CN115504501B - Microwave heating element zinc oxide and preparation method and application thereof - Google Patents

Microwave heating element zinc oxide and preparation method and application thereof Download PDF

Info

Publication number
CN115504501B
CN115504501B CN202110694488.2A CN202110694488A CN115504501B CN 115504501 B CN115504501 B CN 115504501B CN 202110694488 A CN202110694488 A CN 202110694488A CN 115504501 B CN115504501 B CN 115504501B
Authority
CN
China
Prior art keywords
zinc oxide
microwave
microwave heating
zinc
heating element
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
Application number
CN202110694488.2A
Other languages
Chinese (zh)
Other versions
CN115504501A (en
Inventor
马望京
赵濉
赵俊
张路
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Technical Institute of Physics and Chemistry of CAS
Original Assignee
Technical Institute of Physics and Chemistry of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Technical Institute of Physics and Chemistry of CAS filed Critical Technical Institute of Physics and Chemistry of CAS
Priority to CN202110694488.2A priority Critical patent/CN115504501B/en
Publication of CN115504501A publication Critical patent/CN115504501A/en
Application granted granted Critical
Publication of CN115504501B publication Critical patent/CN115504501B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453Shaped 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/45Aggregated particles or particles with an intergrown morphology
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

A zinc oxide of a microwave heating element, which has a bar-shaped and sheet-shaped micro-nano structure. The structure endows multiple interfaces of zinc oxide, thereby being more beneficial to realizing impedance matching and microwave absorption and heat conversion, being capable of rapidly absorbing and converting heat energy under the radiation of 2.45GHz microwave frequency, and being capable of heating to 300-1200 ℃ for 15-180 seconds.

Description

Microwave heating element zinc oxide and preparation method and application thereof
Technical Field
The application belongs to the field of wave-absorbing materials, and particularly relates to a microwave heating element zinc oxide and a preparation method and application thereof.
Background
With the rapid development of electronic devices, electromagnetic radiation in use brings about potential damage to the performance of peripheral devices, human health and the surrounding environment, and in recent years, a wave absorbing material is a medium with excellent electromagnetic wave storage and loss properties, which can capture incident electromagnetic wave energy inside the material and convert it into heat energy or other forms of energy through dielectric loss and magnetic loss mechanisms. (In Situ Synthesis of Hierarchical Rose-Like ports Fe@C with Enhanced Electromagnetic Wave absorption.J. Mater. Chem. C2018,6 (3), 558-567.)
Zinc oxide is a multifunctional material with unique physical and chemical properties, such as high chemical stability, high electrochemical coupling coefficient, wide radiation absorption range and high light stability; in the field of material science, zinc oxide is classified as an important semiconductor material due to its wide band gap and high bond energy; the excellent hardness, rigidity and piezoelectric constant of the material make the material an important material in the ceramic industry; its low toxicity, biocompatibility and biodegradability make it an important material in biomedical and ecological systems. (A comprehensive review of ZnO materials and devices J.appl.Phys.2005, 98.)
For the microwave absorbing material, the micro morphology and the size of the microwave absorber have great influence on the microwave attenuation capability, and the microwave absorption performance represented by different micro morphologies of the same material is often quite different, so that zinc oxide is favorable for realizing impedance matching and generating interface polarization due to various 1D, 2D and 3D structures, and finally microwave energy is dissipated in a thermal form, thereby realizing the microwave dissipation characteristic and making zinc oxide an important wave absorbing material. (Zinc Oxide-From Synthesis to Application: A reviews. Materials,7 (4), 2833-2881.)
Klofac synthesizes rod-shaped zinc oxide by using zinc acetate dihydrate, ammonia water, polyethylene glycol and hexadecyl trimethyl ammonium bromide under microwave radiation, and synthesizes petal-shaped zinc oxide by adjusting a surfactant; the Phura's has successfully synthesized petaloid ZnO with planar pyramids and hexagonal tips using zinc nitrate hexahydrate, hexamethyl tetrazate, sodium hydroxide under microwave radiation (Preparation of Flower-Like ZnO Microparticles by Microwave Assisted Synthesis; nanocon: brno, czech, 2012; controlling morphologies and growth mechanism of hexagonal prisms with planar and pyramid tips of ZnO microflowers by microwave radation. Ceramics International,40 (7), 9069-9076).
However, the synthesis process of the zinc oxide is usually realized by using a surfactant as an auxiliary agent under high pressure, and in addition, the synthesized zinc oxide often generates absorption in a high-frequency band, but does not have absorption in a 2.45GHz band used in the fields of industry, science and medical science, so that the application of the zinc oxide in the related fields is limited.
Disclosure of Invention
A first object of the present application is to provide a microwave heating element zinc oxide.
The second object of the application is to provide a method for preparing zinc oxide by a microwave heating element.
The third object of the application is to provide an application of the zinc oxide of the microwave heating element.
In order to achieve the above purpose, the application adopts the following technical scheme:
a zinc oxide of a microwave heating element, which has a bar-shaped and sheet-shaped micro-nano structure.
According to the application, the zinc oxide is formed by being supported on a carbon material;
according to the present application, the zinc oxide is obtained by forming a zinc oxide supported on a carbon material and removing the carbon material.
According to the application, the zinc oxide is formed by dehydrating zinc hydroxide on a carbon material;
according to the application, the zinc oxide is obtained by dehydrating zinc hydroxide on a carbon material and then calcining to remove the carbon material.
According to the application, the bar-shaped and sheet-shaped micro-nano structures form a single crystal cluster, and the crystal clusters form a micro-structure;
according to the application, the crystal clusters corresponding to the rod-shaped zinc oxide form a radial micron structure, and the crystal clusters corresponding to the flaky zinc oxide form a flower-shaped micron structure;
in one embodiment of the application, the zinc oxide nanorods have a width of 0.1-3um and a length of 1-10um.
In one embodiment of the application, the zinc oxide nanoplatelets have a thickness of 100 to 500nm and a width of 0.1 to 1um.
In one embodiment of the present application, the microwave heating element zinc oxide has an XRD pattern as shown in fig. 1.
In one embodiment of the present application, the microwave heating element zinc oxide has an SEM image as shown in fig. 3 or 5.
According to the application, the temperature of the zinc oxide of the microwave heating element is raised to 300-1200 ℃ in 15-180 seconds under the radiation of 2.45GHz microwave frequency.
The application also provides a preparation method of the microwave heating element zinc oxide, which comprises the following steps:
1) Mixing zinc salt solution with ammonia water, reacting, and mixing with carbon material to obtain dispersion;
2) Heating the dispersion liquid under microwave, and separating to obtain solid substances;
3) Calcining the solid substance obtained in the step 2) to obtain the microwave heating element zinc oxide.
According to the application, in step 1), the zinc salt in the zinc salt solution is zinc acetate, zinc chloride, zinc nitrate, etc., for example zinc acetate dihydrate is dissolved in a solvent.
Preferably, the mass ratio of the zinc salt to the solvent is 1 (1-200); preferably 1 (25-150), more preferably 1: (30-100), for example: 1:20, 1:30, 1:40.
Preferably, the mass ratio of the ammonia water to the solvent is 1 (1-200); preferably 1 (20-150), more preferably 1: (50-100), for example: 1:25, 1:30, 1:100.
Preferably, the mass ratio of the carbon material to the zinc salt is 1 (1-200); preferably 1 (20-100), more preferably 1: (50-80), for example: 1:5, 1:20, 1:60.
Preferably, the solvent is water, such as deionized water;
preferably, the reaction of adding ammonia water and carbon material specifically includes: firstly adding ammonia water into zinc salt solution, stirring for 10min-10h at room temperature, adding carbon material, and stirring for 5min-10h at room temperature;
preferably, the carbon material is activated carbon, carbon black or carbon nanotubes;
according to the application, in step 2), the power of the microwaves is, for example, 400-700W, and the heating time is, for example, 1min-3h;
according to the application, the separation may be carried out by centrifugation, preferably by drying the solid material obtained after separation.
According to the application, in step 3), the calcination is preferably carried out at a temperature of 400 to 1000 ℃, for example 500 to 900 ℃, for a time of 1 to 10 hours, for example.
The application also provides the microwave heating element zinc oxide prepared by the method.
The application further provides application of the zinc oxide of the microwave heating element in microwave chemical synthesis, catalysis, medical treatment and ceramics.
The application further provides application of the microwave heating element zinc oxide in microwave heating.
Advantageous effects
1. The microwave heating element zinc oxide has a regular bar-shaped and sheet-shaped micro-nano structure, and the structure endows multiple interfaces of zinc oxide, thereby being more beneficial to realizing impedance matching and microwave absorption and heat conversion, being capable of rapidly absorbing and converting into heat energy under the radiation of 2.45GHz microwave frequency, and being capable of heating to 300-1200 ℃ for 15-180 seconds. The zinc oxide has the advantages of stable structure, long service cycle, rapid heating and the like.
2. The microwave heating element zinc oxide has simple preparation process, low cost and easy acquisition of raw materials, and is suitable for industrial production. The application adopts the microwave heating method to prepare the zinc oxide, when the microwave heating is carried out, water molecules can vibrate to accelerate the zinc oxide nucleation, and when the microwave reaction is carried out, the temperature of the carbon material is slightly higher than that of the water, thereby being beneficial to the growth of the zinc oxide on the surface of the carbon material.
3. According to the application, by changing the preparation conditions of zinc oxide, the microstructure of zinc oxide can be selectively regulated, so that a radial micron structure (such as a millet banana shape, a feather duster shape and the like) and a petal-shaped zinc oxide structure are obtained, the structure can capture incident electromagnetic waves in the structure and realize microwave thermal conversion through repeated reflection and loss in a short time, thereby realizing rapid heating under microwaves, and being applicable to the fields of microwave chemical synthesis, catalysis, medical treatment, ceramics and the like.
Drawings
Figure 1 shows the XRD pattern of the zinc oxide produced in example 1.
Fig. 2 shows SEM images of the zinc oxide of example 3 after drying and before calcination.
Fig. 3 shows SEM images of the zinc oxide of example 3 after calcination.
Fig. 4 shows SEM images of the zinc oxide prepared in example 10 after drying and before calcination.
Fig. 5 shows SEM images of the zinc oxide prepared in example 10 after calcination.
Fig. 6 shows a microwave heating profile of the zinc oxide prepared in example 2 at a microwave power of 700W for 80 seconds.
Fig. 7 shows a microwave heating profile of the zinc oxide prepared in example 7 at a microwave power of 700W for 20 seconds.
Detailed Description
The compounds of the general formula and the preparation method and application thereof according to the present application will be described in further detail with reference to the accompanying drawings and specific examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the application. All techniques implemented based on the above description of the application are intended to be included within the scope of the application.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 10g of zinc acetate dihydrate was dissolved in 250mL of deionized water and stirred at 1500 rpm for 1h at room temperature to form solution S1;
2) Dropwise adding 6mL of ammonia water into the solution S1, and stirring at the speed of 1500 rpm for 1h at room temperature to obtain a zinc hydroxide solution, namely solution S2;
3) 0.2g of activated carbon powder is added into the solution S2 and stirred at the room temperature for 1h at the speed of 1500 revolutions per minute to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 120min under the power of 500W to obtain zinc oxide covered on active carbon, naturally cooling to room temperature, filtering, washing powder to neutrality by deionized water, drying the obtained sample in an oven at 80 ℃ for 3h, and calcining in a muffle furnace at 500 ℃ for 2h to obtain the zinc oxide.
Referring to fig. 1, the XRD pattern of the zinc oxide prepared in this example shows that the crystal structure of the zinc oxide prepared in this example is regular, and no peaks of the crystalline forms of the carbon material and zinc hydroxide are seen, indicating that the obtained zinc oxide is relatively pure.
Example 2
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 10g of zinc acetate dihydrate was dissolved in 300mL of deionized water and stirred at 1500 rpm for 3 hours at room temperature to form solution S1;
2) 10mL of ammonia water is dripped into the solution S1 and stirred at the speed of 1500 rpm for 2h under the condition of room temperature to form a solution S2;
3) 0.1g of activated carbon powder is added into the solution S2 and stirred at the room temperature for 1h at the speed of 1500 revolutions per minute to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 110min under 500W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 3h, and calcining in a muffle furnace at 500 ℃ for 2h to obtain the final product.
FIG. 6 is a graph showing the microwave heating of 80 seconds of the microwave heating element zinc oxide prepared in this example at a microwave power of 700W, at a temperature of 600 ℃.
Example 3
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 12g of zinc acetate dihydrate was dissolved in 250mL of deionized water and stirred at 2500 rpm for 1h at room temperature to form solution S1;
2) 10mL of ammonia water is dripped into the solution S1 and stirred at the speed of 2500 rpm for 1h under the condition of room temperature to form a solution S2;
3) 0.2g of activated carbon powder is added into the solution S2 and stirred at the room temperature for 1h at the speed of 2500 rpm to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 70min under 550W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 4h, and calcining in a muffle furnace at 550 ℃ for 3h to obtain the final product.
Referring to fig. 2, an SEM image of the sample prepared in this example before calcination after drying in an oven for 4 hours, in which case the zinc oxide has unremoved activated carbon, and the activated carbon is distributed on the surface and gaps of the zinc oxide.
Referring to fig. 3, in the SEM image of the microwave heating element zinc oxide obtained after calcination in this example (different positions are selected to be photographed to show different micro-nano structures), it can be seen that there are three different structures of the microwave heating element zinc oxide from which activated carbon is removed at high temperature, because there are differences in nucleation and growth rates of zinc oxide under different reaction conditions.
After the zinc oxide of the microwave heating body obtained in the embodiment heats for half an hour in a microwave field, the microstructure of the zinc oxide does not change, and is the same as that of the original zinc oxide, so that the zinc oxide has a stable structure when being used for microwave heating.
Example 4
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 15g of zinc acetate dihydrate was dissolved in 600mL of deionized water and stirred at 2000 rpm for 1h at room temperature to form solution S1;
2) 15mL of ammonia water is dripped into the solution S1 and stirred at the speed of 2000 rpm for 4 hours under the condition of room temperature to form a solution S2;
3) 0.5g of activated carbon powder is added into the solution S2 and stirred for 4 hours at the speed of 2000 rpm under the condition of room temperature to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 30min under 700W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 4h, and calcining in a muffle furnace at 550 ℃ for 3h to obtain the nano-particle.
Example 5
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 15g of zinc acetate dihydrate was dissolved in 500mL of deionized water and stirred at 2000 rpm for 3 hours at room temperature to form solution S1;
2) 15mL of ammonia water is dripped into the solution S1 and stirred at the speed of 2000 rpm for 2 hours under the condition of room temperature to form a solution S2;
3) Adding 0.75g of activated carbon powder into the solution S2 and stirring at a speed of 2000 rpm for 20min at room temperature to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 25min under 700W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 4h, and calcining in a muffle furnace at 800 ℃ for 4h to obtain the nano-particle.
Example 6
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 18g of zinc acetate dihydrate was dissolved in 900mL of deionized water and stirred at 1800 rpm for 3 hours at room temperature to form solution S1;
2) 26mL of ammonia water is dropwise added to the solution S1 and stirred at a speed of 1800 revolutions per minute for 3 hours at room temperature to form a solution S2;
3) Adding 0.7g of activated carbon powder into the solution S2 and stirring at a speed of 2000 rpm for 20min at room temperature to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 25min under 700W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 4h, and calcining in a muffle furnace at 800 ℃ for 4h to obtain the nano-particle.
Example 7
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 12g of zinc acetate dihydrate was dissolved in 1000mL of deionized water and stirred at 2800 revolutions per minute for 6 hours at room temperature to form solution S1;
2) 20mL of ammonia water was added dropwise to the S1 solution and stirred at 2800 rpm for 6h at room temperature to form a solution S2;
3) Adding 5g of activated carbon powder into the solution S2 and stirring at the speed of 2800 revolutions per minute for 2 hours at room temperature to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven, heating for 100min under 600W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 7h, and calcining in a muffle furnace at 900 ℃ for 4h to obtain the nano-particle.
Referring to FIG. 7, a microwave heating graph of the microwave heating element zinc oxide prepared in the present example is set at 700W microwave power for 20 seconds, and the temperature is greater than 880 ℃.
Example 8
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 12g of zinc acetate dihydrate was dissolved in 1050mL of deionized water and stirred at 2500 rpm for 6h at room temperature to form solution S1;
2) Dropwise adding 20mL of ammonia water into the solution S1 and stirring at the speed of 2500 rpm for 6h at room temperature to form a solution S2;
3) Adding 4.5g of activated carbon powder into the solution S2 and stirring at the room temperature for 2 hours at the speed of 2500 rpm to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven, heating for 150min under 900W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 7h, and calcining in a muffle furnace at 900 ℃ for 4h to obtain the final product.
Example 9
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 10g of zinc acetate dihydrate was dissolved in 1000mL of deionized water and stirred at 2300 rpm for 4 hours at room temperature to form solution S1;
2) Dropwise adding 10mL of ammonia water into the solution S1 and stirring at the speed of 2300 rpm for 2 hours at room temperature to form a solution S2;
3) 0.5g of activated carbon powder is added into the solution S2 and stirred at the room temperature for 2 hours at the speed of 2300 revolutions per minute to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven, heating for 135min under 600W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 2h, and calcining in a muffle furnace at 900 ℃ for 3h to obtain the final product.
Example 10
The preparation method of the microwave heating element zinc oxide comprises the following steps:
1) 10g of zinc acetate dihydrate was dissolved in 700mL of deionized water and stirred at 2500 rpm for 2 hours at room temperature to form solution S1;
2) 8mL of ammonia water is added into the solution S1 in a dropwise manner and stirred at the speed of 2500 rpm for 2 hours under the condition of room temperature, so as to form a solution S2;
3) 1g of activated carbon powder is added into the solution S2 and stirred at the room temperature for 1h at the speed of 2500 rpm to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven and heating for 100min under 650W power, naturally cooling to room temperature, filtering, washing the powder to neutrality with deionized water, drying the obtained sample in an oven at 80 ℃ for 2h, and calcining in a muffle furnace at 900 ℃ for 2h to obtain the product.
Referring to fig. 4, an SEM image of the sample prepared in this example before calcination after drying in an oven for 2 hours, in which case the zinc oxide has unremoved activated carbon, and the activated carbon is distributed on the surface and gaps of the zinc oxide.
Referring to fig. 5, which is an SEM image of the microwave heating element zinc oxide obtained after calcination in this example, it can be seen that the microwave heating element zinc oxide from which activated carbon is removed at a high temperature has a regular and uniform rod-like structure, indicating that the initially formed nuclei are relatively uniform and the growth rate is also substantially uniform.
After the zinc oxide of the microwave heating body obtained in the embodiment heats for half an hour in a microwave field, the microstructure of the zinc oxide does not change, and is the same as that of the original zinc oxide, so that the zinc oxide has a stable structure when being used for microwave heating.
The embodiments of the present application have been described above. However, the present application is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (12)

1. The zinc oxide of the microwave heating body is characterized by having a bar-shaped or sheet-shaped micro-nano structure;
the preparation method of the zinc oxide of the microwave heating body comprises the following steps:
1) Mixing zinc salt solution with ammonia water, reacting, and mixing with carbon material to obtain dispersion;
2) Heating the dispersion liquid under microwave, and separating to obtain solid substances;
3) Calcining the solid substance obtained in the step 2) to obtain the zinc oxide of the microwave heating element;
the carbon material is activated carbon, carbon black or carbon nano tube;
the micro-nano structure forms a single crystal cluster, and the crystal cluster forms a micro-structure; the crystal clusters corresponding to the rod-shaped zinc oxide form a radial micron structure, and the crystal clusters corresponding to the sheet-shaped zinc oxide form a flower-shaped micron structure.
2. A microwave heating body zinc oxide according to claim 1, wherein the rod-shaped zinc oxide has a width of 0.1 to 3 μm and a length of 1 to 10. Mu.m; the thickness of the flaky zinc oxide is 100-500nm, and the width is 0.1-1 mu m.
3. A microwave applicator zinc oxide according to any one of claims 1 to 2, wherein the microwave applicator zinc oxide is heated to 300 to 1200 ℃ for 15 to 180 seconds under microwave frequency radiation at 2.45 GHz.
4. A method for preparing the microwave heating element zinc oxide according to any one of claims 1 to 3, comprising the steps of:
1) Mixing zinc salt solution with ammonia water, reacting, and mixing with carbon material to obtain dispersion;
2) Heating the dispersion liquid under microwave, and separating to obtain solid substances;
3) Calcining the solid substance obtained in the step 2) to obtain the zinc oxide of the microwave heating element;
the carbon material is activated carbon, carbon black or carbon nano tube, and the mass ratio of the carbon material to zinc salt is 1 (1-200).
5. The method of preparing zinc oxide as claimed in claim 4, wherein in step 1), the zinc salt in the zinc salt solution is zinc acetate, zinc chloride or zinc nitrate.
6. The method for preparing zinc oxide as claimed in claim 4, wherein the mass ratio of the carbon material to zinc salt is 1: (5-100).
7. The method for preparing zinc oxide as claimed in any one of claims 4 to 6, wherein mixing zinc salt solution with ammonia water, reacting, and mixing with carbon material comprises: ammonia water is added into zinc salt solution, stirred for 10min-10h at room temperature, then carbon material is added, and stirred for 5min-10h at room temperature.
8. The method for preparing zinc oxide as claimed in any one of claims 4 to 6, wherein in the step 2), the power of the microwave is 400 to 700W, and the heating time is 1min to 3h.
9. A method for producing a microwave heating body zinc oxide according to any one of claims 4 to 6, wherein the separation is centrifugal separation.
10. The method for producing a microwave heating body zinc oxide according to any one of claims 4 to 6, wherein in step 3), the calcination temperature is 400 to 1000 ℃ and the calcination time is 1 to 10 hours.
11. The use of a microwave heating element zinc oxide according to any one of claims 1 to 3, characterized in that it is used in microwave chemical synthesis, catalysis, medical treatment, ceramics.
12. The use of a microwave heating element zinc oxide according to any one of claims 1 to 3, characterized in that it is used for microwave heating.
CN202110694488.2A 2021-06-22 2021-06-22 Microwave heating element zinc oxide and preparation method and application thereof Active CN115504501B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110694488.2A CN115504501B (en) 2021-06-22 2021-06-22 Microwave heating element zinc oxide and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110694488.2A CN115504501B (en) 2021-06-22 2021-06-22 Microwave heating element zinc oxide and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN115504501A CN115504501A (en) 2022-12-23
CN115504501B true CN115504501B (en) 2023-10-24

Family

ID=84499918

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110694488.2A Active CN115504501B (en) 2021-06-22 2021-06-22 Microwave heating element zinc oxide and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN115504501B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101941731A (en) * 2010-08-20 2011-01-12 桂林电子科技大学 Preparation method of void type nano-sheet zinc oxide and activated carbon load complex
CN102303896A (en) * 2011-05-25 2012-01-04 云南大学 Method for preparing zinc oxide with hollow flower-like micrometer structure
CN107059124A (en) * 2017-03-31 2017-08-18 中原工学院 A kind of method that utilization microwave synthesizes zinc oxide in large size crystal
CN108002423A (en) * 2017-12-19 2018-05-08 云南锡业职业技术学院 The method that a kind of ultrasonic wave and microwave cooperating prepare nano zine oxide
CN108698849A (en) * 2015-12-21 2018-10-23 罗马大学 Pass through the production of the graphene-based composite nanostructure of non-loading type graphene nano on piece growing zinc oxide nanorod or the micron bar acquisition in suspension
CN110357144A (en) * 2019-08-23 2019-10-22 中国科学院兰州化学物理研究所 One type flower shape zinc oxide/ferroso-ferric oxide wave absorbing agent and preparation method thereof and absorbing material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101941731A (en) * 2010-08-20 2011-01-12 桂林电子科技大学 Preparation method of void type nano-sheet zinc oxide and activated carbon load complex
CN102303896A (en) * 2011-05-25 2012-01-04 云南大学 Method for preparing zinc oxide with hollow flower-like micrometer structure
CN108698849A (en) * 2015-12-21 2018-10-23 罗马大学 Pass through the production of the graphene-based composite nanostructure of non-loading type graphene nano on piece growing zinc oxide nanorod or the micron bar acquisition in suspension
CN107059124A (en) * 2017-03-31 2017-08-18 中原工学院 A kind of method that utilization microwave synthesizes zinc oxide in large size crystal
CN108002423A (en) * 2017-12-19 2018-05-08 云南锡业职业技术学院 The method that a kind of ultrasonic wave and microwave cooperating prepare nano zine oxide
CN110357144A (en) * 2019-08-23 2019-10-22 中国科学院兰州化学物理研究所 One type flower shape zinc oxide/ferroso-ferric oxide wave absorbing agent and preparation method thereof and absorbing material

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
四针状氧化锌晶须的性能及应用;刘红;高翠翠;罗小春;;广州化工(第07期);第8-10页 *
微波固相合成氧化锌纳米棒;刘劲松;曹洁明;李子全;柯行飞;;化学学报(第15期);第1476-1480页 *
微波煅烧制备纳米氧化锌;曹俊, 周继承, 吴建懿;无机盐工业(第05期);第31-33页 *

Also Published As

Publication number Publication date
CN115504501A (en) 2022-12-23

Similar Documents

Publication Publication Date Title
Wang et al. Biomass carbon derived from pine nut shells decorated with NiO nanoflakes for enhanced microwave absorption properties
Xia et al. Microwave absorption enhancement and electron microscopy characterization of BaTiO 3 nano-torus
Hu et al. Selective preparation and enhanced microwave electromagnetic characteristics of polymorphous ZnO architectures made from a facile one-step ethanediamine-assisted hydrothermal approach
CN108655411B (en) Preparation method of wave-absorbing material and wave-absorbing coating
Wu et al. Synthesis and characterization of superfine magnesium hydroxide with monodispersity
CN103274396A (en) Preparation method of grapheme and ferriferrous oxide composite nanometer material
Tang et al. Preparation and characterization of cordierite powders by water-based sol-gel method
CN115504501B (en) Microwave heating element zinc oxide and preparation method and application thereof
El-Rafei et al. Effect of alkali concentration and reaction time on the morphology of ZnO nano-microparticles prepared by hydrothermal method
Eftekhari et al. Fabrication and microstructural characterization of the novel optical ceramic consisting of α-Al2O3@ amorphous alumina nanocomposite core/shell structure
CN102408231B (en) Preparation method of hollow Ni-Zn ferrite microsphere
Xiang et al. Effect of process factors on properties of high dispersion spherical α-Al2O3 particles prepared by hydrothermal method
Abdulghani et al. Preparation and characterization of yttrium oxide nanoparticles at different calcination temperatures from yttrium hydroxide prepared by hydrothermal and hydrothermal microwave methods
Li et al. Controlled synthesis of α-Al2O3 via the hydrothermal-pyrolysis method
Li et al. Microwave idrothermal synthesis of magnesium-aluminium spinel
CN108640145B (en) Preparation method of flower-ball-shaped yttrium oxide nano material with controllable appearance
Zheng et al. Preparation of Ce2Fe17N3–δ@ FePO4 composite with excellent microwave absorption performance by reduction-diffusion (R/D) and phosphating processes
Dulina et al. Effects of phase and chemical composition of precursor on structural and morphological properties of (Lu0. 95Eu0. 05) 2O3 nanopowders
KR101994428B1 (en) Method of preparing graphene-magnetic particle composite
Monin et al. Features of phase transitions upon the thermal treatment of Al 2 O 3 nanoparticles
Ebrahimi et al. Effects of high-energy ball milling on the microwave absorption properties of Sr0. 9Nd0. 1Fe12O19
Zhang et al. Anisotropic growth and photoluminescence of Li 2 Si 2 O 5 hydrate rods
Kanagesan et al. Synthesis and magnetic properties of conventional and microwave calcined barium hexaferrite powder
CHEN et al. Microwave-assisted sol-gel synthesis of hydroxyapatite nanoparticles
CN110642280A (en) alpha-Al2O3Nanotube and method for preparing the same

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