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
- Publication number
- CN105749896A CN105749896A CN201610086811.7A CN201610086811A CN105749896A CN 105749896 A CN105749896 A CN 105749896A CN 201610086811 A CN201610086811 A CN 201610086811A CN 105749896 A CN105749896 A CN 105749896A
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- graphene oxide
- oxide
- zinc
- airgel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 104
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 74
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004964 aerogel Substances 0.000 title description 11
- 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 27
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000004246 zinc acetate Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 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
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 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
- 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
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 235000013877 carbamide Nutrition 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 238000004729 solvothermal method Methods 0.000 claims 1
- 239000000725 suspension Substances 0.000 claims 1
- 238000002525 ultrasonication Methods 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 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 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 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
- 238000010276 construction Methods 0.000 description 3
- 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
- 239000002086 nanomaterial 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 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
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明公开了一种制备氧化锌/还原氧化石墨烯气凝胶的方法，属于新型纳米材料和材料制备领域。具体步骤包括：采用改进的Hummers法制备氧化石墨烯，经过超声振荡分散得到氧化石墨烯在乙二醇中的分散液；接着加入一定比例的乙酸锌、柠檬酸钠、乙酸钠至分散液，并磁力搅拌均匀；再将上述混合液转移至反应釜中在150℃?200℃下反应10h后取出，用去离子水和无水乙醇反复清洗多次；之后置于冷冻干燥箱中12h即可得到氧化锌/还原氧化石墨烯气凝胶。这种方法制得的气凝胶结构完整，热稳定性好，且可以实现对气凝胶的形状、尺寸的控制。本发明工艺简单，成本低，实用性强。在光催化降解水中有机污染物等方面具有广阔的应用前景。
The invention discloses a method for preparing zinc oxide/reduced graphene oxide airgel, which belongs to the field of novel nanometer materials and material preparation. The specific steps include: using the improved Hummers method to prepare graphene oxide, and obtaining a dispersion of graphene oxide in ethylene glycol through ultrasonic vibration dispersion; then adding a certain proportion of zinc acetate, sodium citrate, and sodium acetate to the dispersion, and Stir evenly with magnetic force; then transfer the above mixed solution to the reaction kettle and react at 150°C to 200°C for 10 hours, take it out, wash it repeatedly with deionized water and absolute ethanol; then put it in a freeze-drying box for 12 hours to get Zinc oxide/reduced graphene oxide airgel. The airgel prepared by this method has a complete structure, good thermal stability, and can realize the control of the shape and size of the airgel. The invention has simple process, low cost and strong practicability. It has broad application prospects in photocatalytic degradation of organic pollutants in 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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610086811.7A CN105749896A (en) | 2016-02-15 | 2016-02-15 | Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610086811.7A CN105749896A (en) | 2016-02-15 | 2016-02-15 | Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105749896A true CN105749896A (en) | 2016-07-13 |
Family
ID=56330737
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610086811.7A Pending CN105749896A (en) | 2016-02-15 | 2016-02-15 | Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105749896A (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395873A (en) * | 2016-09-27 | 2017-02-15 | 东南大学 | Preparation method of ultra-light blocky aluminum oxide aerogel |
| 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 | Three-dimensional reduced graphene oxide 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 |
| CN110161080A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | The preparation method of highly sensitive gas sensor based on graphene aerogel |
| 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 |
| CN111410191A (en) * | 2020-05-07 | 2020-07-14 | 山东华达新材料有限公司 | Graphene semiconductor preparation device and method |
| CN112973731A (en) * | 2021-03-05 | 2021-06-18 | 江苏美玛技术有限公司 | Preparation method of catalyst for hydrogen purification of new energy fuel cell |
| CN113578212A (en) * | 2021-07-09 | 2021-11-02 | 西安理工大学 | Zinc oxide/graphene oxide/carbon nanotube aerogel and method |
| CN113996297A (en) * | 2021-11-29 | 2022-02-01 | 西南交通大学 | Preparation method of silver/zinc oxide/graphene aerogel photocatalyst |
| CN114575141A (en) * | 2022-03-11 | 2022-06-03 | 罗莱生活科技股份有限公司 | Nano sea-island fibre/terylene composite material and its preparing method |
| CN114622329A (en) * | 2022-03-11 | 2022-06-14 | 罗莱生活科技股份有限公司 | Nano antibacterial sea-island fiber fabric and manufacturing method thereof |
| CN114635208A (en) * | 2022-03-11 | 2022-06-17 | 罗莱生活科技股份有限公司 | Terylene/sea-island fiber non-elastic core-spun yarn and fabric thereof |
| CN119432046A (en) * | 2025-01-10 | 2025-02-14 | 山东英特医疗科技有限公司 | A method for preparing TPU gloves |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430401A (en) * | 2011-09-20 | 2012-05-02 | 上海大学 | Nanometer ZnO/graphene photo-catalyst and preparation method thereof |
| CN102580716A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing zinc oxide/graphene composite by solvothermal method |
| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
-
2016
- 2016-02-15 CN CN201610086811.7A patent/CN105749896A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430401A (en) * | 2011-09-20 | 2012-05-02 | 上海大学 | Nanometer ZnO/graphene photo-catalyst and preparation method thereof |
| CN102580716A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing zinc oxide/graphene composite by solvothermal method |
| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
Non-Patent Citations (1)
| Title |
|---|
| XIN LIU等: "Novel 3D graphene aerogel–ZnO composites as efficient detection for NO2 at room temperature", 《SENSORS AND ACTUATORS B》 * |
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106442642B (en) * | 2016-08-30 | 2019-05-14 | 安徽师范大学 | A kind of preparation method of zinc oxide/graphene composite material, resistor-type gas sensor |
| CN106395873A (en) * | 2016-09-27 | 2017-02-15 | 东南大学 | Preparation method of ultra-light blocky aluminum oxide aerogel |
| 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 |
| CN106732514B (en) * | 2016-11-24 | 2020-02-04 | 河南师范大学 | Recyclable zinc oxide/graphene aerogel photocatalyst 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 |
| CN110117004A (en) * | 2018-02-05 | 2019-08-13 | 庄鹏宇 | A kind of preparation method of redox graphene group compound film |
| CN110161080A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | The preparation method of highly sensitive gas sensor based on graphene aerogel |
| CN109289718A (en) * | 2018-11-06 | 2019-02-01 | 中国人民解放军陆军工程大学 | Three-dimensional reduced graphene oxide 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 |
| 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 |
| CN111410191A (en) * | 2020-05-07 | 2020-07-14 | 山东华达新材料有限公司 | Graphene semiconductor preparation device and method |
| CN112973731A (en) * | 2021-03-05 | 2021-06-18 | 江苏美玛技术有限公司 | Preparation method of catalyst for hydrogen purification of new energy fuel cell |
| CN112973731B (en) * | 2021-03-05 | 2023-08-15 | 山东德易智能科技有限公司 | Preparation method of catalyst for hydrogen purification of new energy fuel cell |
| CN113578212A (en) * | 2021-07-09 | 2021-11-02 | 西安理工大学 | Zinc oxide/graphene oxide/carbon nanotube aerogel and method |
| CN113578212B (en) * | 2021-07-09 | 2022-08-02 | 西安理工大学 | Zinc oxide/graphene oxide/carbon nanotube aerogel and method |
| CN113996297A (en) * | 2021-11-29 | 2022-02-01 | 西南交通大学 | Preparation method of silver/zinc oxide/graphene aerogel photocatalyst |
| CN113996297B (en) * | 2021-11-29 | 2023-02-28 | 西南交通大学 | Preparation method of silver/zinc oxide/graphene airgel photocatalyst |
| CN114575141A (en) * | 2022-03-11 | 2022-06-03 | 罗莱生活科技股份有限公司 | Nano sea-island fibre/terylene composite material and its preparing method |
| CN114622329A (en) * | 2022-03-11 | 2022-06-14 | 罗莱生活科技股份有限公司 | Nano antibacterial sea-island fiber fabric and manufacturing method thereof |
| CN114635208A (en) * | 2022-03-11 | 2022-06-17 | 罗莱生活科技股份有限公司 | Terylene/sea-island fiber non-elastic core-spun yarn and fabric thereof |
| CN119432046A (en) * | 2025-01-10 | 2025-02-14 | 山东英特医疗科技有限公司 | A method for preparing TPU gloves |
| CN119432046B (en) * | 2025-01-10 | 2025-03-28 | 山东英特医疗科技有限公司 | TPU glove preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105749896A (en) | Zinc oxide/reduced graphene oxide aerogel and preparation method of zinc oxide/reduced graphene oxide aerogel | |
| Pant et al. | Carbon nanofibers wrapped with zinc oxide nano-flakes as promising electrode material for supercapacitors | |
| Sun et al. | Diatom silica, an emerging biomaterial for energy conversion and storage | |
| Wang et al. | Construction of Z-scheme MoSe2/CdSe hollow nanostructure with enhanced full spectrum photocatalytic activity | |
| CN105499600B (en) | A kind of method for preparing nano silver wire graphene composite aerogel | |
| Jiang et al. | Intercalation engineering of MXenes towards highly efficient photo (electrocatalytic) hydrogen evolution reactions | |
| CN103816905B (en) | A kind of preparation method of carbon nanotube loaded nanometer cobalt catalyst | |
| Li et al. | Multiscale porous carbon nanomaterials for applications in advanced rechargeable batteries | |
| JP6854531B2 (en) | electrode | |
| Liu et al. | Anchoring ultrafine Co3O4 grains on reduced oxide graphene by dual-template nanocasting strategy for high-energy solid state supercapacitor | |
| Peng et al. | One-dimensionally oriented self-assembly of ordered mesoporous nanofibers featuring tailorable mesophases via kinetic control | |
| CN104001547B (en) | Preparation method and application of an environment-friendly core-shell one-dimensional nano-copper wire-organometallic framework ZIF-8 composite catalyst | |
| Cao et al. | Two-dimensional porous micro/nano metal oxides templated by graphene oxide | |
| CN106044754A (en) | Preparation method of heteroatom doped graphene hierarchical pore carbon material | |
| Han et al. | Research progresses in the preparation of Co-based catalyst derived from Co-MOFs and application in the catalytic oxidation reaction | |
| Li et al. | Novel freestanding core-shell nanofibrillated cellulose/polypyrrole/tubular graphitic carbon nitride composite film for supercapacitors electrodes | |
| CN105384193A (en) | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst | |
| Bai et al. | Acetylenic bond-driven efficient hydrogen production of a graphdiyne based catalyst | |
| Yao et al. | Amorphous FeOOH nanoparticles decorated on defect-rich porous Ni MOF nanosheet based hierarchical architectures toward superior OER performance | |
| Yuan et al. | Template-free synthesis of ordered mesoporous NiO/poly (sodium-4-styrene sulfonate) functionalized carbon nanotubes composite for electrochemical capacitors | |
| CN105836738A (en) | Non-carbon heteroatom-modified porous graphene framework and preparation method thereof | |
| CN104347877A (en) | A nanometer level graphene-based composite material and a preparing method thereof | |
| Wang et al. | ZIF-derived porous carbon composites coated on NiCo2S4 nanotubes array toward efficient water splitting | |
| Zhong et al. | Metal–organic frameworks on versatile substrates | |
| Tan et al. | Fabrication of graphene-supported Zn-BTC with different morphologies and their supercapacitor performance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160713 |
|
| RJ01 | Rejection of invention patent application after publication |