CN107473261A - A kind of preparation method of zinc oxide/redox graphene composite - Google Patents
A kind of preparation method of zinc oxide/redox graphene composite Download PDFInfo
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- CN107473261A CN107473261A CN201710777049.1A CN201710777049A CN107473261A CN 107473261 A CN107473261 A CN 107473261A CN 201710777049 A CN201710777049 A CN 201710777049A CN 107473261 A CN107473261 A CN 107473261A
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention provides a kind of preparation method of zinc oxide/redox graphene composite, belongs to novel inorganic nano composite material preparation field.Specific steps include：Polyvinyl alcohol and soluble zinc salt are well mixed with certain proportion first, and foaming solid is obtained using Vacuum Freezing ＆ Drying Technology, in Muffle furnace calcining it is standby to obtain ZnO powder；Then graphite oxide is prepared using improved Hummers chemical oxidization methods, and adds the ZnO powder ultrasound prepared, stir thermal response kettle reaction of falling back, and finally centrifuges product, washs, being dried to obtain zinc oxide/redox graphene composite.The present invention preparation technology it is simply efficient, raw material is cheap and easy to get, and preparation process is green, obtained composite granule particle diameter distribution uniformly and good dispersion, can be widely used for the multiple fields such as light, electricity, chemistry.
Description
Technical field
The invention belongs to novel inorganic nano composite material preparation field, and in particular to a kind of zinc oxide/oxygen reduction fossil
The preparation method of black alkene composite.
Background technology
Zinc oxide is a kind of common race's multifunctional semiconductor material of broad-band gap II-VI, has unique optical property, electricity
Performance etc. is learned, is widely used in the fields such as chemistry, photoelectricity and Aero-Space.When the particle diameter of zinc oxide is reduced to Nano grade
When, can show again not available for macroscopic material one such as quantum size effect, macro quanta tunnel effect, skin effect
The excellent physicochemical characteristics of series, becomes the irreplaceable additive of the industries such as ceramics, rubber, paint, feed,
And one of preferred material of numerous areas such as sensor, fluorescent material, capacitor, absorbing material.
Graphene be one kind by carbon atom through sp2The monolayer honeycomb shape material with benzene six-membered ring structure that hydridization is formed,
Unique two-dimensional structure makes graphene have excellent physicochemical properties, such as big specific surface area, good electron-transporting
Energy, mechanical property etc..Redox graphene is the intermediate that the oxidized reducing process of graphite prepares graphene process, structure and stone
Black alkene is substantially the same, not only with the characteristics of specific surface area is big, electron transport ability is strong, also with one not available for graphene
A little oxygen-containing functional groups, the reunion of particle can be being reduced during compound with zinc oxide, is increasing electron transfer rate.
The method that the present invention prepares a kind of zinc oxide/redox graphene composite.Prepare zinc oxide/graphite at present
The method of alkene has a lot, such as Chinese patent CN101857222B discloses one kind and prepares graphene/zinc oxide using hydro-thermal method
The method of composite, the zinc oxide of generation exist in the form of nanoscale twins, nano particle, nano wire；Chinese patent
CN104098088B discloses a kind of method that the grapheme modified hybrid material of nano zine oxide is prepared using sol-gal process,
And it has been dispersed in rubber matrix and has improved mechanical property；Other Chinese patent CN103435033B discloses a kind of use and ground
Mill and ultrasonic technique combine the method for preparing graphene/zinc oxide composite, and wherein zinc oxide is with corynebacterium nano particle shape
State is present.Although the above method can prepare zinc oxide/graphene composite material, organic solvent be present and use more, process
Cumbersome, the problems such as pollution is high, while the composite prepared easily is reunited.Therefore, find a kind of process simplicity and be easily controlled,
The good dispersion and small preparation method of pollution, the popularization and application to zinc oxide/graphene composite material have great importance.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides the oxidation that a kind of technological process is simple, cost is low, pollution is small
The preparation method of zinc/redox graphene composite.First by graphite oxide, ultrasonic disperse is centrifuged and aoxidized in water
Graphene solution, the Zinc oxide powder that polyvinyl alcohol auxiliary desivac is prepared then is added, is finally obtained by hydro-thermal reaction
To zinc oxide/redox graphene composite.
Polyvinyl alcohol is combined by being unique in that for the present invention with Vacuum Freezing ＆ Drying Technology.On the one hand poly- second is utilized
The good surface-active of enol, particle is set to disperse to be more uniformly distributed in aqueous, while the particle in its polymer mesh structure
Movement be restricted, help to form the composite granule that particle diameter is smaller and is evenly distributed；On the other hand done using vacuum refrigeration
Dry technology, it is irreversible hard to avoid surface tension effects appearance of the conventional drying process when preparing nano-powder due to liquid phase
Agglomeration, in the drying process solvent by distil directly from solid-state be changed into gaseous form remove from product without formed times
What liquid phase, is so not only maintained the size of particle and chemical uniformity, and can obtain the preferable nanometer of dispersiveness
Powder.Meanwhile zinc oxide-graphene oxide mixed solution is subjected to hydro-thermal reaction, it can preferably realize graphene sheet layer pair
The cladding of Zinc oxide particles, greatly improves electron transfer rate.
The preparation method of a kind of zinc oxide/redox graphene composite, it is characterised in that comprise the following steps：
(1) graphite oxide is made using improved Hummers oxidizing process；
(2) polyvinyl alcohol of certain molecular weight is dissolved in deionized water, and adds a certain proportion of soluble zinc salt, magnetic
Power stirs；
(3) it will be put into vacuum freeze drier and be dried after the solution pre-freeze in step (2), obtain in foam-like
Between product；
(4) intermediate product described in step (3) is put into Muffle furnace and calcined, obtain zinc oxide nano-powder；
(5) in the step of graphite oxide described in step (1) being dissolved in into water ultrasound to peel off, and adding certain proportion (4)
The Zinc oxide powder continues ultrasound, and magnetic agitation uniformly obtains milk yellow zinc oxide-graphene oxide mixed solution；
(6) zinc oxide described in step (5)-graphene oxide mixed solution is poured into hydrothermal reaction kettle, oil bath adds
Product is centrifuged after hot certain time, washed, is dried to obtain zinc oxide/redox graphene composite.
In above-mentioned preparation method, the mass concentration of polyvinyl alcohol described in step (2) is 1%~5%, when mass concentration is small
When 1%, the solid not easily collecting after freezing, when mass concentration is more than 5%, the easy gelation of polyvinyl alcohol water solution, make sample
Product are difficult to freeze.
In above-mentioned preparation method, the soluble zinc salt described in step (2) is zinc nitrate hexahydrate [Zn (NO3)2·6H2O]
With acetic anhydride zinc [Zn (CH3COO)2]。
In above-mentioned preparation method, the mass ratio of polyvinyl alcohol and soluble zinc salt described in step (2) is 4:1~1:8,
When mass ratio is less than 4:When 1, obtained particle diameter of nanometer powder skewness, when mass ratio is more than 1:When 8, obtained nano powder
Body is easily reunited, and dispersiveness declines.
In above-mentioned preparation method, the pre-freeze time of freeze-drying is 10~15h in step (3), is -55 in condenser temperature
DEG C, operating pressure be 10Pa vacuum freeze drier in cooling time be 10~15h.
In above-mentioned preparation method, calcining heat in step (4) is 400~800 DEG C, and the heating-up time is 1~6h, during insulation
Between be 1~6h.
In above-mentioned preparation method, the ultrasonic time that graphene oxide solution is prepared described in step (5) is 0.5~2h, is surpassed
When the sound time is less than 0.5h, the peeling effect of graphite oxide is very poor, when ultrasonic time is more than 2h, graphene oxide layer structure quilt
Destroy.
In above-mentioned preparation method, the hydro-thermal reaction time of zinc oxide-graphene oxide mixed solution is described in step (6)
1~20h, with the growth in reaction time, it is more abundant that graphene oxide is reduced to graphene.
Compared with prior art, advantage of the invention is that：
(1) preparation technology of the invention is simple, and synthesis condition is gentle, and practical operation is convenient；
(2) raw material used in the present invention is cheap and easy to get, in operating process be not used organic solvent, environmental pollution compared with
It is small, be advantageous to industrialized production；
(3) zinc oxide/redox graphene composite prepared by the present invention is evenly distributed, and wherein zinc oxide is six
Square wurtzite structure, zinc oxide show good dispersiveness in the presence of polyvinyl alcohol, and redox graphene can
Good coating zinc oxide particle.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram (XRD) of zinc oxide/redox graphene (ZnO/rGO) in the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of zinc oxide/redox graphene in the embodiment of the present invention 1.
Embodiment
Below in conjunction with drawings and examples, the present invention is described in detail.
Embodiment 1
The preparation of graphite oxide：It is using improved Hummers oxidizing process, 5g graphite powders, 2.5g sodium nitrate and 120ml is dense
Sulfuric acid (98%) is added in beaker, magnetic agitation under condition of ice bath.15g potassium permanganate is slowly added to, controlling reaction temperature does not surpass
10 DEG C are crossed, stirring reaction carries out medium temperature reaction after 2 hours, question response system temperature continues reaction 2 hours after rising to 35 DEG C, slowly
Add 200ml deionized waters, controlling reaction temperature reacts 1.5 hours solution and becomes golden yellow at 98 DEG C or so, add it is a large amount of go from
Sub- water terminating reaction, 20ml hydrogen peroxide (30%) is continuously added, is washed after cooling with 1mol/L aqueous hydrochloric acid solution, then with largely
Until neutral, finally freeze-drying obtains graphite oxide powder for deionized water washing.
The polyvinyl alcohol that 1g molecular weight is 16000 is weighed, pours into 50ml deionized waters, is stirred under the conditions of 75 DEG C of oil baths
30min makes polyvinyl alcohol fully dissolve, room temperature cooling.Weigh the poly-vinyl alcohol solution that 4g zinc nitrate hexahydrates are added after cooling
In, magnetic agitation 1h.Then mixed solution is poured into freeze dryer sample disc, vacuum refrigeration is transferred to after abundant pre-freeze under low temperature
10h is dried in drying machine, obtains foam-like intermediate product.Intermediate product is put into Muffle furnace, 2h is warming up under air atmosphere
550 DEG C and it is incubated 6h and obtains zinc oxide nano-powder.
30mg graphite oxides are weighed, add 30ml deionized water ultrasonic disperse 0.5h, add 300mg Zinc oxide powders, after
After continuing ultrasonic 0.5h, magnetic agitation 3h, 120 DEG C of reaction 5h in 50ml hydrothermal reaction kettles are poured into, finally product is centrifuged, washed,
It is dried to obtain zinc oxide/redox graphene composite granule.
The X-ray diffractogram (XRD) of zinc oxide/redox graphene prepared by the present embodiment is as shown in Figure 1.By scheming
1, as can be seen that nano zine oxide is hexagonal wurtzite structure in the zinc oxide/redox graphene prepared, has higher
Purity and crystallinity.
The scanning electron microscope (SEM) photograph (SEM) of zinc oxide/redox graphene prepared by the present embodiment is as shown in Figure 2.By Fig. 2
Coat to form tridimensional network as can be seen that Zinc oxide nanoparticle is reduced graphene oxide layer, zinc oxide it is straight
Footpath is 60~150nm.
Embodiment 2
The preparation of graphite oxide：Repeat the preparation process of graphite oxide in embodiment 1.
The polyvinyl alcohol that 1g molecular weight is 95000 is weighed, pours into 50ml deionized waters, is stirred under the conditions of 75 DEG C of oil baths
30min makes polyvinyl alcohol fully dissolve, room temperature cooling.Weigh in the poly-vinyl alcohol solution after 1g acetic anhydrides zinc adds cooling,
Magnetic agitation 1h.Then mixed solution is poured into freeze dryer sample disc, being transferred to vacuum refrigeration after abundant pre-freeze under low temperature does
10h is dried in dry machine, obtains foam-like intermediate product.Intermediate product is put into Muffle furnace, 2h is warming up to 500 under air atmosphere
DEG C and be incubated 1h and obtain zinc oxide nano-powder.
3mg graphite oxides are weighed, add 30ml deionized water ultrasonic disperse 0.5h, add 300mg Zinc oxide powders, are continued
After ultrasonic 0.5h, magnetic agitation 1h, 100 DEG C of reaction 3h in 50ml hydrothermal reaction kettles are poured into, finally product is centrifuged, wash, done
It is dry to obtain zinc oxide/redox graphene composite granule.
Embodiment 3
The preparation of graphite oxide：Repeat the preparation process of graphite oxide in embodiment 1.
The polyvinyl alcohol that 4g molecular weight is 16000 is weighed, pours into 50ml deionized waters, is stirred under the conditions of 75 DEG C of oil baths
30min makes polyvinyl alcohol fully dissolve, room temperature cooling.Weigh the poly-vinyl alcohol solution that 1g zinc nitrate hexahydrates are added after cooling
In, magnetic agitation 2h.Then mixed solution is poured into freeze dryer sample disc, vacuum refrigeration is transferred to after abundant pre-freeze under low temperature
10h is dried in drying machine, obtains foam-like intermediate product.Intermediate product is put into Muffle furnace, 3h is warming up under air atmosphere
550 DEG C and it is incubated 3h and obtains zinc oxide nano-powder.
90mg graphite oxides are weighed, add 30ml deionized water ultrasonic disperse 1h, add 300mg Zinc oxide powders, are continued
After ultrasonic 0.5h, magnetic agitation 2h, 120 DEG C of reaction 10h in 50ml hydrothermal reaction kettles are poured into, finally product is centrifuged, wash, done
It is dry to obtain zinc oxide/redox graphene composite granule.
Embodiment 4
The preparation of graphite oxide：Repeat the preparation process of graphite oxide in embodiment 1.
The polyvinyl alcohol that 1g molecular weight is 16000 is weighed, pours into 50ml deionized waters, is stirred under the conditions of 75 DEG C of oil baths
30min makes polyvinyl alcohol fully dissolve, room temperature cooling.Weigh the poly-vinyl alcohol solution that 4g zinc nitrate hexahydrates are added after cooling
In, magnetic agitation 2h.Then mixed solution is poured into freeze dryer sample disc, vacuum refrigeration is transferred to after abundant pre-freeze under low temperature
10h is dried in drying machine, obtains foam-like intermediate product.Intermediate product is put into Muffle furnace, 5h is warming up under air atmosphere
800 DEG C and it is incubated 3h and obtains zinc oxide nano-powder.
15mg graphite oxides are weighed, add 30ml deionized water ultrasonic disperse 0.5h, add 300mg Zinc oxide powders, after
After continuing ultrasonic 1h, magnetic agitation 5h, 140 DEG C of reaction 5h in 50ml hydrothermal reaction kettles are poured into, finally product is centrifuged, wash, done
It is dry to obtain zinc oxide/redox graphene composite granule.
It can be seen from the present embodiment the present invention have the characteristics that technological process be simple and convenient to operate, pollute it is small.It is every
Similarity method and similar change using the present invention, all should be included in protection scope of the present invention.
Claims (9)
1. the preparation method of a kind of zinc oxide/redox graphene composite, it is characterised in that comprise the following steps：
(1) graphite oxide is made using improved Hummers oxidizing process；
(2) polyvinyl alcohol of certain molecular weight is dissolved in deionized water, and adds a certain proportion of soluble zinc salt, magnetic force stirs
Mix uniformly；
(3) it will be put into vacuum freeze drier and be dried after the solution pre-freeze in step (2), obtain the middle production of foam-like
Thing；
(4) intermediate product described in step (3) is put into Muffle furnace and calcined, obtain zinc oxide nano-powder；
(5) described in the step of graphite oxide described in step (1) being dissolved in into water ultrasound to peel off, and adding certain proportion (4)
Zinc oxide powder continues ultrasound, and magnetic agitation uniformly obtains milk yellow zinc oxide-graphene oxide mixed solution；
(6) zinc oxide described in step (5)-graphene oxide mixed solution is poured into hydrothermal reaction kettle, oil bath heating one
Product is centrifuged after fixing time, washed, is dried to obtain zinc oxide/redox graphene composite.
2. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the molecular weight of polyvinyl alcohol described in step (2) is 10000~100000.
3. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the soluble zinc salt described in step (2) is zinc nitrate hexahydrate [Zn (NO3)2·6H2O] and acetic anhydride zinc [Zn
(CH3COO)2] in it is any.
4. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the mass ratio of polyvinyl alcohol and soluble zinc salt described in step (2) is 4:1~1:8, time of magnetic agitation for 0.5~
2h。
5. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the drying process used in step (3) is Vacuum Freezing ＆ Drying Technology.
6. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the calcining heat in step (4) is 400~800 DEG C, and the heating-up time is 1~6h, and soaking time is 1~6h.
7. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the mass ratio of graphite oxide and zinc oxide in step (5) is 1:2~1:100, ultrasonic time is 0.5~2h, magnetic agitation
Time is 1~5h.
8. according to the preparation method of zinc oxide/redox graphene composite described in claim 1, its feature exists
In the hydro-thermal reaction time in step (6) is 1~20h, and hydrothermal temperature is 100~200 DEG C.
9. a kind of zinc oxide/redox graphene composite prepared by claim 1 to 8 methods described, its feature exist
In redox graphene lamella coating zinc oxide nanometer in prepared zinc oxide/redox graphene composite
Particle shape is into tridimensional network, a diameter of 60~150nm of zinc oxide.
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Cited By (11)
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| CN108168613A (en) * | 2017-12-29 | 2018-06-15 | 李文清 | The air-quality monitoring system to cooperate with unmanned plane |
| CN108807961A (en) * | 2018-06-06 | 2018-11-13 | 上海电力学院 | A kind of zinc-base cell negative electrode material and preparation method thereof |
| CN109399616A (en) * | 2018-12-11 | 2019-03-01 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene organic material and its application in gas sensor |
| CN110627108A (en) * | 2019-09-27 | 2019-12-31 | 东华大学 | Zinc oxide/reduced graphene oxide composite material and preparation method and application thereof |
| CN110707319A (en) * | 2019-09-27 | 2020-01-17 | 上海应用技术大学 | Three-dimensional structured graphene-based iron oxide composite material and preparation and application thereof |
| CN110790988A (en) * | 2019-10-28 | 2020-02-14 | 安徽锦华氧化锌有限公司 | Processing method of high-performance rubber containing nano zinc oxide |
| CN111229316A (en) * | 2020-03-06 | 2020-06-05 | 浙江工业大学 | Preparation method of zinc oxide supported three-dimensional honeycomb carbon-based nano material with adjustable aperture |
| WO2020134252A1 (en) * | 2018-12-28 | 2020-07-02 | Tcl科技集团股份有限公司 | Composite material, thin film and preparing method therefor and quantum dot light-emitting diode |
| CN111509401A (en) * | 2020-04-24 | 2020-08-07 | 张荣虎 | Wave-absorbing material of cobalt-doped zinc oxide-polymer-based carbon material and preparation method thereof |
| CN113582218A (en) * | 2021-07-30 | 2021-11-02 | 陕西科技大学 | Oxygen-deficient gray zinc oxide and preparation method and application thereof |
| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108168613A (en) * | 2017-12-29 | 2018-06-15 | 李文清 | The air-quality monitoring system to cooperate with unmanned plane |
| CN108807961A (en) * | 2018-06-06 | 2018-11-13 | 上海电力学院 | A kind of zinc-base cell negative electrode material and preparation method thereof |
| CN109399616A (en) * | 2018-12-11 | 2019-03-01 | 四川省安德盖姆石墨烯科技有限公司 | A kind of graphene organic material and its application in gas sensor |
| WO2020134252A1 (en) * | 2018-12-28 | 2020-07-02 | Tcl科技集团股份有限公司 | Composite material, thin film and preparing method therefor and quantum dot light-emitting diode |
| CN110627108A (en) * | 2019-09-27 | 2019-12-31 | 东华大学 | Zinc oxide/reduced graphene oxide composite material and preparation method and application thereof |
| CN110707319A (en) * | 2019-09-27 | 2020-01-17 | 上海应用技术大学 | Three-dimensional structured graphene-based iron oxide composite material and preparation and application thereof |
| CN110790988A (en) * | 2019-10-28 | 2020-02-14 | 安徽锦华氧化锌有限公司 | Processing method of high-performance rubber containing nano zinc oxide |
| CN111229316A (en) * | 2020-03-06 | 2020-06-05 | 浙江工业大学 | Preparation method of zinc oxide supported three-dimensional honeycomb carbon-based nano material with adjustable aperture |
| CN111509401A (en) * | 2020-04-24 | 2020-08-07 | 张荣虎 | Wave-absorbing material of cobalt-doped zinc oxide-polymer-based carbon material and preparation method thereof |
| CN111509401B (en) * | 2020-04-24 | 2021-09-24 | 桂阳银龙科技有限责任公司 | Wave-absorbing material of cobalt-doped zinc oxide-polymer-based carbon material and preparation method thereof |
| CN113582218A (en) * | 2021-07-30 | 2021-11-02 | 陕西科技大学 | Oxygen-deficient gray zinc oxide and preparation method and application thereof |
| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
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