CN115340361B - High-entropy ceramic for microwave kiln and preparation method and application thereof - Google Patents
High-entropy ceramic for microwave kiln and preparation method and application thereof Download PDFInfo
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- 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
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Abstract
The invention belongs to the technical field of materials for microwave kilns, and particularly discloses a high-entropy ceramic for a microwave kiln and a preparation method and application thereof. The invention dissolves MgCl by absolute ethyl alcohol 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 And drying, ball milling, pressing and molding, and calcining in air atmosphere to obtain the high-entropy ceramic for the microwave kiln. The high-entropy ceramic disclosed by the invention is used for a heat-insulating material of a microwave kiln, and has excellent wave-transmitting, heat-insulating and high-temperature stability performances.
Description
Technical Field
The invention relates to the technical field of materials for microwave kilns, in particular to high-entropy ceramic for a microwave kiln and a preparation method and application thereof.
Background
As an advanced material preparation technology, microwave sintering has the characteristics of high temperature rise speed, high energy utilization rate, high heating efficiency, safety, no pollution and the like, and becomes a new research hotspot in the field of material sintering. Due to the particularity of microwave heating, higher requirements are also put forward on the microwave heat-insulating material, and the excellent synergy of wave transmission, heat insulation and high-temperature stability is the bottleneck to be broken through by the heat-insulating material for the microwave kiln. At present, corundum-mullite light bricks and mullite heat insulation cotton are commonly used as heat insulation materials, and although corundum-mullite has good high-temperature strength and thermal shock resistance, the dielectric loss of corundum-mullite is still high, and the dielectric loss of corundum-mullite is increased rapidly along with the temperature rise, so that thermal runaway is easily generated in the heat insulation materials. In order to solve the above problems, the invention patent CN106747574A discloses a Si for microwave kiln 2 N 2 The O wave-transparent and heat-insulating integrated lining material and the preparation method thereof realize the synergistic improvement of wave-transparent and heat-insulating, but Si 2 N 2 The preparation conditions of the O material are harsh, and the high-temperature stability is still all in short. Since the insulation material is in an air atmosphere during use, the oxide material system is still preferred. Magnesium oxide is a common refractory material, has low dielectric loss and does not change obviously with the temperature rise, but the product is difficult to sinter, and the magnesium oxide has high thermal expansion coefficient and poor high-temperature volume stability.
Therefore, how to provide a microwave thermal insulation material of an oxide material system, so that the microwave thermal insulation material has higher thermal insulation performance and high-temperature stability, and simultaneously satisfies excellent wave permeability is a bottleneck to be urgently broken through in the field.
Disclosure of Invention
In view of the above, the invention provides a preparation method of high-entropy ceramic for a microwave kiln, and the high-entropy ceramic prepared by the invention has high heat insulation performance, excellent wave-transmitting performance and high-temperature stability when being used as a heat insulation material for the microwave kiln.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-entropy ceramics for a microwave kiln comprises the following specific preparation steps:
1) Mixing MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 Mixing, adding absolute ethyl alcohol, dissolving, ball-milling and drying to obtain mixed powder;
2) And (2) pressing, molding and calcining the mixed powder obtained in the step 1) to obtain the high-entropy ceramic for the microwave kiln.
Preferably, mgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 The molar ratio of 16.
Preferably, the mass of anhydrous ethanol is related to MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 The molar ratio of the total amount is 400-800 (g): 1 (mol).
Preferably, the ball milling time is 2 to 5 hours, and the ball milling rotating speed is 100 to 300r/min.
Preferably, the drying temperature is 50-70 ℃, and the drying time is 12-14 h.
Preferably, the pressing pressure is 10-30MPa, and the pressing time is 1-5min.
Preferably, the calcining temperature is 800-1200 ℃, and the calcining time is 3-8 h.
Preferably, the calcining atmosphere in step 2) is an air atmosphere.
The invention also aims to provide the high-entropy ceramic prepared by the preparation method for the high-entropy ceramic for the microwave kiln.
The invention further aims to provide application of the high-entropy ceramic in microwave thermal insulation materials.
The invention selects (Mg) with a common magnesium oxide lattice structure 16 Ni 1 Co 1 Cu 1 Zn 1 )O 20 For research objects, metal chloride is used as a high-entropy ceramic precursor, and after compression molding, the chloride is promoted to be converted into oxide by calcining in the air atmosphere, and pores with different pore diameters are left in a matrix, so that the high-porosity high-entropy ceramic is obtained. By optimizing the preparation modeThe material structure is regulated and controlled, and the synergistic improvement of wave transmission, heat insulation and high-temperature stability is realized.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the sintering of the high-entropy ceramic and the formation of pores are carried out simultaneously, the preparation process is simplified, and chloride is directly pyrolyzed into oxide and is easy to sinter. Meanwhile, the obtained high-entropy ceramic has excellent wave-transmitting, heat-preserving and high-temperature stability;
the high-entropy ceramic prepared by the invention is an oxide, and has stable phase and structure at the temperature of less than 1200 ℃. The porosity is 30-60%, the thermal conductivity is 0.5-1.0W/(mK), and the microwave transmittance at 2.45GHz is more than 95%;
the invention can provide a new idea for the design and preparation of the heat insulation material for the microwave kiln.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a diagram of in-situ high temperature XRD pattern of the high entropy ceramic of example 1;
FIG. 2 is an SEM photograph of a high-entropy ceramic of example 1;
FIG. 3 is a profile diagram of the high-entropy ceramic of example 1 during a high-temperature stability test.
Detailed Description
The invention provides a preparation method of high-entropy ceramics for a microwave kiln, which comprises the following specific operation steps:
1) Mixing MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 Mixing, adding absolute ethyl alcohol, dissolving, ball-milling, and drying to obtain mixed powder;
2) And (2) pressing and molding the mixed powder obtained in the step 1), and calcining to obtain the high-entropy ceramic for the microwave kiln.
In the present invention, mgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 The preferred molar ratio is 16.
In the present invention, the mass of anhydrous ethanol and MgCl are added 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 The total molar ratio of (b) is 400 to 800 (g): 1 (mol), preferably 500 to 600, more preferably 500.
In the invention, the ball milling time is 2-5 h, and the ball milling speed is 100-300 r/min; preferably, the ball milling time is 2-4 h, and the ball milling rotating speed is 260-300 r/min; more preferably 3h, and the ball milling rotating speed is 300r/min.
In the invention, the drying temperature is 50-70 ℃, and the drying time is 12-14 h; preferably, the drying temperature is 55-65 ℃, and the drying time is 12-13 h; more preferably, the drying temperature is 60 ℃ and the drying time is 12 hours.
In the present invention, the pressing pressure is 10 to 30MPa and the pressing time is 1 to 5min, preferably 15MPa and 2min.
In the invention, the calcining temperature is 800-1200 ℃, and the calcining time is 3-8 h; preferably, the calcination temperature is 1000-1200 ℃, and the calcination time is 4-6 h; further preferably, the calcination temperature is 1200 ℃ and the calcination time is 5 hours.
In the present invention, the calcination atmosphere is preferably an air atmosphere.
The invention also provides the high-entropy ceramic prepared by the preparation method of the high-entropy ceramic for the microwave kiln.
The invention also provides application of the high-entropy ceramic in a microwave heat-insulating material.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The vector network analyzer used in the invention is an Agilent N5234A microwave network analyzer; the flat plate heat conduction instrument is a BPD-12-4P flat plate heat conduction instrument (Shanghai Shuichuan); the high temperature melting point tester is an LZ-3 high temperature melting point tester (university of northeast).
Example 1
Separately taking MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 1.6mol, 0.1mol and 0.1mol respectively, mixing the five materials, adding 1000g of absolute ethyl alcohol for dissolution, carrying out ball milling for 3 hours after dissolution at the rotating speed of 300r/min, and drying the uniformly mixed materials at the temperature of 60 ℃ for 12 hours to obtain mixed powder. And pressing the obtained powder for 2min under 15MPa, and calcining for 5h at 1200 ℃ in an air atmosphere to obtain the high-entropy ceramic. The in-situ high-temperature XRD pattern and the SEM pattern of the high-entropy ceramic prepared by the embodiment are shown in figure 1 and figure 2 respectively.
The wave-transmitting performance of the material at (2-18 GHz) is tested by using a vector network analyzer and adopting a coaxial line method, the thermal conductivity of the material is measured by adopting a flat plate thermal conductivity method, the porosity of the material is measured by adopting an Archimedes principle, and the high-temperature stability of the material is tested by adopting a high-temperature melting point tester. In the embodiment, the porosity of the high-entropy ceramic is about 42%, the thermal conductivity is 0.50W/(mK), the microwave transmittance at 2.45GHz is more than 98%, the volume of the material is stable and unchanged within 1200 ℃ (see figure 3), and the high-entropy ceramic has good high-temperature stability.
Example 2
Separately taking MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 1.6mol, 0.1mol and 0.1mol respectively, mixing the five materials, adding 1200g of absolute ethyl alcohol for dissolving, ball-milling for 4h after dissolving, rotating speed of 100r/min, and drying the uniformly mixed materials at 55 ℃ for 12h to obtain mixed powder. The obtained powder is processed under 12MPaPressing for 2min, and calcining for 3h at 1200 ℃ in air atmosphere to obtain the high-entropy ceramic.
The test method of the embodiment is the same as the test method of the embodiment 1, and the porosity of the high-entropy ceramic is measured to be about 35%, the thermal conductivity is 0.72W/(mK), the microwave transmittance at 2.45GHz is more than 96%, the volume of the material is stable and unchanged within 1200 ℃, and the high-temperature stability is good.
Example 3
Separately taking MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 1.6mol, 0.1mol and 0.1mol respectively, mixing the five materials, adding 800g of absolute ethyl alcohol for dissolving, ball-milling for 2h after dissolving, rotating speed of 200r/min, and drying the uniformly mixed materials at 60 ℃ for 14h to obtain mixed powder. And pressing the obtained powder for 1min under 30MPa, and calcining for 6h at 800 ℃ in an air atmosphere to obtain the high-entropy ceramic.
The test method of the embodiment is the same as the test method of the embodiment 1, and the porosity of the high-entropy ceramic is measured to be about 30%, the thermal conductivity is 1.0W/(mK), the microwave transmittance at 2.45GHz is more than 95%, the volume of the material is stable and unchanged within 1200 ℃, and the high-temperature stability is good.
Example 4
Separately taking MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 1.6mol, 0.1mol and 0.1mol respectively, mixing the five materials, adding 1000g of absolute ethyl alcohol for dissolving, ball-milling for 5h after dissolving, rotating speed of 300r/min, and drying the uniformly mixed materials at 70 ℃ for 13h to obtain mixed powder. And pressing the obtained powder under 10MPa for 4min, and calcining at 900 ℃ for 8h in an air atmosphere to obtain the high-entropy ceramic.
The test method of the embodiment is the same as the test method of the embodiment 1, and the porosity of the high-entropy ceramic is measured to be about 52%, the thermal conductivity is 0.80W/(mK), the microwave transmittance of 2.45GHz is greater than 95%, the volume of the material is stable within 1200 ℃, and the high-temperature stability is good.
Example 5
Separately taking MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 1.6mol, 0.1mol and 0.1mol respectively, mixing the five materials, adding 1600g of absolute ethyl alcohol for dissolution, ball-milling for 3h after dissolution at the rotating speed of 300r/min, and drying the uniformly mixed materials at the temperature of 50 ℃ for 12h to obtain mixed powder. And pressing the obtained powder for 5min under 12MPa, and calcining for 7h at 1200 ℃ in an air atmosphere to obtain the high-entropy ceramic.
The test method of the embodiment is the same as the test method of the embodiment 1, and the porosity of the high-entropy ceramic is measured to be about 60%, the thermal conductivity is 0.76W/(mK), the microwave transmittance of 2.45GHz is more than 97%, the volume of the material is stable within 1200 ℃, and the high-temperature stability is good.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of high-entropy ceramics for a microwave kiln is characterized by comprising the following specific preparation steps:
1) Mixing MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 Mixing, adding absolute ethyl alcohol, dissolving, ball grinding,then drying to obtain mixed powder;
2) Pressing and molding the mixed powder obtained in the step 1), and calcining to obtain the high-entropy ceramic for the microwave kiln;
MgCl 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 o and ZnCl 2 The molar ratio of 16;
the calcining atmosphere in the step 2) is air atmosphere.
2. The method for preparing high-entropy ceramics for microwave kilns as claimed in claim 1, wherein the mass of anhydrous ethanol and MgCl are added 2 ·6H 2 O、CoCl 2 ·6H 2 O、CuCl 2 ·2H 2 O、NiCl 2 ·6H 2 O and ZnCl 2 The molar ratio of the total amount is 400-800g.
3. The preparation method of the high-entropy ceramic for the microwave kiln according to any one of claims 1 to 2, wherein the ball milling time is 2 to 5 hours, and the ball milling rotation speed is 100 to 300r/min.
4. The preparation method of the high-entropy ceramic for the microwave kiln, according to claim 3, is characterized in that the drying temperature is 50-70 ℃, and the drying time is 12-14 h.
5. A preparation method of high-entropy ceramic for a microwave kiln according to any one of claims 1 to 2 and 4, wherein the pressing pressure is 10-30MPa, and the pressing time is 1-5min.
6. The preparation method of the high-entropy ceramic for the microwave kiln as claimed in claim 5, wherein the calcination temperature is 800-1200 ℃ and the calcination time is 3-8 h.
7. The high-entropy ceramic prepared by the method for preparing the high-entropy ceramic for the microwave kiln as claimed in any one of claims 1 to 6.
8. The use of the high-entropy ceramic of claim 7 in microwave insulation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019701A (en) * | 2018-07-23 | 2018-12-18 | 安徽工业大学 | A kind of preparation method of rock salt (MgCoCuNiZn) O high entropy oxide powder material |
| CN110204328A (en) * | 2019-06-05 | 2019-09-06 | 西南交通大学 | A kind of preparation method of high entropy oxide ceramics |
| CN110818430A (en) * | 2019-11-12 | 2020-02-21 | 西安交通大学 | Uniform high-entropy oxide ceramic submicron spherical powder and preparation method thereof |
| CN110903084A (en) * | 2019-11-12 | 2020-03-24 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20020159914A1 (en) * | 2000-11-07 | 2002-10-31 | Jien-Wei Yeh | High-entropy multielement alloys |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019701A (en) * | 2018-07-23 | 2018-12-18 | 安徽工业大学 | A kind of preparation method of rock salt (MgCoCuNiZn) O high entropy oxide powder material |
| CN110204328A (en) * | 2019-06-05 | 2019-09-06 | 西南交通大学 | A kind of preparation method of high entropy oxide ceramics |
| CN110818430A (en) * | 2019-11-12 | 2020-02-21 | 西安交通大学 | Uniform high-entropy oxide ceramic submicron spherical powder and preparation method thereof |
| CN110903084A (en) * | 2019-11-12 | 2020-03-24 | 西安交通大学 | High-entropy oxide submicron powder and preparation method thereof |
Non-Patent Citations (1)
| 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 Socity》;20180915;第102卷(第4期);第2228-2237页 * |
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