CN115504501A - Microwave heating body zinc oxide and preparation method and application thereof - Google Patents
Microwave heating body zinc oxide and preparation method and application thereof Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 111
- 238000010438 heat treatment Methods 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims description 20
- 239000002086 nanomaterial Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 230000005855 radiation Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 238000001354 calcination Methods 0.000 claims description 25
- 239000003575 carbonaceous material Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 18
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 13
- 150000003751 zinc Chemical class 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims description 6
- 229940007718 zinc hydroxide Drugs 0.000 claims description 6
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000002073 nanorod Substances 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 description 21
- 229910021641 deionized water Inorganic materials 0.000 description 21
- 238000001035 drying Methods 0.000 description 14
- 239000000843 powder Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 238000001914 filtration Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 230000007935 neutral effect Effects 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 241000571645 Sabellastarte magnifica Species 0.000 description 1
- 244000062793 Sorghum vulgare Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 235000019713 millet Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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Abstract
A microwave heating body zinc oxide is provided, and the zinc oxide has a rod-shaped and sheet-shaped micro-nano structure. The structure endows zinc oxide with multiple interfaces, thereby being more beneficial to realizing impedance matching and microwave absorption and heat conversion, being capable of rapidly absorbing and converting the zinc oxide into heat energy under the radiation of 2.45GHz microwave frequency, and being capable of heating to 300-1200 ℃ within 15-180 seconds.
Description
Technical Field
The invention belongs to the field of wave-absorbing materials, and particularly relates to a microwave heating body zinc oxide and a preparation method and application thereof.
Background
With the rapid development of electronic devices, the potential hazards of electromagnetic radiation during use to the performance of peripheral devices, human health and the surrounding environment have attracted much attention in recent years, and wave-absorbing materials are a medium with excellent electromagnetic wave storage and loss performance, and can capture the incident electromagnetic wave energy inside the material and convert the energy into heat energy or other forms of energy through dielectric loss and magnetic loss mechanisms. (In Situ Synthesis of structural Rose-Like Porous Fe @ C with Enhanced electronic 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 make the material important in the ceramic industry; its low toxicity, biocompatibility and biodegradability make it an important material in biomedicine and ecosystem. (A comprehensive review of ZnO materials and devices. J. Appl. Phys.2005, 98.)
For microwave absorbing materials, the influence of the microscopic morphology and size of a microwave absorbing agent on the microwave attenuation capacity is large, the microwave absorbing performance represented by different microscopic morphologies of the same material is often different, zinc oxide has various 1D, 2D and 3D structures, so that impedance matching is favorably realized, interface polarization is generated, and finally microwave energy is dissipated in a heat mode, so that the microwave dissipation characteristic is realized, and the zinc oxide becomes an important absorbing material. (Zinc Oxide-From Synthesis to Application: A review. 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; phurugrat successfully synthesized petal-Like ZnO with planar pyramids and hexagonal pyramidal tips under Microwave irradiation using zinc nitrate hexahydrate, hexamethylenetetramine, sodium hydroxide (Preparation of Flower-Like ZnO microspheres by Microwave Assisted Synthesis; nanocon: brno, czech, 2012; control morphology and growth mechanism of hexagonal prisms with sodium and platinum coatings of ZnO microfluidics by Microwave irradiation, 40 (7), 9069-9076).
However, the synthesis process of the zinc oxide is usually realized under high pressure by using a surfactant as an auxiliary agent, and in addition, the synthesized zinc oxide is often absorbed in a high-frequency band, but does not absorb in a 2.45GHz band used in the industrial, scientific and medical fields, so that the application of the zinc oxide in the related fields is limited.
Disclosure of Invention
The first purpose of the invention is to provide a microwave heating element zinc oxide.
The second purpose of the invention is to provide a preparation method of the microwave heating element zinc oxide.
The third purpose of the invention is to provide the application of the microwave heating element zinc oxide.
In order to achieve the purpose, the invention adopts the following technical scheme:
a microwave heating body zinc oxide is provided, and the zinc oxide has a rod-shaped and sheet-shaped micro-nano structure.
According to the present invention, the zinc oxide is formed by being supported on a carbon material;
according to the present invention, the zinc oxide is supported on a carbon material, and the carbon material is removed to obtain the zinc oxide.
According to the invention, the zinc oxide is formed by dehydrating zinc hydroxide on a carbon material;
according to the present invention, the zinc oxide is obtained by dehydrating zinc hydroxide on a carbon material and then removing the carbon material by calcination.
According to the invention, the rod-shaped and sheet-shaped micro-nano structures form a single crystal cluster, and the crystal cluster forms a micron structure;
according to the invention, crystal clusters corresponding to the rodlike zinc oxide form a radial micron structure, and crystal clusters corresponding to the flaky zinc oxide form a flower-like micron structure;
in one embodiment of the present invention, the zinc oxide nanorods have a width of 0.1 to 3um and a length of 1 to 10um.
In one embodiment of the invention, the zinc oxide nanosheets are 100 to 500nm thick and 0.1 to 1um wide.
In one embodiment of the present invention, the microwave heating element zinc oxide has an XRD pattern as shown in fig. 1.
In one embodiment of the invention, the microwave heating element zinc oxide has an SEM image as shown in FIG. 3 or FIG. 5.
According to the invention, the temperature of the microwave heating body zinc oxide is raised to 300-1200 ℃ in 15-180 seconds under the radiation of 2.45GHz microwave frequency.
The invention also provides a preparation method of the microwave heating element zinc oxide, which comprises the following steps:
1) Mixing a zinc salt solution with ammonia water, reacting, and mixing with a carbon material to obtain a dispersion liquid;
2) Heating the dispersion liquid under microwave, and separating to obtain solid matters;
3) Calcining the solid matter obtained in the step 2) to obtain the microwave heating element zinc oxide.
According to the invention, 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.
Preferably, the mass ratio of the ammonia water to the solvent is 1 (1-200); preferably, it is 1 (20-150), more preferably, it is 1: (50-100), for example: 1.
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.
Preferably, the solvent is water, such as deionized water;
preferably, the adding of the ammonia water and the carbon material for reaction specifically comprises: firstly, adding ammonia water into a zinc salt solution, stirring at room temperature for 10min-10h, then adding a carbon material, and stirring at room temperature for 5min-10h;
preferably, the carbon material is activated carbon, carbon black or carbon nanotubes;
according to the invention, in the step 2), the power of the microwave is 400-700W, and the heating time is 1min-3h;
according to the invention, the separation can be performed by centrifugation, preferably by drying the solid material obtained after separation.
According to the invention, in step 3), the calcination is preferably carried out at a temperature of 400 to 1000 ℃, for example 500 to 900 ℃, for example for a time of 1 to 10 hours.
The invention also provides the microwave heating body zinc oxide prepared by the method.
The invention further provides the application of the microwave heating element zinc oxide in microwave chemical synthesis, catalysis, medical treatment and ceramics.
The invention further provides application of the microwave heating element zinc oxide in microwave heating.
Advantageous effects
1. The microwave heating body zinc oxide has a regular rod-shaped and sheet-shaped micro-nano structure, and the structure endows zinc oxide with multiple interfaces, so that impedance matching is realized, microwave absorption and heat conversion are facilitated, the zinc oxide can be rapidly absorbed and converted into heat energy under the radiation of 2.45GHz microwave frequency, and the temperature can be raised to 300-1200 ℃ within 15-180 seconds. The zinc oxide has the advantages of stable structure, long service cycle, rapid heating and the like.
2. The microwave heating body zinc oxide has simple preparation process, cheap and easily obtained raw materials, and is suitable for industrial production. This application adopts the microwave heating method to prepare zinc oxide, and when microwave heating, the hydrone can appear vibrating and accelerate the progress of zinc oxide nucleation to, at microwave reaction, the temperature of carbon material is a little higher than water, helps zinc oxide to grow on the surface of carbon material.
3. The invention can selectively regulate and control the microstructure of the zinc oxide by changing the preparation conditions of the zinc oxide, thereby obtaining a radial micron structure (millet shape, feather duster shape, and the like) and a petaloid zinc oxide structure, and the structure can capture the incident electromagnetic wave in the structure and realize microwave thermal conversion through multiple reflection and loss in a short time, thereby realizing rapid temperature rise under microwave, and can be used in the fields of microwave chemical synthesis, catalysis, medical treatment, ceramics, and the like.
Drawings
Figure 1 shows the XRD pattern of the zinc oxide prepared in example 1.
Fig. 2 shows an SEM image of the zinc oxide of example 3 after drying and before calcination.
Figure 3 shows an SEM image of the zinc oxide of example 3 after calcination.
Fig. 4 shows an SEM image of zinc oxide prepared in example 10 before calcination after baking.
Fig. 5 shows an SEM image of zinc oxide produced by example 10 after calcination.
Fig. 6 shows the microwave ignition profile of zinc oxide prepared in example 2 at 700W microwave power for 80 seconds.
Fig. 7 shows the microwave profile of the zinc oxide obtained in example 7 at 700W microwave power for 20 seconds.
Detailed Description
The compounds of the general formula and the preparation and use thereof according to the present invention 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 only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the techniques realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
The preparation method of the microwave heating body zinc oxide comprises the following steps:
1) Dissolving 10g of zinc acetate dihydrate into 250mL of deionized water, and stirring at the room temperature at the speed of 1500 rpm for 1h to form a solution S1;
2) Dripping 6mL of ammonia water into the S1 solution, and stirring at the room temperature at the speed of 1500 rpm for 1h to obtain a zinc hydroxide solution, namely a solution S2;
3) Adding 0.2g of activated carbon powder into the solution S2, and stirring at the room temperature at the speed of 1500 rpm for 1h to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 120min under the power of 500W to obtain zinc oxide covered on the activated carbon, filtering after the zinc oxide is naturally cooled to room temperature, washing the powder to be neutral by using 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, which is an XRD pattern of the zinc oxide prepared in this example, it can be seen that the zinc oxide prepared in this example has a regular crystal structure, and no crystal peaks 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 body zinc oxide comprises the following steps:
1) Dissolving 10g of zinc acetate dihydrate into 300mL of deionized water, and stirring at the room temperature at the speed of 1500 rpm for 3 hours to form a solution S1;
2) Adding 10mL of ammonia water into the S1 solution dropwise and stirring at the room temperature at the speed of 1500 rpm for 2 hours to form a solution S2;
3) Adding 0.1g of activated carbon powder into the solution S2, and stirring at the room temperature at the speed of 1500 rpm for 1 hour to form a dispersion S3;
4) Transferring the dispersion S3 into a microwave oven, heating for 110min under 500W, naturally cooling to room temperature, filtering, washing the powder with deionized water to neutrality, and (3) drying the obtained sample in an oven at 80 ℃ for 3h, and calcining the dried sample in a muffle furnace at 500 ℃ for 2h to obtain the catalyst.
FIG. 6 is a microwave heating chart of the microwave heating element zinc oxide prepared in this example, which is set at 600 ℃ for 80 seconds under 700W microwave power.
Example 3
The preparation method of the microwave heating body zinc oxide comprises the following steps:
1) Dissolving 12g of zinc acetate dihydrate into 250mL of deionized water, and stirring at the room temperature at the speed of 2500 rpm for 1h to form a solution S1;
2) Adding 10mL of ammonia water into the S1 solution dropwise and stirring at the room temperature at the speed of 2500 rpm for 1h to form a solution S2;
3) Adding 0.2g of activated carbon powder into the solution S2 and stirring at the room temperature for 1 hour at the speed of 2500 rpm to form a dispersion liquid S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 70min under 550W power, filtering after naturally cooling to room temperature, washing the powder to neutrality by using 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-composite material.
Referring to fig. 2, it is an SEM image of the sample prepared in this example before calcination after drying in an oven for 4h, when there is unremoved activated carbon in the zinc oxide, and the activated carbon is distributed on the surface and in the gaps of the zinc oxide.
Referring to fig. 3, SEM images (different positions are selected for shooting to show different micro-nano structures) of the microwave heating element zinc oxide obtained after calcination in this example show that there are three different structures of the microwave heating element zinc oxide with high-temperature activated carbon removed, because there are differences in nucleation and growth rates of zinc oxide under different reaction conditions.
After the microwave heating element zinc oxide obtained in the embodiment is heated in a microwave field for half an hour, the microstructure of the zinc oxide does not change, and is the same as the original microstructure, which shows that the zinc oxide has a stable structure when used for microwave heating.
Example 4
A preparation method of microwave heating body zinc oxide comprises the following steps:
1) Dissolving 15g of zinc acetate dihydrate into 600mL of deionized water, and stirring at the room temperature at the speed of 2000 rpm for 1h to form a solution S1;
2) Adding 15mL of ammonia water into the S1 solution dropwise and stirring at the room temperature at the speed of 2000 rpm for 4 hours to form a solution S2;
3) Adding 0.5g of activated carbon powder into the solution S2, and stirring for 4 hours at the room temperature at the speed of 2000 r/min to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 30min under the power of 700W, filtering after naturally cooling to room temperature, washing the powder to be neutral by using deionized water, drying the obtained sample in an oven at 80 ℃ for 4h, and calcining in a muffle at 550 ℃ for 3h to obtain the nano-composite material.
Example 5
A preparation method of microwave heating body zinc oxide comprises the following steps:
1) Dissolving 15g of zinc acetate dihydrate into 500mL of deionized water, and stirring for 3 hours at room temperature at a speed of 2000 rpm to form a solution S1;
2) Adding 15mL of ammonia water into the S1 solution dropwise and stirring the solution at room temperature at a speed of 2000 rpm for 2 hours to form a solution S2;
3) Adding 0.75g of activated carbon powder into the solution S2, and stirring at the room temperature at the speed of 2000 rpm for 20min to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 25min under the power of 700W, filtering after naturally cooling to room temperature, washing the powder to be neutral by using 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-composite material.
Example 6
A preparation method of microwave heating body zinc oxide comprises the following steps:
1) Dissolving 18g of zinc acetate dihydrate into 900mL of deionized water, and stirring at the room temperature at the speed of 1800 rpm for 3h to form a solution S1;
2) Adding 26mL of ammonia water into the S1 solution dropwise and stirring at the room temperature at a speed of 1800 rpm for 3 hours to form a solution S2;
3) Adding 0.7g of activated carbon powder into the solution S2, and stirring at the room temperature at the speed of 2000 r/min for 20min to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 25min under the power of 700W, filtering after naturally cooling to room temperature, washing the powder to be neutral by using 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-silver powder.
Example 7
A preparation method of microwave heating body zinc oxide comprises the following steps:
1) Dissolving 12g of zinc acetate dihydrate into 1000mL of deionized water, and stirring for 6h at 2800 rpm at room temperature to form a solution S1;
2) Adding 20mL of ammonia water into the S1 solution dropwise and stirring 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 2800 rpm for 2h at room temperature to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 100min under 600W power, filtering after naturally cooling to room temperature, washing the powder to neutrality by using 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-silver-based nano-silver powder.
Referring to FIG. 7, the microwave heating element prepared in this example, namely zinc oxide, was exposed to 700W microwave power for 20 seconds, and the temperature thereof was higher than 880 ℃.
Example 8
The preparation method of the microwave heating body zinc oxide comprises the following steps:
1) Dissolving 12g of zinc acetate dihydrate into 1050mL of deionized water, and stirring for 6 hours at the room temperature at the speed of 2500 rpm to form a solution S1;
2) Adding 20mL of ammonia water into the S1 solution dropwise and stirring for 6h at the room temperature at the speed of 2500 rpm 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 liquid S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 150min under 900W, naturally cooling to room temperature, filtering, washing the powder to neutrality by using 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-silver-based nano-silver powder.
Example 9
The preparation method of the microwave heating body zinc oxide comprises the following steps:
1) Dissolving 10g of zinc acetate dihydrate into 1000mL of deionized water, and stirring at room temperature at 2300 rpm for 4h to form a solution S1;
2) Adding 10mL of ammonia water into the S1 solution dropwise and stirring the solution at room temperature at the speed of 2300 revolutions per minute for 2 hours to form a solution S2;
3) Adding 0.5g of activated carbon powder into the solution S2, and stirring for 2 hours at room temperature at the speed of 2300 rpm to form a dispersion S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 135min under the power of 600W, filtering after naturally cooling to room temperature, washing the powder to be neutral by using 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 nano-composite material.
Example 10
A preparation method of microwave heating body zinc oxide comprises the following steps:
1) Dissolving 10g of zinc acetate dihydrate into 700mL of deionized water, and stirring for 2h at the room temperature at the speed of 2500 rpm to form a solution S1;
2) Adding 8mL of ammonia water into the S1 solution dropwise and stirring at the room temperature at the speed of 2500 rpm for 2 hours to form a solution S2;
3) Adding 1g of activated carbon powder into the solution S2, and stirring at the room temperature for 1 hour at the speed of 2500 rpm to form a dispersion liquid S3;
4) And transferring the dispersion liquid S3 into a microwave oven, heating for 100min under 650W power, filtering after naturally cooling to room temperature, washing the powder to neutrality by using 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 nano-silver-based nano-silver powder.
Referring to fig. 4, it is an SEM image of the sample prepared in this example before calcination after drying in an oven for 2h, when there is unremoved activated carbon in the zinc oxide, and the activated carbon is distributed on the surface and in the 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 with the activated carbon removed at high temperature has a regular and uniform rod-like structure, indicating that the initially formed nuclei are relatively uniform and the growth rate is substantially uniform.
After the microwave heating element zinc oxide obtained in the embodiment is heated in a microwave field for half an hour, the microstructure of the zinc oxide does not change, and is the same as the original microstructure, which shows that the zinc oxide has a stable structure when used for microwave heating.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The microwave heating body zinc oxide is characterized in that the zinc oxide has a rod-shaped and sheet-shaped micro-nano structure.
2. A microwave heating body zinc oxide as described in claim 1, wherein said zinc oxide is obtained by forming a support on a carbon material and then removing the carbon material;
preferably, the zinc oxide is formed by dehydrating zinc hydroxide on a carbon material;
preferably, the zinc oxide is obtained by dehydrating zinc hydroxide on a carbon material to form zinc oxide and calcining the zinc oxide to remove the carbon material.
3. A microwave heating body zinc oxide as claimed in claim 1, wherein the microwave heating body zinc oxide has a rod-like and sheet-like micro-nano structure, the micro-nano structure forms a single crystal cluster, and the crystal cluster forms a micron structure;
preferably, the crystal clusters corresponding to the rod-shaped zinc oxide form a radial micron structure, and the crystal clusters corresponding to the flake-shaped zinc oxide form a flower-shaped micron structure;
preferably, the width of the zinc oxide nano rod is 0.1-3um, and the length is 1-10um;
preferably, the thickness of the zinc oxide nano-sheet is 100-500nm, and the width is 0.1-1um.
4. A microwave heating body zinc oxide as described in claim 1, wherein said microwave heating body zinc oxide is heated to 300-1200 ℃ in 15-180 seconds under 2.45GHz microwave frequency radiation.
5. A preparation method of microwave heating element zinc oxide is characterized by comprising the following steps:
1) Mixing a zinc salt solution with ammonia water, reacting, and mixing with a carbon material to obtain a dispersion liquid;
2) Heating the dispersion liquid under microwave, and separating to obtain solid substance;
3) Calcining the solid substance obtained in the step 2) to obtain the microwave heating element zinc oxide.
6. A method for preparing a microwave heating body zinc oxide as claimed in claim 5, characterized in that, 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 to obtain a zinc acetate solution;
preferably, the mass ratio of the carbon material to the zinc salt is 1 (1-200); preferably, 1 (20-100),
preferably, the solvent is water;
preferably, the adding of the ammonia water and the carbon material for reaction specifically comprises: firstly, adding ammonia water into a zinc salt solution, stirring at room temperature for 10min-10h, then adding a carbon material, and stirring at room temperature for 5min-10h;
preferably, the carbon material is activated carbon, carbon black or carbon nanotubes.
7. A method for preparing a microwave heating body zinc oxide as claimed in claim 5, characterized in that in step 2), the power of the microwave is 400-700W, and the heating time is 1min-3h;
preferably, the separation can be performed by centrifugation, and the obtained solid substance is preferably dried after separation.
In step 3), the calcination temperature is preferably 400 to 1000 ℃, for example 500 to 900 ℃, and the calcination time is, for example, 1 to 10 hours.
8. A microwave heating body zinc oxide prepared by the method of any one of claims 5 to 7.
9. Use of a microwave heating element zinc oxide according to any one of claims 1 to 4 and 8, characterized by its use in microwave chemical synthesis, catalysis, medical treatment, ceramics.
10. Use of a microwave heating element zinc oxide according to any one of claims 1 to 4 and 8, characterized by its use in microwave heating.
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