-1100 ℃, and the calcination time is 3-5 h.
7. The method of producing zirconia toughened alumina powder of claim 1, wherein: the zirconia toughening alumina powder contains 15-25 parts by mass of zirconia and 85-92 parts by mass of alumina.
8. A preparation method of zirconia toughened alumina ceramic is characterized by comprising the following steps: a method of making a zirconia toughened alumina powder comprising the method of claim 1, further comprising the steps of:
and S4, carrying out dry pressing molding on the zirconia toughened alumina powder to obtain a molded body.
9. A preparation method of zirconia toughened alumina ceramic is characterized by comprising the following steps: a method of making a zirconia toughened alumina powder comprising the method of claim 1, further comprising the steps of:
s5, mixing the zirconia toughened alumina powder with a dispersant and a binder to prepare slurry, preparing the slurry into a green body, and heating and discharging the green body to obtain a formed body.
10. The method for preparing zirconia toughened alumina ceramic according to claim 8 or 9, further comprising the steps of:
and S6, sintering the formed body in an air atmosphere to obtain the zirconia toughened alumina ceramic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011437485.2A CN112456979A (en) | 2020-12-07 | 2020-12-07 | Preparation method of zirconia toughened alumina powder and ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011437485.2A CN112456979A (en) | 2020-12-07 | 2020-12-07 | Preparation method of zirconia toughened alumina powder and ceramic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112456979A true CN112456979A (en) | 2021-03-09 |
Family
ID=74801535
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011437485.2A Pending CN112456979A (en) | 2020-12-07 | 2020-12-07 | Preparation method of zirconia toughened alumina powder and ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112456979A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908959A (en) * | 2014-03-27 | 2014-07-09 | 台州欧信环保净化器有限公司 | Ce-Zr composite alumina oxide material and preparation method thereof |
| CN109574659A (en) * | 2018-12-14 | 2019-04-05 | 南京云启金锐新材料有限公司 | A kind of ceramic manual casing white oxide zirconium powder body and preparation method thereof |
-
2020
- 2020-12-07 CN CN202011437485.2A patent/CN112456979A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908959A (en) * | 2014-03-27 | 2014-07-09 | 台州欧信环保净化器有限公司 | Ce-Zr composite alumina oxide material and preparation method thereof |
| CN109574659A (en) * | 2018-12-14 | 2019-04-05 | 南京云启金锐新材料有限公司 | A kind of ceramic manual casing white oxide zirconium powder body and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈国清等: "纳米Al2O3/ZrO2复合粉体的制备及表征", 《材料科学与工艺》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107628643B (en) | A kind of nanometer of yttrium stable zirconium oxide raw powder's production technology | |
| CN113831136B (en) | Solid-phase sintered silicon carbide product and preparation method thereof | |
| CN106977185B (en) | A kind of aluminium oxide ceramics and preparation method thereof | |
| CN108059479B (en) | Preparation process of novel porous ceramic heating body | |
| CN108203300B (en) | Preparation method of high-toughness and high-resistivity silicon carbide ceramic | |
| CN106966732B (en) | Fine powder silicon carbide ceramic and preparation method thereof | |
| CN111004034B (en) | Silicon carbide ceramic, method for producing same, and semiconductor component | |
| CN106747557A (en) | The preparation method of plate diamond spar ceramic film support | |
| CN111153434A (en) | Preparation method of lanthanum zirconate spherical powder for thermal spraying | |
| CN113277859B (en) | Nano-coated alumina particles and high-purity thermal shock resistant alumina ceramic material prepared from same | |
| CN102875157A (en) | Preparation method of aluminum oxide ceramics | |
| CN110668813A (en) | Preparation method of nano zirconia granulated powder | |
| WO2023088019A1 (en) | Preparation method for silicon nitride ceramic granulated powder | |
| CN101687710B (en) | Composite article and related method | |
| CN111233468B (en) | Preparation method of yttrium-stabilized zirconium powder for structural component | |
| CN107963890B (en) | Preparation method of titanium nitride porous conductive ceramic | |
| CN110078120A (en) | A kind of preparation method of the yttria-stabilized zirconia powder based on supercritical dispersion roasting | |
| CN110015889A (en) | A kind of ZTA ceramic material preparation method and its material of preparation | |
| CN103449819A (en) | Gel casting molding process for mass production of silicon nitride ceramics | |
| CN112194491A (en) | Pressureless sintering boron carbide ceramic powder and preparation method and application thereof | |
| CN112456979A (en) | Preparation method of zirconia toughened alumina powder and ceramic | |
| CN116354729B (en) | SiC ceramic part and preparation method and application thereof | |
| CN112430114A (en) | Zirconium-aluminum composite nano ceramic and preparation method thereof | |
| CN108046834B (en) | Preparation process of porous ceramic heating body with mosaic structure | |
| CN108147814B (en) | Method for sintering zirconia ceramic at low temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210309 |