CN110204328B - Preparation method of high-entropy oxide ceramic - Google Patents
Preparation method of high-entropy oxide ceramic Download PDFInfo
- Publication number
- CN110204328B CN110204328B CN201910485418.9A CN201910485418A CN110204328B CN 110204328 B CN110204328 B CN 110204328B CN 201910485418 A CN201910485418 A CN 201910485418A CN 110204328 B CN110204328 B CN 110204328B
- Authority
- CN
- China
- Prior art keywords
- oxide ceramic
- powder
- entropy oxide
- preset
- entropy
- 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.)
- Active
Links
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
-
- 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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium 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
- C04B35/01—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
- C04B35/45—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 copper oxide or solid solutions thereof with other oxides
-
- 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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
-
- 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
- C04B35/64—Burning or sintering processes
-
- 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
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
- C04B2235/3277—Co3O4
-
- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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)
Abstract
The invention discloses a preparation method of high-entropy oxide ceramic, which comprises the following steps: step 1: respectively weighing 4 or less than 5 metal oxide powders according to the metal atom molar ratio of 1:1:1:1 or 1:1:1: 1; the oxide powder includes: MgO, ZnO, NiO, CuO, CaO, CoO, ZrO2、CeO2、Al2O3、Gd2O3、La2O3、Er2O3、Y2O3、Fe2O3、Co3O4、CaCO3(ii) a Step 2: performing ball milling, drying and granulation on the powder weighed in the step 1; and step 3: pressing and molding the granulated powder to obtain a green body; and 4, step 4: carrying out heat treatment on the green body obtained in the step 3; and 5: heating the green body subjected to the heat treatment in the step 4 to reach a preset temperature, applying an electric field with a preset electric field intensity to the sample, converting a power supply from a constant voltage state to a constant current state after flash firing, preserving heat for 1-60 min under a preset current density, and then quenching to obtain the required high-entropy oxide ceramic; the invention adopts flash firing to prepare the high-entropy oxide ceramic, thereby obviously reducing the sintering temperature and shortening the sintering time.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a preparation method of high-entropy oxide ceramic.
Background
The high-entropy ceramic material is a ceramic material which is composed of more than three metal elements and 1 non-metal element and has a single crystal structure. Wherein the mole percentages of the metal elements are substantially the same. At present, the reported high-entropy ceramics mainly comprise high-entropy oxides, high-entropy borides, high-entropy carbides and high-entropy silicides. The high-entropy ceramic material has higher entropy value and larger lattice distortion, and shows unique mechanical, electrical and optical properties.
The current method for preparing high-entropy oxide ceramics is generally solid-phase sintering, and binary oxide powder is mixed and sintered at high temperature to ensure that atoms are fully diffused and mixed. However, such solid phase sintering generally requires a long time; for example, 1000A is prepared from powders of MgO, NiO, CoO, CuO, ZnO, etcoSynthesis of Mg under C conditions0.2Ni0.2Co0.2Cu0.2Zn0.2O takes 12 hours [ C.M. Rost, E. Sachet, T. Borman, et al, control-stabilized oxides, nat. Commun. 6 (2015) 8485.]. In addition, the atomization spray pyrolysis, flame spray pyrolysis and reverse coprecipitation methods are also used for synthesizing high-entropy oxide powders [ A. Sarkar, R. Djenadic, N.J. Usharani, et al, Nanocrystalline multicomponent entry stable transformation metals, J. Eur. Ceram. Soc. 37(2 (2017)) 747-.]. The atomization spray pyrolysis and the flame spray pyrolysis have the advantages of short synthesis time, rapid quenching and the like, and are suitable for synthesizing high-entropy oxide powder. However, the method is only suitable for synthesizing high-entropy oxide powder and is not suitable for preparing high-entropy oxide ceramics.
Disclosure of Invention
The invention provides a preparation method of high-entropy oxide ceramic, which has simple preparation process, low sintering temperature and short sintering time.
The technical scheme adopted by the invention is as follows: a preparation method of high-entropy oxide ceramic comprises the following steps:
step 1: respectively weighing 4 or less than 5 metal oxide powders according to the metal atom molar ratio of 1:1:1:1 or 1:1:1: 1; the oxide powder includes: MgO, ZnO, NiO, CuO, CaO, CoO, ZrO2、CeO2、Al2O3、Gd2O3、La2O3、Er2O3、Y2O3、Fe2O3、Co3O4、CaCO3；
Step 2: performing ball milling, drying and granulation on the powder weighed in the step 1;
and step 3: pressing and molding the granulated powder to obtain a green body;
and 4, step 4: carrying out heat treatment on the green body obtained in the step 3;
and 5: heating the green body subjected to the heat treatment in the step 4 to reach a preset temperature, applying an electric field with a preset electric field intensity to the sample, converting a power supply from a constant voltage state to a constant current state after flash firing, preserving heat for 1-60 min under a preset current density, and then quenching to obtain the required high-entropy oxide ceramic;
the preset electric field intensity is 10-1000V/cm, and the preset current density is 10-3000 mA/mm2。
Further, planetary ball milling is adopted for ball milling in the step 2, the rotating speed of the ball mill is 50-180 r/min, and the ball milling time is 10-50 h.
Further, in the step 5, the preset temperature is room temperature to 0.7 Tm, the heating rate is 10 to 30 ℃/min, and the temperature is kept for 10 min after the preset temperature is reached.
Further, in the step 2, granulation is performed, and PVA is added to the ceramic powder for granulation, wherein the concentration of the PVA is 3 wt%.
Further, secondary pressing is adopted in the pressing and molding in the step 3, and pressure is maintained for 30-60 s under the condition that the pressure is 100-200 MPa; and then carrying out secondary pressurization under the pressure of 200-300 MPa.
Further, the heat treatment process in step 4 is as follows:
heat treatment is carried out for 2 hours under the condition of 0.5 Tm, and the heating rate is 2-5 ℃/min.
Further, in the step 2, the drying temperature is 100 ℃, and the heat preservation time is 10-30 hours.
The invention has the beneficial effects that:
(1) the invention adopts flash firing to prepare high-entropy oxide ceramics, thereby obviously reducing the synthesis temperature and shortening the sintering time;
(2) the method can realize the rapid movement and mixing of metal atoms in a short time, and obtain the high-entropy oxide ceramic with a single crystal structure.
Drawings
FIG. 1 is an XRD pattern of the high-entropy oxide ceramic prepared in example 1 of the present invention.
FIG. 2 is an XRD pattern of the high-entropy oxide ceramic prepared in example 2 of the present invention.
FIG. 3 is an EDS diagram of the high-entropy oxide ceramic prepared in example 1 of the present invention.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
A preparation method of high-entropy oxide ceramic comprises the following steps:
step 1: respectively weighing 4 or less than 5 metal oxide powders according to the metal atom molar ratio of 1:1:1:1 or 1:1:1: 1; the oxide powder includes: MgO, ZnO, NiO, CuO, CaO, CoO, ZrO2、CeO2、Al2O3、Gd2O3、La2O3、Er2O3、Y2O3、Fe2O3、Co3O4、CaCO3；
Step 2: performing ball milling, drying and granulation on the powder weighed in the step 1;
and adding deionized water into the weighed powder, and mixing in a planetary ball mill at the rotating speed of 50-180 r/min for 10-50 h. And drying the obtained slurry at the drying temperature of 100 ℃ for 10-30 h to obtain uniformly mixed ceramic powder. And adding PVA into the dried ceramic powder for granulation, wherein the concentration of the PVA is 3 wt%.
And step 3: pressing and molding the granulated powder to obtain a green body;
pressing the granulated powder into a sample by adopting a die pressing method, wherein the sample is a bone sample, the pressure is 100-200 MPa, and the pressure is maintained for 30-60 s; and then placing the sample in a cold isostatic press to carry out secondary pressure test at the pressure of 200-300 MPa.
And 4, step 4: carrying out heat treatment on the green body obtained in the step 3;
and carrying out heat treatment on the obtained green body at 0.5 Tm for 2 h, wherein the heating rate is 2-5 ℃/min.
And 5: and (4) connecting the green body subjected to the heat treatment in the step (4) with a platinum electrode in a flash furnace, heating to room temperature to 0.7 Tm at a heating rate of 10-30 ℃/min, and after reaching a preset temperature, keeping the temperature at the temperature for 1-10 min to ensure that the temperature of the sample is consistent with the furnace temperature.
Applying an electric field with preset electric field strength to the sample, keeping the electric field constant until the power supply is changed from a constant voltage state to a constant current state after flash burning occurs, preserving the heat for 1-60 min under the preset current density, and then putting the sample into ice water for quenching to obtain the required high-entropy oxide ceramic;
the preset electric field intensity is 10-1000V/cm, and the preset current density is 10-3000 mA/mm2。
Example 1
A preparation method of high-entropy oxide ceramic comprises the following steps:
step 1: weighing oxide powder and ZnO according to the following molar ratio: MgO: NiO: CuO: co3O4Powder was weighed to total 21.37 g, 3:3:3: 1.
Step 2: adding 200 mL of deionized water into the weighed powder, and mixing in a planetary ball mill at the rotating speed of 180r/min for 12 h; drying the obtained slurry at the drying temperature of 98 ℃ for 24 hours to obtain ceramic powder which is uniformly mixed; and adding PVA into the dried ceramic powder for granulation, wherein the concentration of the PVA is 3 wt%.
And step 3: pressing the granulated powder into a dog-bone-shaped sample by adopting a mould pressing method (the sample is conveniently connected with an electrode in a flash furnace); maintaining the pressure for 60 s under the condition that the pressure is 200 MPa. The sample was placed in a cold isostatic press and subjected to secondary pressing at a pressure of 290 MPa.
And 4, step 4: carrying out heat treatment on the green body obtained in the step 3 at 500 ℃ for 2 h, wherein the heating rate is 2oAnd C/min. To facilitate the testing of samples withPlatinum wires are connected, and holes with phi of 1.6 +/-0.1 mm are formed at two ends of the sample. The gauge length dimensions of the test specimen were 16.52 mm by 2.85 mm by 1.50 mm.
And 5: after the green body was prepared, the sample was attached to a platinum electrode in a scintillation furnace. Under the condition of room temperature, the current density is set to be 100 mA/mm2Subsequently, an electric field of 250V/cm was applied. The electric field intensity is kept constant until flash burning occurs, and the power supply is changed from a constant voltage state to a constant current state. At 100 mA/mm2And (3) keeping the temperature for 1min under a constant current state, then removing the applied electric field, and quickly placing the sample in ice water for quenching to obtain the high-entropy oxide ceramic.
As can be seen from FIG. 1, the crystal structures of ZnO, MgO, NiO, CuO and Co are different from each other3O4After the five ceramic materials are subjected to flash firing treatment, the rapid movement and mixing of metal atoms are realized in a short time, and the five-element high-entropy oxide ceramic with a single crystal structure is obtained. As can be seen from FIG. 3, ZnO, MgO, NiO, CuO, and Co were formed by flash firing at room temperature3O4Zn, Mg, Ni, Cu and Co elements in the five ceramic materials are completely uniformly mixed within 1min of heat preservation time, and no enrichment of metal cations appears on an energy spectrum diagram.
Example 2
A preparation method of high-entropy oxide ceramic comprises the following steps:
step 1: weighing oxide powder and ZnO according to the following molar ratio: NiO: CuO: co3O4Powder was weighed to give 20 g in total, where =3:3:3: 1.
Step 2: adding 200 mL of deionized water into the weighed powder, and mixing in a planetary ball mill at the rotating speed of 180r/min for 12 h; drying the obtained slurry at the drying temperature of 98 ℃ for 24 hours to obtain ceramic powder which is uniformly mixed; and adding PVA into the dried ceramic powder for granulation, wherein the concentration of the PVA is 3 wt%.
And step 3: pressing the granulated powder into a dog-bone-shaped sample by adopting a mould pressing method (the sample is conveniently connected with an electrode in a flash furnace); maintaining the pressure for 60 s under the condition that the pressure is 200 MPa. The sample was placed in a cold isostatic press and subjected to secondary pressing at a pressure of 290 MPa.
And 4, step 4: carrying out heat treatment on the green body obtained in the step 3 at 500 ℃ for 2 h, wherein the heating rate is 2oAnd C/min. In order to facilitate the connection of the sample and the platinum wire, holes with phi of 1.6 +/-0.1 mm are formed at two ends of the sample. The gauge length dimensions of the test specimen were 16.52 mm by 2.85 mm by 1.50 mm.
And 5: after the green body was prepared, the sample was attached to a platinum electrode in a scintillation furnace. Under the condition of room temperature, the current density is set to be 200 mA/mm2Subsequently, an electric field of 60V/cm was applied. The electric field intensity is kept constant until flash burning occurs, and the power supply is changed from a constant voltage state to a constant current state. At 200 mA/mm2And (3) keeping the temperature for 5 min under a constant current state, then removing the applied electric field, and quickly placing the sample in ice water for quenching to obtain the high-entropy oxide ceramic.
As can be seen from FIG. 2, the crystal structures of ZnO, NiO, CuO and Co are different from each other3O4After the four ceramic materials are subjected to flash firing treatment, the rapid movement and mixing of metal atoms are realized in a short time, and the quaternary high-entropy oxide ceramic with a single crystal structure is obtained.
The invention applies the flash sintering technology to the preparation of the high-entropy oxide ceramic, and can obviously reduce the sintering temperature and shorten the sintering time.
Claims (6)
1. A preparation method of high-entropy oxide ceramic is characterized by comprising the following steps:
step 1: respectively weighing 4 or less than 5 metal oxide powders according to the metal atom molar ratio of 1:1:1:1 or 1:1:1: 1; the oxide powder includes: MgO, ZnO, NiO, CuO, CaO, CoO, -ZrO2 、-CeO2 、-Al2O3 、-Gd2O3 、-La2O3 、-Er2O3 、-Y2O3 、-Fe2O3 、-Co3O4 、-CaCO3 ；
Step 2: performing ball milling, drying and granulation on the powder weighed in the step 1;
and step 3: pressing and molding the granulated powder to obtain a green body;
and 4, step 4: carrying out heat treatment on the green body obtained in the step 3;
and 5: heating the green body subjected to the heat treatment in the step (4) to reach a preset temperature, applying an electric field with a preset electric field intensity to the sample, converting a power supply from a constant voltage state to a constant current state after flash firing, preserving heat for 1-60 min under a preset current density, and then quenching with ice water to obtain the required high-entropy oxide ceramic; the preset electric field intensity is 10-1000V/cm, and the preset current density is 10-3000 mA/-mm2 ；
In the step 5, the preset temperature is room temperature to 0.7 Tm, the heating rate is 10 to 30 ℃/min, and the temperature is kept for 10 min after the preset temperature is reached.
2. The preparation method of high-entropy oxide ceramic according to claim 1, wherein ball milling in the step 2 is planetary ball milling, the rotating speed of the ball mill is 50-180 r/min, and the ball milling time is 10-50 h.
3. A process for the preparation of a high entropy oxide ceramic according to claim 1, wherein in step 2, the ceramic powder is granulated by adding PVA to the powder at a concentration of 3 wt%.
4. A preparation method of high-entropy oxide ceramics according to claim 1, wherein the press molding in the step 3 adopts secondary pressing, and firstly, the pressure is maintained for 30-60 s under the condition that the pressure is 100-200 MPa; and then carrying out secondary pressurization under the pressure of 200-300 MPa.
5. A method for preparing a high-entropy oxide ceramic according to claim 1, wherein the heat treatment in step 4 is as follows: heat treatment is carried out for 2 hours under the condition of 0.5 Tm, and the heating rate is 2-5 ℃/min.
6. The preparation method of high-entropy oxide ceramic according to claim 1, wherein the drying temperature in the step 2 is 100 ℃ and the holding time is 10-30 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910485418.9A CN110204328B (en) | 2019-06-05 | 2019-06-05 | Preparation method of high-entropy oxide ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910485418.9A CN110204328B (en) | 2019-06-05 | 2019-06-05 | Preparation method of high-entropy oxide ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110204328A CN110204328A (en) | 2019-09-06 |
| CN110204328B true CN110204328B (en) | 2021-09-07 |
Family
ID=67791027
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910485418.9A Active CN110204328B (en) | 2019-06-05 | 2019-06-05 | Preparation method of high-entropy oxide ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110204328B (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818430B (en) * | 2019-11-12 | 2021-01-19 | 西安交通大学 | Uniform high-entropy oxide ceramic submicron spherical powder and preparation method thereof |
| CN110903084B (en) * | 2019-11-12 | 2021-02-02 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
| CN110950654A (en) * | 2019-12-16 | 2020-04-03 | 东南大学 | High-entropy magnesium aluminate spinel type complex oxide and preparation method thereof |
| CN111924899B (en) * | 2020-08-11 | 2023-03-17 | 中钢集团南京新材料研究院有限公司 | Method for preparing nickel-cobalt-iron-aluminum-magnesium five-element high-entropy material, product and application |
| CN112341160B (en) * | 2020-11-06 | 2022-08-30 | 南京工业大学 | Broadband high-Q low-temperature coefficient barium-magnesium-calcium-niobium-tantalum composite ceramic and preparation method thereof |
| CN113041398A (en) * | 2021-03-16 | 2021-06-29 | 上海大学绍兴研究院 | High-entropy ceramic composite collagen material, preparation method and application thereof, and high-entropy ceramic composite collagen artificial bone |
| CN115340361B (en) * | 2021-05-14 | 2023-02-24 | 郑州大学 | High-entropy ceramic for microwave kiln and preparation method and application thereof |
| CN115594494A (en) * | 2021-07-08 | 2023-01-13 | 武汉苏泊尔炊具有限公司（Cn） | Non-stick material, preparation method thereof, non-stick coating and cooking utensil |
| CN113461415B (en) * | 2021-07-19 | 2022-08-30 | 中国科学院兰州化学物理研究所 | Hydrothermal method for preparing high-entropy oxide material (MAlFeCuMg) 3 O 4 Method (2) |
| CN113912396B (en) * | 2021-11-11 | 2023-03-17 | 江苏金石研磨有限公司 | High-entropy ceramic grinding ball and preparation method thereof |
| CN113929449A (en) * | 2021-11-25 | 2022-01-14 | 西南科技大学 | Nano high-entropy oxide ceramic powder and preparation method thereof |
| CN114907102A (en) * | 2022-04-18 | 2022-08-16 | 国网江西省电力有限公司电力科学研究院 | Ceramic material and room-temperature ultrafast reactive sintering method thereof |
| CN115196968B (en) * | 2022-06-10 | 2023-03-21 | 华南理工大学 | High-entropy boride ceramic powder and preparation method and application thereof |
| CN115159974A (en) * | 2022-06-24 | 2022-10-11 | 东莞理工学院 | SrFeO 3-x Reactive flash firing preparation method of ceramic |
| CN115286389B (en) * | 2022-07-07 | 2023-08-18 | 华南理工大学 | High-entropy carbide ceramic powder and preparation method and application thereof |
| CN115093214A (en) * | 2022-07-21 | 2022-09-23 | 南京信息工程大学 | Ultrafast preparation method of high-entropy oxide |
| CN115838993B (en) * | 2022-12-13 | 2023-09-15 | 南京邮电大学 | High infrared radiation fiber mat and preparation method thereof |
| CN116354407A (en) * | 2023-03-20 | 2023-06-30 | 南京航空航天大学 | High-entropy oxide and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188544A (en) * | 2017-05-04 | 2017-09-22 | 武汉理工大学 | A kind of application flash burning technology sinters the preparation method of zirconium aluminium complex phase eutectic ceramic |
| CN108358646A (en) * | 2018-05-23 | 2018-08-03 | 广东工业大学 | A kind of boronation zirconia-based ceramic and preparation method thereof |
| CN108640659A (en) * | 2018-04-19 | 2018-10-12 | 江苏星源电站冶金设备制造有限公司 | A kind of preparation method of novel oxidized aluminium nanocomposite |
| CN108947542A (en) * | 2018-08-21 | 2018-12-07 | 苏州山人纳米科技有限公司 | The direct flash burning molding method for preparing of ceramic powder stock |
-
2019
- 2019-06-05 CN CN201910485418.9A patent/CN110204328B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188544A (en) * | 2017-05-04 | 2017-09-22 | 武汉理工大学 | A kind of application flash burning technology sinters the preparation method of zirconium aluminium complex phase eutectic ceramic |
| CN108640659A (en) * | 2018-04-19 | 2018-10-12 | 江苏星源电站冶金设备制造有限公司 | A kind of preparation method of novel oxidized aluminium nanocomposite |
| CN108358646A (en) * | 2018-05-23 | 2018-08-03 | 广东工业大学 | A kind of boronation zirconia-based ceramic and preparation method thereof |
| CN108947542A (en) * | 2018-08-21 | 2018-12-07 | 苏州山人纳米科技有限公司 | The direct flash burning molding method for preparing of ceramic powder stock |
Non-Patent Citations (2)
| Title |
|---|
| Microstructural Evolution and Mechanical properties of (Mg,Co,Ni,Cu,Zn)O High Entropy Ceramics;Weichen Hong et al.;《Journal of the American Ceramic Society》;20190430;第102卷(第4期);第2228-2237页 * |
| Reaction assisted flash sintering of Al2O3-YAG ceramic composites with eutectic composition;Hui Zhang et al.;《Ceramics International》;20190328;第45卷(第10期);第13552页的第2-4段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110204328A (en) | 2019-09-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110204328B (en) | Preparation method of high-entropy oxide ceramic | |
| CN109037759B (en) | Sintering method for preparing compact garnet-type lithium ion solid electrolyte | |
| CN110759728A (en) | Linear-like lead-free relaxor ferroelectric ceramic material and preparation method thereof | |
| CN110937893B (en) | Method for improving energy density of pyroelectric composite ceramic material | |
| CN113582667B (en) | Low-temperature cofiring high-energy-storage antiferroelectric ceramic material and preparation method and application thereof | |
| Chen et al. | Ferroelectric and dielectric properties of Sr2− x (Na, K) xBi4Ti5O18 lead-free piezoelectric ceramics | |
| CN114907102A (en) | Ceramic material and room-temperature ultrafast reactive sintering method thereof | |
| CN114436643A (en) | Giant dielectric constant and low dielectric loss ceramic and preparation method thereof | |
| CN103951414A (en) | Method for manufacturing ceramic material with low dielectric loss, large capacitivity and varistor characteristics | |
| CN116063067A (en) | Multi-main-element giant dielectric ceramic material and preparation method and application thereof | |
| CN110862257A (en) | Graphite ceramic closing resistor and preparation method thereof | |
| CN115321976B (en) | CCTO ceramic material with giant dielectric constant and low dielectric loss and preparation method thereof | |
| CN114573338B (en) | Preparation method and application of dielectric ceramic with high energy storage density | |
| CN112794712B (en) | Method for preparing nano hydroxyapatite-zirconia composite material by flash firing method | |
| CN113683419A (en) | Silver niobate-based antiferroelectric energy storage ceramic with high energy storage characteristic and low-temperature sintering method thereof | |
| CN101913857A (en) | Method for preparing high-gradient, high-dielectric and low-loss pressure-sensitive material | |
| CN112062559A (en) | Antiferroelectric ceramic material and low-temperature sintering method thereof | |
| Chang et al. | Preparation of high-Tc superconducting (Bi, Pb) 2Sr2Ca2Cu3Oy phase via an oxalate route | |
| CN114890786B (en) | Near-zero temperature drift 5G ceramic filter material and preparation method thereof | |
| CN111454062B (en) | AlMgB14Preparation method of ceramic material powder | |
| CN108439970B (en) | Rare earth doped perovskite type NTC composite thermosensitive ceramic material and preparation method thereof | |
| JP2638052B2 (en) | High temperature electrical insulating filler and method for producing the same | |
| CN115466102A (en) | Magnesium oxide-based microwave dielectric ceramic with low sintering temperature and high electric strength and preparation method thereof | |
| CN115504770A (en) | Transition metal ion and Nd 3+ Co-doped solid electrolyte ceramic material and preparation method thereof | |
| RU2289552C1 (en) | High-temperature permeable current-conducting material and the method of its production |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |