CN101759146A - Method for preparing ZnO/ZnFe2O4 compound nano hollow sphere - Google Patents

Method for preparing ZnO/ZnFe2O4 compound nano hollow sphere Download PDF

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CN101759146A
CN101759146A CN201010101120A CN201010101120A CN101759146A CN 101759146 A CN101759146 A CN 101759146A CN 201010101120 A CN201010101120 A CN 201010101120A CN 201010101120 A CN201010101120 A CN 201010101120A CN 101759146 A CN101759146 A CN 101759146A
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compound
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znfe
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hollow sphere
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CN101759146B (en
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钱海生
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Zhejiang Normal University CJNU
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Abstract

The invention relates to the technical field of nano material preparation, in particular to a method for preparing ZnO/ZnFe2O4 compound nano hollow spheres. The method comprises the following steps of: (1) preparing a water solution of glucide compound; (2) placing the prepared water solution of glucide compound into a reaction container; (3) sealing the reaction container containing the prepared water solution of a glucide compound, after the heating, the reaction and the cooling of the sealed container, conduct centrifugal separation to obtain a product, washing the product with distilled water and absolute ethyl alcohol, and drying the washed product to obtain carbon spheres with the diameter of 200 nm to 4 mu m; (4) preparing an alcoholic solution containing the carbon spheres; (5) after the reaction of the prepared alcoholic solution containing the carbon spheres, conducting cooling and centrifugal separation to obtain carbon nano spheres cladded with metal hydroxides; (6) calcining the obtained arbon nano spheres clad with metal hydroxides to obtain the ZnO/ZnFe2O4 compound nano hollow spheres. The invention has the characteristics of simple operation and low technological requirements.

Description

A kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere
Technical field
The present invention relates to the nano material preparing technical field, particularly a kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere.
Background technology
Because nano hollow sphere material is the important nano structural material of a big class, have much important application in fields such as nanometer medicine, medicine release, air-sensitives, particularly have photoluminescent property, have the ZnO/ZnFe of magnetic property 2O 4The composite hollow ball nano material is at nanometer medicine, and a lot of fields such as photoelectric device all have very high using value, in addition, and ZnFe 2O 4Or a kind of gas sensitive of novelty as gas sensor, can be used for the detection of chlorine and alcohol gas.At present, the report of relevant preparation nano hollow sphere material, particularly relevant making ZnO/ZnFe 2O 4The report of compound nano-hollow sphere is few.U.S.'s " materials chemistry " (Chemistry of Materials,, the 17th volume, 95-101 page or leaf in 2005) has reported with a kind of novel presoma Fe 2Zn (OR) 8(R=tBu, iPr) under the condition of alkalescence, the process of collosol and gel obtains nano zine oxide and zinc ferrite composite nanometer particle, similar to the problem of other nano materials of Prepared by Sol Gel Method in the past, because reaction is finished under sol-gel process, product mainly is made up of nano particle.U.S.'s " Applied Physics wall bulletin " (Applied Physics Letters, 2005, the 86th volume, the 091906th page) reported the nano composite membrane that has prepared zinc ferrite and titanium dioxide with the radio frequency magnetic technique, this method is widely used in the film of the various materials of preparation, so can not get the compound nano-hollow sphere of zinc ferrite.Germany " applied chemistry " (Angewandte Chemie International Edition, 2004, the 43rd volume, the 597-601 page or leaf) reported that with glucose molecule charing taking place under the condition of hydro-thermal has prepared colloidal carbon sphere, this material with carbon element is owing to be that glucose molecule low-temperature carbonization under hydrothermal condition obtains, and there are a lot of organic functional groups on the surface.Germany's " Europe chemistry " (Chemistry-A European Journal, 2006, the 12nd volume, the 2039-2047 page or leaf) reported and utilize Nano carbon balls to show a layer adsorbing metal ions, the nano-hollow ball that has synthesized a series of oxides simultaneously as hard template, this method complex process requires high to operation.
To sum up, the existing method for preparing nano hollow sphere material exists complex process, the weak point high to operation requirements, making ZnO/ZnFe 2O 4Compound nano-hollow sphere does not also have the precedent of success.
Summary of the invention
The purpose of this invention is to provide a kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere.
The technical solution adopted in the present invention is finished in the following way: a kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere, making ZnO/ZnFe 2O 4The step of compound nano-hollow sphere is:
(1) with the saccharide compound compound concentration is the aqueous solution of the saccharide compound of 8～48g/L;
(2) the saccharide compound aqueous solution of being prepared is put into reaction vessel;
(3) will put into the reaction vessel sealing of the saccharide compound aqueous solution of being prepared, the reaction vessel of sealing is heated to 160～200 ℃, reacted 4～24 hours, through natural cooling, centrifugation obtains product, product is used distilled water and absolute ethanol washing respectively three times, and after the drying, obtaining diameter is the carbon ball of 200nm～4um;
(4) alcoholic solution of preparation carbon containing ball, the method for the alcoholic solution of preparation carbon containing ball is: adding diameter in the alcoholic solution of every L is carbon ball 1～25g, zinc salt 12.5～100g, molysite 0.1～5g, the weak base 12.5～200g of 200nm～4um;
(5) alcoholic solution with preparation carbon containing ball reacted 4～20 hours under 30～80 ℃ of conditions, obtained metal hydroxides carbon coated nanosphere after cooling, centrifugation;
(6) with gained metal hydroxides carbon coated nanosphere through 450～800 ℃ the calcining 2～10 hours, namely obtain ZnO/ZnFe 2O 4The composite hollow nanosphere.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, employed reaction vessel is that liner is made by polytetrafluoroethylene (PTFE), the reaction vessel that shell is made by steel material.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, saccharide compound is more than one in starch, glucose, beta-schardinger dextrin-, fructose, maltose and the sucrose.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, alcohol is more than one in methyl alcohol, ethanol and the propyl alcohol.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, zinc salt is more than one in zinc acetate, zinc chloride, zinc sulfate and the zinc nitrate.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, molysite is more than one in iron chloride, ferric nitrate, ferric acetate and the ferric sulfate.
At above-mentioned making ZnO/ZnFe 2O 4In the step of compound nano-hollow sphere, weak base is a kind of in urea, ammoniacal liquor, sodium acid carbonate, alanine and the methylamine.
A kind of making ZnO/ZnFe of the present invention 2O 4The product that the method for composite hollow nanosphere obtains is ZnO and ZnFe 2O 4Nano particle forms the hollow nano-sphere of shell.The ZnO/ZnFe that the inventive method prepares 2O 4The size of composite hollow nanosphere is to determine that by the size of employed template carbon ball the size range of composite oxides hollow ball is 60nm～2um.Can control the size of prepared composite hollow nanosphere by the size of controlling prepared carbon ball.
The present invention has following characteristics:
1, because the present invention has adopted Nano carbon balls as template, adopt molysite and zinc salt as reaction raw materials, temperature co-precipitation in alcoholic solution of control reaction has realized a large amount of making ZnO/ZnFe 2O 4Compound nano-hollow sphere has been avoided formation ZnO/ZnFe 2O 4Nano particle.
2, because the present invention adopts the carbonized product Nano carbon balls of the sugary carbohydrates be easy to get as hard template, molysite and zinc salt be in Nano carbon balls surface co-precipitation, operate simple and easyly, and technological requirement is simple, suitable industrialization production.
Description of drawings
Fig. 1 is the stereoscan photograph of Nano carbon balls.
Fig. 2 is ZnO/ZnFe 2O 4The transmission electron microscope photo of compound nano-hollow sphere.
Fig. 3 is ZnO/ZnFe 2O 4The X-ray diffraction style of composite hollow ball.
Fig. 4 is ZnO/ZnFe 2O 4The photoluminescence spectra of composite hollow nanosphere.
Fig. 5 is ZnO/ZnFe 2O 4The magnetization curve of composite hollow nanosphere.
The specific embodiment
Below by embodiment the present invention is made further instructions.
Embodiment 1
A kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere the steps include:
(1) 0.6g is restrained sucrose, be dispersed in the water of 24ml, become the aqueous solution of saccharide compound after the stirring and dissolving;
(2) liner of the saccharide compound aqueous solution of being prepared being put into 30ml is made by polytetrafluoroethylene (PTFE), in the reactor that shell is made by steel material;
(3) with after the reactor sealing, place 160 ℃ of baking ovens to keep 20 hours, through natural cooling, centrifugation obtains product, and product is used respectively distilled water and absolute ethanol washing three times, after the drying, obtains Nano carbon balls;
(4) get above-mentioned Nano carbon balls 0.02 gram, be dispersed in the ethanol of 20ml, add 0.25 zinc acetate, 2mg iron chloride and 0.25g sodium acid carbonate successively, after ultrasonic dispersion, obtain the alcoholic solution of carbon containing ball;
(5) the above-mentioned alcoholic solution of preparing the carbon containing ball was reacted 20 hours down at 80 ℃, after cooling, centrifugation, obtain metal hydroxides carbon coated nanosphere;
(6) gained metal hydroxides carbon coated nanosphere was calcined 10 hours at 450 ℃, namely obtained ZnO/ZnFe 2O 4The composite hollow nanosphere.
Adopt Philip X ' Pert PRO SUPER X-ray diffractometer respectively, field emission scanning electron microscope, the H-8010 of Hitachi transmission electron microscope, Perkin-Elmer LS55 XRF, MPMS (SQUID) magnetic measurement systems of Quantum Design company characterizes sample.
Adopt X-ray diffractometer that the result of study of final product is shown that product is by ZnO and ZnFe 2O 4Two phase compositions, illustrate that synthetic is ZnO/ZnFe 2O 4Nano-complex, as shown in Figure 1.
By field emission scanning electron microscope Nano carbon balls is observed.The diameter of the Nano carbon balls that provides from Fig. 2 is 500nm.
By the ZnO/ZnFe of transmission electron microscope to obtaining in the present embodiment 2O 4Nano-complex is observed.The transmission electron microscope photo that provides from Fig. 3 shows: the ZnO/ZnFe that obtains 2O 4Nano-complex is the hollow Nano spherical structure, diameter 200 nanometers of hollow ball, and the thickness of shell is 5～15 nanometers.
The ZnO/ZnFe that present embodiment is prepared 2O 4The luminescence generated by light of compound nano-hollow sphere studies show that at 376.8nm one narrow fluorescence emission peak is arranged, and this is the feature band gap emission peak of typical ZnO, and there is a wide fluorescence emission peak at the 609nm place, this be since fault in material cause luminous.
Process is to ZnO/ZnFe 2O 4The magnetic of compound nano-hollow sphere studies show that sample has ferromagnetism.
Embodiment 2
A kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere the steps include:
(1) 0.12g is restrained starch, be dispersed in the water of 24ml, become the aqueous solution of saccharide compound after the stirring and dissolving;
(2) liner of the saccharide compound aqueous solution of being prepared being put into 30ml is made by polytetrafluoroethylene (PTFE), in the reactor that shell is made by steel material;
(3) with after the reactor sealing, place 180 ℃ of baking ovens to keep 10 hours, through natural cooling, centrifugation obtains product, and product is used respectively distilled water and absolute ethanol washing three times, after the drying, obtains Nano carbon balls;
(4) get above-mentioned Nano carbon balls 0.5 gram, be dispersed in the methyl alcohol of 20ml, add the 2g zinc chloride successively, 0.05g ferric nitrate and 4g urea obtain the alcoholic solution of carbon containing ball after ultrasonic dispersion;
(5) the above-mentioned alcoholic solution of preparing the carbon containing ball was reacted 8 hours down at 60 ℃, after cooling, centrifugation, obtain metal hydroxides carbon coated nanosphere;
(6) gained metal hydroxides carbon coated nanosphere was calcined 5 hours at 600 ℃, namely obtained ZnO/ZnFe 2O 4The composite hollow nanosphere.
Adopt Philip X ' Pert PRO SUPER X-ray diffractometer respectively, field emission scanning electron microscope, the H-8010 of Hitachi transmission electron microscope, Perkin-Elmer LS55 XRF, MPMS (SQUID) magnetic measurement systems of Quantum Design company characterizes sample.
Adopt X-ray diffractometer that the result of study of final product is shown that product is by ZnO and ZnFe 2O 4Two phase compositions, illustrate that synthetic is ZnO/ZnFe 2O 4Nano-complex.
By field emission scanning electron microscope Nano carbon balls is observed and to be shown that the diameter of Nano carbon balls is 800nm.
By the ZnO/ZnFe of transmission electron microscope to obtaining in the present embodiment 2O 4Nano-complex is observed and is shown, the ZnO/ZnFe that obtains 2O 4Nano-complex is the hollow Nano spherical structure, and the diameter of hollow ball is 400 nanometers, and the thickness of shell is 6～12 nanometers.
The ZnO/ZnFe that present embodiment is prepared 2O 4The luminescence generated by light of compound nano-hollow sphere studies show that at 377.2nm one narrow fluorescence emission peak is arranged, and this is the feature band gap emission peak of typical ZnO, and there is a wide fluorescence emission peak at the 608.5nm place, this be since fault in material cause luminous.
Process is to ZnO/ZnFe 2O 4The magnetic of compound nano-hollow sphere studies show that sample also has ferromagnetism.
Embodiment 3
A kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere the steps include:
(1) 0.72g is restrained beta-schardinger dextrin-, be dispersed in the water of 24ml, become the aqueous solution of saccharide compound after the stirring and dissolving;
(2) liner of the saccharide compound aqueous solution of being prepared being put into 30ml is made by polytetrafluoroethylene (PTFE), in the reactor that shell is made by steel material;
(3) with after the reactor sealing, place 200 ℃ of baking ovens to keep 4 hours, through natural cooling, centrifugation obtains product, and product is used respectively distilled water and absolute ethanol washing three times, after the drying, obtains Nano carbon balls;
(4) get above-mentioned Nano carbon balls 0.1 gram, be dispersed in the methyl alcohol of 20ml, add 1g zinc nitrate, 0.1g ferric acetate and 1g ammoniacal liquor successively, after ultrasonic dispersion, obtain the alcoholic solution of carbon containing ball;
(5) the above-mentioned alcoholic solution of preparing the carbon containing ball was reacted 4 hours down at 30 ℃, leave standstill more than 10 minutes, obtain metal hydroxides carbon coated nanosphere after the centrifugation;
(6) gained metal hydroxides carbon coated nanosphere was calcined 2 hours at 800 ℃, namely obtained ZnO/ZnFe 2O 4The composite hollow nanosphere.
Adopt Philip X ' Pert PRO SUPER X-ray diffractometer respectively, field emission scanning electron microscope, the H-8010 of Hitachi transmission electron microscope, Perkin-Elmer LS55 XRF, MPMS (SQUID) magnetic measurement systems of Quantum Design company characterizes sample.
Adopt X-ray diffractometer that the result of study of final product is shown that product is by ZnO and ZnFe 2O 4The compound of two phase compositions.
By field emission scanning electron microscope Nano carbon balls is observed, the diameter of Nano carbon balls is 100nm.
By the ZnO/ZnFe of transmission electron microscope to obtaining in the present embodiment 2O 4Nano-complex is observed, the ZnO/ZnFe that obtains 2O 4Nano-complex is the hollow Nano spherical structure, and the diameter of hollow ball is 60 nanometers, and the thickness of shell is 4～9 nanometers.
The ZnO/ZnFe that present embodiment is prepared 2O 4The luminescence generated by light of compound nano-hollow sphere studies show that at 375.9nm one narrow fluorescence emission peak is arranged, and this is the feature band gap emission peak of typical ZnO, and there is a wide fluorescence emission peak at the 607.2nm place, this be since fault in material cause luminous.
Process is to ZnO/ZnFe 2O 4The magnetic of compound nano-hollow sphere studies show that sample has ferromagnetism.
Embodiment 4
A kind of making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere the steps include:
(1) with 1 gram glucose, is dispersed in the water of 24ml, becomes the aqueous solution of saccharide compound after the stirring and dissolving;
(2) liner of the saccharide compound aqueous solution of being prepared being put into 30ml is made by polytetrafluoroethylene (PTFE), in the reactor that shell is made by steel material;
(3) with after the reactor sealing, place 200 ℃ of baking ovens to keep 20 hours, through natural cooling, centrifugation obtains product, and product is used respectively distilled water and absolute ethanol washing three times, after the drying, obtains Nano carbon balls;
(4) get above-mentioned Nano carbon balls 0.2 gram, be dispersed in the propyl alcohol of 20ml, add 1g zinc nitrate, 0.1g ferric acetate and 1g urea successively, after ultrasonic dispersion, obtain the alcoholic solution of carbon containing ball;
(5) the above-mentioned alcoholic solution of preparing the carbon containing ball was reacted 8 hours down at 23 ℃, leave standstill more than 10 minutes, obtain metal hydroxides carbon coated nanosphere after the centrifugation;
(6) gained metal hydroxides carbon coated nanosphere was calcined 2 hours at 800 ℃, namely obtained ZnO/ZnFe 2O 4The composite hollow nanosphere.
Adopt Philip X ' Pert PRO SUPER X-ray diffractometer respectively, field emission scanning electron microscope, the H-8010 of Hitachi transmission electron microscope, Perkin-Elmer LS55 XRF, MPMS (SQUID) magnetic measurement systems of Quantum Design company characterizes sample.
Adopt X-ray diffractometer that the result of study of final product is shown that product is by ZnO and ZnFe 2O 4The compound of two phase compositions.
By field emission scanning electron microscope Nano carbon balls is observed, the diameter of carbon ball is 4um.
By the ZnO/ZnFe of transmission electron microscope to obtaining in the present embodiment 2O 4Nano-complex is observed, the ZnO/ZnFe that obtains 2O 4Nano-complex is hollow ball structure, and the diameter of hollow ball is 2um, and the thickness of shell is 15～20 nanometers.
The ZnO/ZnFe that present embodiment is prepared 2O 4The luminescence generated by light of compound nano-hollow sphere studies show that at 375.3nm one narrow fluorescence emission peak is arranged, and this is the feature band gap emission peak of typical ZnO, and there is a wide fluorescence emission peak at the 606.8nm place, this be since fault in material cause luminous.
Process is to ZnO/ZnFe 2O 4The magnetic of compound nano-hollow sphere studies show that sample has ferromagnetism.

Claims (8)

1. making ZnO/ZnFe 2O 4The method of compound nano-hollow sphere is characterized in that: making ZnO/ZnFe 2O 4The step of compound nano-hollow sphere is:
(1) with the saccharide compound compound concentration is the aqueous solution of the saccharide compound of 8～48g/L;
(2) the saccharide compound aqueous solution of being prepared is put into reaction vessel;
(3) will put into the reaction vessel sealing of the saccharide compound aqueous solution of being prepared, the reaction vessel of sealing is heated to 160～200 ℃, reacted 4～24 hours, through natural cooling, centrifugation obtains product, product is used distilled water and absolute ethanol washing respectively three times, and after the drying, obtaining diameter is the carbon ball of 200nm～4um;
(4) alcoholic solution of preparation carbon containing ball, the method for the alcoholic solution of preparation carbon containing ball is: adding diameter in the alcoholic solution of every L is carbon ball 1～25g, zinc salt 12.5～100g, molysite 0.1～5g, the weak base 12.5～200g of 200nm～4um;
(5) alcoholic solution with preparation carbon containing ball reacted 4～20 hours under 30～80 ℃ of conditions, obtained metal hydroxides carbon coated nanosphere after cooling, centrifugation;
(6) with gained metal hydroxides carbon coated nanosphere through 450～800 ℃ the calcining 2～10 hours, namely obtain ZnO/ZnFe 2O 4The composite hollow nanosphere.
2. making ZnO/ZnFe according to claim 1 2O 4The method of compound nano-hollow sphere is characterized in that: described reaction vessel is that liner is made by polytetrafluoroethylene (PTFE), the reaction vessel that shell is made by steel material.
3. making ZnO/ZnFe according to claim 1 and 2 2O 4The method of compound nano-hollow sphere is characterized in that: described saccharide compound is more than one in starch, glucose, beta-schardinger dextrin-, fructose, maltose and the sucrose.
4. making ZnO/ZnFe according to claim 1 and 2 2O 4The method of compound nano-hollow sphere is characterized in that: described alcohol is more than one in methyl alcohol, ethanol and the propyl alcohol.
5. making ZnO/ZnFe according to claim 1 and 2 2O 4The method of compound nano-hollow sphere is characterized in that: described zinc salt is more than one in zinc acetate, zinc chloride, zinc sulfate and the zinc nitrate.
6. making ZnO/ZnFe according to claim 1 and 2 2O 4The method of compound nano-hollow sphere is characterized in that: described molysite is more than one in iron chloride, ferric nitrate, ferric acetate and the ferric sulfate.
7. making ZnO/ZnFe according to claim 1 and 2 2O 4The method of compound nano-hollow sphere is characterized in that: described weak base is a kind of in urea, ammoniacal liquor, sodium acid carbonate, alanine and the methylamine.
8. making ZnO/ZnFe according to claim 3 2O 4The method of compound nano-hollow sphere is characterized in that: described alcohol is more than one in methyl alcohol, ethanol and the propyl alcohol; Described zinc salt is more than one in zinc acetate, zinc chloride, zinc sulfate and the zinc nitrate; Described molysite is more than one in iron chloride, ferric nitrate, ferric acetate and the ferric sulfate; Described weak base is a kind of in urea, ammoniacal liquor, sodium acid carbonate, alanine and the methylamine.
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CN105126855A (en) * 2015-07-15 2015-12-09 浙江大学 ZnO/ZnFe2O4/C nano-structure hollow spheres and preparation method of same
CN105126855B (en) * 2015-07-15 2018-08-07 浙江大学 ZnO/ZnFe2O4/ C nano structure hollow ball and preparation method thereof
CN105552334A (en) * 2016-01-11 2016-05-04 杭州电子科技大学 Preparation method for carbon-film-coated zinc oxide hollow sphere
CN105552334B (en) * 2016-01-11 2018-04-17 杭州电子科技大学 A kind of preparation method of carbon film coated zinc oxide hollow ball
CN109107562A (en) * 2018-09-19 2019-01-01 安庆师范大学 A kind of preparation method of Zinc oxide/titanium dioxide complex microsphere
CN109107562B (en) * 2018-09-19 2021-12-10 安庆师范大学 Preparation method of zinc oxide/titanium dioxide composite microspheres
CN109115843A (en) * 2018-09-20 2019-01-01 东北大学 A kind of Cu doping ZnFe2O4Nano particle and its preparation method and application
CN109115843B (en) * 2018-09-20 2020-12-25 东北大学 Cu-doped ZnFe2O4Nanoparticles, and preparation method and application thereof
CN110902726A (en) * 2019-11-15 2020-03-24 安徽建筑大学 Micro-nano structure zinc ferrite hollow sphere and preparation method thereof
CN110902726B (en) * 2019-11-15 2022-06-24 安徽建筑大学 Zinc ferrite hollow sphere with micro-nano structure and preparation method thereof
CN112708394A (en) * 2020-12-31 2021-04-27 东莞市深丰光电科技有限公司 Coating glue, protective film and preparation method
CN116328777A (en) * 2023-03-17 2023-06-27 西安交通大学 Preparation method of magnetic zinc oxide@zinc ferrite photocatalyst
CN116328777B (en) * 2023-03-17 2024-04-19 西安交通大学 Preparation method of magnetic zinc oxide@zinc ferrite photocatalyst

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