CN105749896A - Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel - Google Patents
Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 106
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 76
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004964 aerogel Substances 0.000 title abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000001632 sodium acetate Substances 0.000 claims abstract description 8
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 8
- 239000001509 sodium citrate Substances 0.000 claims abstract description 8
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004246 zinc acetate Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 239000013067 intermediate product Substances 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 150000003751 zinc Chemical class 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 239000002077 nanosphere Substances 0.000 claims description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical group [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract 2
- 230000000593 degrading effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- DIOZVWSHACHNRT-UHFFFAOYSA-N 2-(2-prop-2-enoxyethoxy)ethanol Chemical compound OCCOCCOCC=C DIOZVWSHACHNRT-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/23—
Abstract
The invention discloses a method for preparing zinc oxide/reduced graphene oxide aerogel and belongs to the field of novel nano materials and preparation of the materials. The method comprises the specific steps: preparing graphene oxide by adopting an improved Hummers method; carrying out ultrasonic oscillation and dispersion to obtain a dispersion solution of graphene oxide in ethylene glycol; then adding zinc acetate, sodium citrate and sodium acetate into the dispersion solution at a certain ratio, and uniformly stirring with a magnetic force; transferring the mixed solution into a reaction kettle and reacting at 150 DEG C to 200 DEG C for 10h; then taking out the product and repeatedly washing the product with de-ionized water and absolute ethyl alcohol for a plurality of times; then storing the product into a freezing drying box for 12h to obtain the zinc oxide/reduced graphene oxide aerogel. The aerogel prepared by the method has a complete structure and good heat stability; the control of shapes and sizes of the aerogel can be realized. The method is simple in process, low in cost and strong in practicability. The zinc oxide/reduced graphene oxide aerogel has a wide application prospect in the aspects of photocatalytically degrading organic pollutants and the like in the water.
Description
Technical field
The present invention relates to a kind of method preparing zinc oxide/redox graphene aeroge, belong to novel nano
Material and field of material preparation.Technique is simple, and low cost is practical, organic dirt in photocatalytic degradation water
The aspects such as dye thing have broad application prospects.
Background technology
Nanometer technology is 21 century particularly important scientific research field, and device based on nanometer technology etc. will
Revolutionary change is brought to every field, and in the basic nano structured unit of assemble nanometer device, two
It is indispensable for planting functional material strong, that structure is unique, and one is zinc oxide, and another kind is currently to process hand
Can heat Graphene, the two dimensional crystal of the most single Graphene atomic layer.Bi-material all has the photo electric of uniqueness
Can, the former has abundant low dimensional structures, and the latter has electricity, mechanics and the thermal conduction characteristic of excellence.
Aeroge is that a kind of density is ultralow, can keep water in a large number and don't can be dissolved in water, and can be swelling
Three-dimensional netted nano solid porous polymer material, has good electric conductivity and thermal conductivity.It was in 1931
Found by Kistler and propose.The preparation process of aeroge is relatively complicated, and under usual condition, it leads to before this
Cross the gel process of colloidal sol to make wet gel, afterwards through certain solvent switch, by surface in network space
The relatively large dissolution filter of tension force out, forms aeroges through a series of complex process the most again.
All superior functions based on aeroge, the research for its structure in recent years the most gradually increases, especially
Aerogel structure is applied to improve battery electrode performance, utilize its extra specific surface area as new catalyst or
Catalyst carrier processes the most serious water pollution problem, additionally, aerogel structure is in energy storage field,
The aspects such as pernicious gas absorption, Aero-Space all have the performance of brilliance, it is conceivable that, by zinc oxide, reduction
Graphene oxide composite material is expanded into three-dimensional aerogel structure, it will improves it further and leads in original application
Territory, the performance in terms of Degradation of Organo-pollutants in Water with Photo-catalysis etc..
Within 2013, it is published in the opinion " Self-Assembled of ACS Sustainable Chemistry&Engineering
Three-Dimensional Graphene-Based Aerogel with Embedded Multifarious Functional
Nanoparticles and Its Excellent Photoelectrochemical Activities " report a kind of employing water
Hot method one step is by TiO2Nano particle embeds and defines a kind of three-dimensional self assembly aerogel structure in Graphene, and
Predict this structure catalytic water under light illumination and produce H2In potential application.2009 at Appl.Phys.Lett
On deliver one about compound paper " the Vertically Aligned ZnO of Graphene and zinc oxide
Nanostructures Grown On Graphene Layers " report and utilize MOCVD at graphene film
The zinc oxide nano-wire array that surface deposition is vertical, the pattern of research zinc oxide controls and optical characteristics.But at present
Zinc oxide and graphene composite structure in these reports are substantially in the plane of a Graphene deposition oxygen
Change zinc, seldom realize developing zinc oxide while Graphene upper and lower surface, Graphene and oxidation more do not occur
Zinc is three-dimensional compound, as constituted aerogel structure.The most also there are some such as patent CN103482615A
" preparation method of a kind of foam-like Graphene-ZnO composite " is referred to answering of Graphene and zinc oxide
Close, including having made three-dimensional structure, but there is the problems such as temperature in building-up process is higher, be unfavorable for big face
Long-pending preparation.
In sum, current Graphene and the compound of zinc oxide are also only limited to single graphenic surface, really will
It is little that zinc oxide/redox graphene carries out being combined the report with prepared aeroge at three dimensions, so
The exploration of this respect will be work highly significant.
Summary of the invention
Technical problem: the present invention relates to a kind of zinc oxide/redox graphene aeroge and preparation method thereof, this
Bright be mostly in a plane based on current zinc oxide and Graphene are compound, use solvent-thermal method realize Graphene with
Zinc oxide is compound on three dimensions, the defect before preferably overcoming, and technique is simple, and low cost is practical
Property strong, have broad application prospects at aspects such as Degradation of Organo-pollutants in Water with Photo-catalysis.
Technical scheme: a kind of method preparing zinc oxide/redox graphene aeroge, the concrete step of described method
Rapid as follows:
1) preparation graphene oxide uniform dispersion in ethylene glycol；
2) addition soluble zinc salt, reducing agent, weak base reagent to dispersion liquid stirs；
3) above-mentioned mixed liquor is transferred in reactor, and at 150 DEG C-200 DEG C, carries out solvent-thermal process reaction fully
Rear taking-up, obtains intermediate product with deionized water and washes of absolute alcohol, and described intermediate product is by Graphene
The composite construction constituted with zinc oxide nanosphere；
4) intermediate product freeze-drying obtains zinc oxide/redox graphene aeroge.
Step 1) described in graphene oxide uniform dispersion in ethylene glycol refer to prepared oxidation
Graphene uniform is dispersed in ethylene glycol, is ultrasonically formed stable aaerosol solution, and the dispersion liquid concentration of preparation is
0.5mg/ml～1mg/ml.
Described soluble zinc salt includes any one in zinc acetate, zinc chloride or zinc nitrate, described weak base reagent bag
Including any one in sodium acetate, urea or ammoniacal liquor, described reducing agent is sodium citrate or hydrazine hydrate.
Soluble zinc salt and the mass ratio 10:1 of graphene oxide, described weak base reagent and reducing agent mass ratio
About 6:1；
The aeroge that the preparation method of described zinc oxide/redox graphene aeroge obtains, is by graphite
Jie's cavernous structure that alkene fold is formed, Graphene and zinc oxide composite construction are connected with each other stacking on three dimensions
And forming loose structure, spherical Zinc oxide nanoparticle is between graphene sheet layer.
Beneficial effect: the invention discloses a kind of method preparing zinc oxide/redox graphene aeroge.To
The sample characterization prepared eventually shows: sample achieves zinc oxide and Graphene being combined on three dimensions, this
Bright have a series of advantage: 1. reaction is temperature required relatively low, is effectively improved the security 2. technique letter of experiment
Single, use solvent-thermal method to synthesize in the solution, reaction speed is very fast, and raw material availability is high；3. pair equipment requirement
Low, it is only necessary to an isoperibol (baking oven), it is simple to industrialization large area produces, and cost is relatively low；4. repeat
Property strong, can be by the control in terms of adjusting related process parameters such as reagent dosage realizing aerogel structure.This
Zinc oxide/redox graphene the aeroge of invention preparation may be used for gas sensor, photocatalysis absorption fall
Solve the aspects such as organic pollution, solar cell and nano-device.5. intermediate product is being carried out freeze-drying
Time, the aerogel structure of generation can be with loading varying in size and producing different aerogel structure of container.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 sample surfaces；
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 2 sample surfaces；
Fig. 3 is the scanning electron microscope (SEM) photograph of embodiment 3 sample surfaces；
Fig. 4 is the transmission electron microscope figure preparing zinc oxide/redox graphene aeroge sample, permissible by figure
Find out that Graphene pleated structure is preferably wrapped in the spherical zinc oxide nano-particle grown, and this similar
Structure large area exist, be not difficult to confirm that the zinc oxide of preparation and Graphene composite effect are fine, the present invention proposes
This method there is feasibility.
Detailed description of the invention
A kind of method preparing zinc oxide/redox graphene aeroge, prepares certain density graphite oxide
Allyl diglycol dispersion liquid, is the most once proportionally added into other reagent, uses solvent-thermal method growth postlyophilization
Zinc oxide/redox graphene aeroge sample can be obtained.Specifically comprising the following steps that of described method
(1) uniform dispersion in the ethylene glycol of preparation graphene oxide: weigh the graphene oxide of certain mass
Spent glycol soaks 1h, and in the Vltrasonic device that power is 100W, ultrasonic 4h under room temperature, obtains uniform oxygen
Functionalized graphene ethylene glycol dispersion liquid；
(2) a certain proportion of zinc acetate, sodium citrate, sodium acetate to above-mentioned dispersion liquid, and magnetic it are sequentially added into
Power stirs；
(3) above-mentioned mixed liquor is transferred in reactor, takes out after reacting 10h at 150 DEG C-200 DEG C, and
Repeatedly clean repeatedly with deionized water and absolute ethyl alcohol；
(4) it is placed in 12h in freeze drying box and i.e. can get zinc oxide/redox graphene aeroge.
The concentration of described graphene oxide dispersion preparation is 0.5mg/ml～1mg/ml.
With instantiation, technical scheme is described below, but protection scope of the present invention is not limited to this；
Embodiment 1
(1) weigh 30mg graphene oxide 60ml ethylene glycol and soak 1h, be the ultrasonic of 100W at power
Ultrasonic 4h under room temperature in device, obtains uniform graphite oxide allyl diglycol dispersion liquid；
(2) 0.544g zinc acetate, 0.2g sodium citrate, 1.2g sodium acetate to above-mentioned dispersion liquid it are sequentially added into,
And magnetic agitation is uniform；
(3) above-mentioned mixed liquor is transferred in reactor, takes out after reacting 10h at 160 DEG C, and spend
Ionized water and absolute ethyl alcohol clean repeatedly repeatedly；
(4) it is placed in 12h in freeze drying box and i.e. can get zinc oxide/redox graphene aeroge.Its surface shape
Looks are as it is shown in figure 1, it may be seen that Jie's cavernous structure significantly formed by Graphene fold, due to system
Graphene and zinc oxide composite construction for going out are connected with each other stacking on three dimensions and form loose structure, very
Being all visible on naked eyes to this structure, the most spherical Zinc oxide nanoparticle is positioned at graphene film
Between Ceng.
Embodiment 2
(1) weigh 60mg graphene oxide 60ml ethylene glycol and soak 1h, be the ultrasonic of 100W at power
Ultrasonic 4h under room temperature in device, obtains uniform graphite oxide allyl diglycol dispersion liquid；
(2) 0.544g zinc chloride, 0.2g sodium citrate, 1.2g sodium acetate to above-mentioned dispersion liquid it are sequentially added into,
And magnetic agitation is uniform；
(3) above-mentioned mixed liquor is transferred in reactor, takes out after reacting 10h at 160 DEG C, and spend
Ionized water and absolute ethyl alcohol clean repeatedly repeatedly；
(4) it is placed in 12h in freeze drying box and i.e. can get zinc oxide/redox graphene aeroge.Its table
Face pattern, as in figure 2 it is shown, in this embodiment, reduce the concentration of graphene oxide, is being observed and embodiment
While Jie's cavernous structure similar in 1, find that spherical Zinc oxide nanoparticle is more, also
It is interspersed between graphene sheet layer.
Embodiment 3
(1) weigh 60mg graphene oxide 60ml ethylene glycol and soak 1h, be the ultrasonic of 100W at power
Ultrasonic 4h under room temperature in device, obtains uniform graphite oxide allyl diglycol dispersion liquid；
(2) 1.088g zinc acetate, 0.2g sodium citrate, 1.2g sodium acetate to above-mentioned dispersion liquid it are sequentially added into,
And magnetic agitation is uniform；
(3) above-mentioned mixed liquor is transferred in reactor, takes out after reacting 10h at 160 DEG C, and spend
Ionized water and absolute ethyl alcohol clean repeatedly repeatedly；
(4) it is placed in 12h in freeze drying box and i.e. can get zinc oxide/redox graphene aeroge.Its surface shape
Looks are as it is shown on figure 3, in fact much like with embodiment 2, and meso-hole structure is it is also obvious that be possibly due to
Add Zn2+Consumption so that final ZnO nano spherical structure becomes many.
Embodiment 4
(1) weigh 60mg graphene oxide 60ml ethylene glycol and soak 1h, be the ultrasonic of 100W at power
Ultrasonic 4h under room temperature in device, obtains uniform graphite oxide allyl diglycol dispersion liquid；
(2) 0.544g zinc nitrate, 0.2g sodium citrate, 1.2g sodium acetate to above-mentioned dispersion liquid it are sequentially added into,
And magnetic agitation is uniform；
(3) above-mentioned mixed liquor is transferred in reactor, takes out after reacting 10h at 200 DEG C, and spend
Ionized water and absolute ethyl alcohol clean repeatedly repeatedly；
(4) it is placed in 12h in freeze drying box and i.e. can get zinc oxide/redox graphene aeroge.Its table
Face pattern as shown in Figure 4, in this embodiment, improves reaction temperature, but the pattern of final sample and reality
Execute in example 3 substantially similar.
Claims (5)
1. the method preparing zinc oxide/redox graphene aeroge, it is characterised in that specifically comprising the following steps that of described method
1) preparation graphene oxide uniform dispersion in ethylene glycol；
2) addition soluble zinc salt, reducing agent, weak base reagent to dispersion liquid stirs；
3) above-mentioned mixed liquor is transferred in reactor, and take out after carrying out solvent-thermal process reaction fully at 150 DEG C-200 DEG C, obtaining intermediate product with deionized water and washes of absolute alcohol, described intermediate product is the composite construction being made up of Graphene and zinc oxide nanosphere；
4) intermediate product freeze-drying obtains zinc oxide/redox graphene aeroge.
2. according to the preparation method of the zinc oxide described in claim 1/redox graphene aeroge, it is characterized in that: step 1) described in graphene oxide uniform dispersion in ethylene glycol refer to be dispersed in ethylene glycol prepared graphene oxide, being ultrasonically formed stable aaerosol solution, the dispersion liquid concentration of preparation is 0.5mg/ml～1mg/ml.
3. according to the preparation method of the zinc oxide described in claim 1/redox graphene aeroge, it is characterized in that: described soluble zinc salt includes zinc acetate, in zinc chloride or zinc nitrate any one, described weak base reagent includes sodium acetate, in urea or ammoniacal liquor any one, described reducing agent is sodium citrate or hydrazine hydrate.
4. according to the preparation method of the zinc oxide described in claim 1/redox graphene aeroge, it is characterised in that: soluble zinc salt and the mass ratio 10:1 of graphene oxide, described weak base reagent and reducing agent mass ratio about 6:1.
5. the aeroge obtained according to the preparation method of the arbitrary described zinc oxide/redox graphene aeroge of Claims 1 to 4, it is characterized in that: be Jie's cavernous structure formed by Graphene fold, Graphene and zinc oxide composite construction are connected with each other stacking on three dimensions and form loose structure, and spherical Zinc oxide nanoparticle is between graphene sheet layer.
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| CN106442642A (en) * | 2016-08-30 | 2017-02-22 | 安徽师范大学 | Preparation method of zinc oxide/graphene composite material and resistance type gas sensor |
| CN106732514A (en) * | 2016-11-24 | 2017-05-31 | 河南师范大学 | Recoverable version zinc oxide/graphene aerogel photochemical catalyst and preparation method thereof |
| CN108187653A (en) * | 2018-01-11 | 2018-06-22 | 绍兴文理学院 | Preparation method of graphene-based photocatalytic material |
| CN109289718A (en) * | 2018-11-06 | 2019-02-01 | 中国人民解放军陆军工程大学 | A kind of three-dimensional redox graphene aerogel material and preparation method thereof |
| CN109775695A (en) * | 2019-01-31 | 2019-05-21 | 清华大学深圳研究生院 | Graphene micro-sphere material, preparation method and electrochemical energy storing device |
| CN110117004A (en) * | 2018-02-05 | 2019-08-13 | 庄鹏宇 | A kind of preparation method of redox graphene group compound film |
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| 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 |
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