CN110204328B - Preparation method of high-entropy oxide ceramic - Google Patents
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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.
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