CN116789186A - Uniform (ZrTiCoNiNb) O high-entropy oxide powder and preparation method and application thereof - Google Patents
Uniform (ZrTiCoNiNb) O high-entropy oxide powder and preparation method and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 9
- 238000011049 filling Methods 0.000 claims abstract description 4
- 239000000919 ceramic Substances 0.000 claims description 21
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 11
- 229910052863 mullite Inorganic materials 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 9
- 239000000835 fiber Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 5
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract description 19
- 239000011224 oxide ceramic Substances 0.000 abstract description 19
- 238000005245 sintering Methods 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
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- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
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- 230000000052 comparative effect Effects 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
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- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
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Abstract
The invention relates to the technical field of preparation of high-entropy ceramic materials, in particular to uniform (ZrTiCoNiNb) O high-entropy oxide powder, and a preparation method and application thereof. (ZrTiCoNiNb) O high entropy oxide powder is prepared according to the following steps: zrO (ZrO) 2 、TiO 2 、CoO、NiO、Nb 2 O 5 Ball milling and mixing uniformly to obtain raw material mixed powder; and filling the raw material mixed powder into a crucible, introducing a temperature field adjusting mechanism, and performing microwave treatment to obtain the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material. Based on the characteristic of microwave heating, the SiC rod is introduced into the microwave heating heat-preserving structure to adjust the temperature field of the sample, so that uniform and stable high-entropy oxide ceramic powder is obtained by utilizing microwave heating, and the sintering process is short-time, rapid, environment-friendly and efficient, and has a good application prospect.
Description
Technical Field
The invention relates to the technical field of high-entropy ceramic materials, in particular to uniform (ZrTiCoNiNb) O high-entropy oxide powder, and a preparation method and application thereof.
Background
The high-entropy material is a new material which appears in recent years, is a novel multi-principal material which is composed of a plurality of elements in the same amount of substances or in the same amount of substances, and breaks through the design concept of the traditional material. The high-entropy material shows a plurality of tissue and performance characteristics different from those of the traditional material due to the unique crystal structure characteristics, and the special mechanical, electrical, magnetic and other performances of the high-entropy material are also a great hot spot for material research in recent years.
At present, reports on high-entropy ceramic powder are few, most researches focus on preparation of blocks and coatings, and the high-entropy ceramic powder can be used for preparation of block materials, coating materials, 3D printing and other rapid prototyping technologies, so that the high-entropy ceramic is applied to more fields. Different from the powder prepared by crushing the bulk material, the particle size and shape of the directly prepared powder are more uniform, the efficiency is improved, and the production cost is reduced.
In the current preparation method of the high-entropy ceramic powder, the traditional sintering equipment has the defects of slow heat conduction rate of an electric furnace, long preparation period, high cost, insufficient energy utilization and environmental pollution; other novel preparation methods, such as spray pyrolysis, injection molding and the like, have complex procedures and are not beneficial to popularization and mass production. If the preparation method can be used for making a great breakthrough in the preparation process of the high-entropy ceramic powder, the preparation method has great significance for the application of the high-entropy ceramic powder in various fields.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the uniform (ZrTiCoNiNb) O high-entropy oxide powder and the preparation method and application thereof.
The invention aims to provide a method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by regulating a microwave temperature field, which comprises the following steps: the energy dissipation of the ceramic material to the outside is reduced in the heating process, and the sample is kept heated uniformly;
in order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of uniform (ZrTiCoNiNb) O high-entropy oxide powder comprises the following steps:
step 1, zrO 2 、TiO 2 、CoO、NiO、Nb 2 O 5 Uniformly mixing to obtain raw material mixed powder;
and 2, filling the raw material mixed powder in the step 1 into a crucible, then adjusting a temperature field, and heating by microwaves at 800-1200 ℃ for 0.5-1.5 h to obtain the (ZrTiCoNiNb) O high-entropy oxide powder material.
Preferably, the mixing method in the step 1 is a wet ball milling method, and the ball-to-material ratio is 3-6: 1, the ball milling rotating speed is 200-350 r/min, and the ball milling time is 6-10 h.
Preferably, the ball milling in the step 1 is carried out until the average particle size of the raw material mixed powder is 0.1-1 mu m.
Preferably, zrO in the step 1 2 、TiO 2 、CoO、NiO、Nb 2 O 5 The molar ratio of (2) to (1).
Preferably, the microwave heating frequency in the step 2 is 2.45GHz, the heating temperature is 800-2000 ℃, the heating time is 1-2 h, and the heating rate is 50-100 ℃/min.
Preferably, the temperature field adjusting method in the step 2 is as follows: a plurality of mullite plates are added around a crucible to construct a placing cavity, ceramic fiber heat preservation cotton is wound on the inner side and the outer side of the mullite plates together, siC rods are inserted into the ceramic fiber heat preservation cotton, then the crucible is placed in the placing cavity formed by the mullite plates, and then the top of the crucible is covered with the SiC rods.
Preferably, the SiC rod has a length of 3 to 10cm and a diameter of 3 to 10mm.
The invention also protects the uniform (ZrTiCoNiNb) O high-entropy oxide powder material prepared by the preparation method.
The invention also protects the application of the uniform (ZrTiCoNiNb) O high-entropy oxide powder material in preparing the high-entropy ceramic material.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention effectively reduces the sintering temperature, shortens the sintering time, realizes the microwave synthesis of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder, and enriches the ceramic material system.
(2) The invention adopts the microwave heating sintering technology to successfully prepare the high-entropy ceramic powder material, and the preparation method has simple process and low cost. The method is suitable for mass production of novel high-entropy ceramic materials, engineering application is further realized, and the prepared process substrate is high in strength and suitable for fine processing under severe conditions, so that the application range of the high-entropy ceramic materials is further widened.
(3) The invention provides a preparation method of the uniform and stable ceramic material, which adopts a process for optimizing a heat preservation structure, regulates and controls a sample temperature field through a SiC rod, reduces the temperature gradient between the sample and the environment, reduces heat dissipation, can effectively improve the heating rate, improves the uniformity of the material and reduces energy consumption.
Drawings
FIG. 1 is a schematic diagram of a microwave heating insulation structure of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material prepared in example 1;
FIG. 2 is a graph showing the temperature rise of microwave heating of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material prepared in example 1;
FIG. 3 is a comparative image of the (ZrTiCoNiNb) O high entropy oxide ceramic powder material obtained in example 1 with or without SiC rod added to regulate the temperature field;
FIG. 4 is an XRD contrast image of the (ZrTiCoNiNb) O high entropy oxide ceramic powder material prepared in example 1 with or without the addition of SiC rod to regulate the temperature field.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods described in the examples of the present invention are conventional methods unless otherwise specified.
Example 1
A method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by adjusting a microwave temperature field comprises the following steps:
step 1, preparing raw material mixed powder: zrO is weighed according to the mol ratio of 2:2:2:2:1 respectively 2 、TiO 2 、CoO、NiO、Nb 2 O 5 Mixing the obtained mixture with absolute ethyl alcohol, performing wet ball milling, wherein the ball-milling ball-material ratio is 5:1, the rotating speed is 290r/min, the ball milling time is 6h, and the ball milling is performed until the average particle size of the mixed powder is 0.5 mu m, so as to obtain raw material mixed powder;
step 2, preparing high-entropy ceramic powder: taking 30g of raw material mixed powder, filling the mixed powder into an alumina crucible, placing the alumina crucible into a tetragonal thermal insulation structure consisting of a mullite plate and ceramic fiber thermal insulation cotton, placing four SiC rods with the length of 3cm in the thermal insulation structure, placing three SiC rods with the length of 4cm above the crucible, heating the crucible to 900 ℃ for 25min by normal-temperature microwaves, then preserving the temperature at 900 ℃ for 5min, wherein the frequency is 2.45GHz, and the heating rate is 50 ℃/min, thus obtaining the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material.
Example 2
A method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by adjusting a microwave temperature field comprises the following steps:
step 1, preparing raw material mixed powder: zrO is weighed according to the mol ratio of 2:2:2:2:1 respectively 2 、TiO 2 、CoO、Nb 2 O 5 Mixing the obtained mixture with absolute ethyl alcohol, performing wet ball milling, wherein the ball-material ratio of ball milling is 5:1, the rotating speed is 300r/min, the ball milling time is 8 hours, and the ball milling is performed until the average particle size of the mixed powder is 0.4 mu m, so as to obtain mixed powder;
step 2, preparing high-entropy ceramic powder: 50g of mixed powder is filled in an alumina crucible, the alumina crucible is placed in a tetragonal thermal insulation structure consisting of a mullite plate and ceramic fiber thermal insulation cotton, six SiC rods with the length of 5cm are placed in the thermal insulation structure, the SiC rods are heated to 1000 ℃ by normal-temperature microwaves for 30min, then the mixed powder is subjected to thermal insulation at 1000 ℃ for 10min, the frequency is 2.45GHz, and the heating rate is 60 ℃/min, so that the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material is obtained.
Example 3
A method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by adjusting a microwave temperature field comprises the following steps:
step 1, preparing raw material mixed powder: zrO is weighed according to the mol ratio of 2:2:2:2:1 respectively 2 、TiO 2 、CoO、Nb 2 O 5 Mixing the obtained mixture with absolute ethyl alcohol, performing wet ball milling, wherein the ball-material ratio of ball milling is 5:1, the rotating speed is 310r/min, the ball milling time is 10h, and the ball milling is performed until the average particle size of the mixed powder is 0.3 mu m, so as to obtain mixed powder;
step 2, preparing high-entropy ceramic powder: 80g of mixed powder is filled in an alumina crucible, the alumina crucible is placed in a tetragonal thermal insulation structure consisting of a mullite plate and ceramic fiber thermal insulation cotton, four SiC rods with the length of 6cm are placed above a sample, the temperature is kept at 1100 ℃ for 50min by microwave heating at normal temperature, the temperature is kept at 1100 ℃ for 15min, the frequency is 2.45GHz, and the heating rate is 80 ℃/min, so that the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material is obtained.
Example 4
A method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by adjusting a microwave temperature field comprises the following steps:
step 1, preparing raw material mixed powder: zrO is weighed according to the mol ratio of 2:2:2:2:1 respectively 2 、TiO 2 、CoO、Nb 2 O 5 Mixing the obtained mixture with absolute ethyl alcohol, performing wet ball milling, wherein the ball-material ratio of ball milling is 3:1, the rotating speed is 200r/min, the ball milling time is 10 hours, and the ball milling is performed until the average particle size of the mixed powder is 1 mu m, so as to obtain mixed powder;
step 2, preparing high-entropy ceramic powder: 80g of mixed powder is filled in an alumina crucible, the alumina crucible is placed in a tetragonal thermal insulation structure consisting of a mullite plate and ceramic fiber thermal insulation cotton, four SiC rods with the length of 6cm are placed above a sample, the temperature is kept at the temperature of 800 ℃ for 20min after being heated to 1100 ℃ by normal-temperature microwaves, the temperature is kept at the temperature of 800 ℃ for 70min, the frequency is 2.45GHz, and the heating rate is 50 ℃/min, so that the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material is obtained.
Example 5
A method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder by adjusting a microwave temperature field comprises the following steps:
step 1, preparing raw material mixed powder: zrO is weighed according to the mol ratio of 2:2:2:2:1 respectively 2 、TiO 2 、CoO、Nb 2 O 5 Mixing the obtained mixture with absolute ethyl alcohol, performing wet ball milling, wherein the ball-material ratio of ball milling is 6:1, the rotating speed is 350r/min, the ball milling time is 6h, and the ball milling is performed until the average particle size of the mixed powder is 0.1 mu m, so as to obtain mixed powder;
step 2, preparing high-entropy ceramic powder: 80g of mixed powder is filled in an alumina crucible, the alumina crucible is placed in a tetragonal thermal insulation structure consisting of a mullite plate and ceramic fiber thermal insulation cotton, four SiC rods with the length of 10cm are placed above a sample, the temperature is kept at 1200 ℃ for 60min by microwave heating at normal temperature, the temperature is kept at 1200 ℃ for 20min, the frequency is 2.45GHz, and the heating rate is 100 ℃/min, so that the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material is obtained.
Experimental part
In order to observe the phase difference of the high-entropy oxide ceramic powder materials prepared under different variables, the (ztic oninb) O high-entropy oxide ceramic powder materials obtained in examples 1 to 3 were phase-characterized by means of an X-ray diffraction analyzer (XRD) (SmartLab, japan electric motor corporation);
FIG. 1 is a schematic view of the thermal insulation structure of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material prepared in the embodiment 1 of the invention. Fig. 2 is a microwave sintering heating curve of the (zrticenb) O high-entropy oxide ceramic powder material prepared in embodiment 1 of the present invention, and as can be seen from the microwave heating curve in fig. 2, the heating rate is gentle, the SiC rod helps to construct a temperature field around the sample, so that the internal and external temperature fields of the sample are uniform, the temperature gradient difference is slowed down, the heating rate is balanced, the sample starts to heat up in about 12min, the temperature can be raised to 900 ℃ in about 20min, and the overall sintering time is within 30min, so that the experimental cost and energy consumption are saved.
Fig. 3 and fig. 4 are characterization images of example 1 of the present invention, and fig. 3 is a comparative image of the (ztic) ninb) O high entropy oxide ceramic powder material finally prepared in example 1, with or without SiC rod added to regulate the temperature field; it can be seen that the surface reaction of the temperature field is more complete by adding the SiC rod;
FIG. 4 is an XRD contrast image of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material prepared in example 1, wherein the temperature field is regulated by adding a SiC rod, and the result shows that the composition structure of a surface layer sample after the temperature field is regulated is more consistent with that of the inside.
Compared with other traditional sintering methods, the microwave heating mode is a bulk heating mode, in the microwave heating process, microwaves with special wave bands can directly interact with material particles (molecules and ions) to be coupled with basic microstructure of the material to generate heat, so that rapid heating is realized, and the components of the sample are uniform. The microwave heating technology can effectively reduce the synthesis cost of the (ZrTiCoNiNb) O high-entropy oxide ceramic powder material and improve the synthesis efficiency.
It should be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (9)
1. The preparation method of the uniform (ZrTiCoNiNb) O high-entropy oxide powder is characterized by comprising the following steps of:
step 1, zrO 2 、TiO 2 、CoO、NiO、Nb 2 O 5 Uniformly mixing to obtain raw material mixed powder;
and 2, filling the raw material mixed powder in the step 1 into a crucible, then adjusting a temperature field, and heating by microwaves at 800-1200 ℃ for 0.5-1.5 h to obtain the (ZrTiCoNiNb) O high-entropy oxide powder material.
2. The method for preparing uniform (zrticenb) O high-entropy oxide powder according to claim 1, wherein the mixing method in step 1 is a wet ball milling method, and the ball-to-material ratio is 3-6: 1, the ball milling rotating speed is 200-350 r/min, and the ball milling time is 6-10 h.
3. The method for preparing uniform (zrticenb) O high-entropy oxide powder according to claim 2, wherein the average particle size of the raw material mixed powder is 0.1-1 μm.
4. The method for preparing uniform (ZrTiCoNiNb) O high-entropy oxide powder according to claim 1, wherein ZrO in said step 1 2 、TiO 2 、CoO、NiO、Nb 2 O 5 The molar ratio of (2) to (1).
5. The method for preparing uniform (ztic oninb) O high-entropy oxide powder according to claim 1, wherein the microwave heating frequency in the step 2 is 2.45GHz, the heating temperature is 800-2000 ℃, the heating time is 1-2 h, and the heating rate is 50-100 ℃/min.
6. The method for preparing uniform (zrticenb) O high-entropy oxide powder according to claim 1, wherein the method for adjusting the temperature field in step 2 is as follows: a plurality of mullite plates are added around a crucible to construct a placing cavity, ceramic fiber heat preservation cotton is wound on the inner side and the outer side of the mullite plates together, siC rods are inserted into the ceramic fiber heat preservation cotton, then the crucible is placed in the placing cavity formed by the mullite plates, and then the top of the crucible is covered with the SiC rods.
7. The method for preparing uniform (zrticenb) O high-entropy oxide powder according to claim 1, wherein the SiC rod has a length of 3 to 10cm and a diameter of 3 to 10mm.
8. A homogeneous (ztic oninb) O high entropy oxide powder material prepared by the preparation method of any one of claims 1 to 7.
9. Use of a homogeneous (ztic oninb) O high-entropy oxide powder material according to claim 8 for the preparation of a high-entropy ceramic material.
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| CN117658242A (en) * | 2024-01-30 | 2024-03-08 | 太原理工大学 | Nano spinel type high entropy oxide with high wave absorbing capacity, preparation method and application thereof |
| CN117658242B (en) * | 2024-01-30 | 2024-04-19 | 太原理工大学 | Nano spinel type high entropy oxide with high wave absorbing capacity, preparation method and application thereof |
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