CN103482615B - A kind of preparation method of spumescence Graphene-ZnO matrix material - Google Patents
A kind of preparation method of spumescence Graphene-ZnO matrix material Download PDFInfo
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- CN103482615B CN103482615B CN201310407118.1A CN201310407118A CN103482615B CN 103482615 B CN103482615 B CN 103482615B CN 201310407118 A CN201310407118 A CN 201310407118A CN 103482615 B CN103482615 B CN 103482615B
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Abstract
The present invention discloses a kind of preparation method of spumescence Graphene-ZnO matrix material, comprises the following steps: step one, material oxidation Graphene and zinc salt is mixed than soluble in water by certain mass; Step 2, graphene oxide to be separated by centrifugal or suction filtration by the liquid mixed in step one, and with water or alcohol washes clean; Step 3, the product obtained in step 2 is re-dispersed in the aqueous solution, subsequently product is carried out lyophilize process; Step 4, by step 3 obtain product thermal treatment under air or oxygen obtain spumescence Graphene-ZnO matrix material, wherein said thermal treatment temp is at 300-1050 degree Celsius, and heat treatment time was at 10 seconds-10 hours.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of preparation method of spumescence Graphene-ZnO matrix material.
Background technology
Nano zinc oxide material has good optical correlation character, has broad application prospects in electrode of solar battery material, lithium ion battery electrode material etc.Graphene is by a kind of carbon material with bi-dimensional cellular shape structure of monolayer carbon atomic arrangement, has excellent mechanical property, electric property.Meanwhile, Graphene has high specific surface area, can as the solid support material of nano material.Graphene-zinc oxide nanometer composite material while inhibited oxidation zinc nano material is reunited, can keep the advantageous property of material itself, is therefore widely studied.
This type of material is mainly Powdered at present, and dusty material needs bonding or compacting in use, loses the high-ratio surface performance of Graphene.Grapheme foam material has higher specific surface area character, thus may be used for preparing high performance composite.ACSAppl.Mater.Interfaces2013,5,3764-3769 disclose the preparation method of a kind of Graphene-ferric oxide aerogel, are first obtained the colloidal sol of Graphene-ferric oxide by hydrothermal method, then obtain aerogel by freeze-drying method.Report about spumescence Graphene-ZnO matrix material is not yet found, although aforesaid method can obtain Graphene-ferric oxide three-dimensional foam simultaneously, technique is comparatively complicated.In addition, the Graphene after hydrothermal reduction still has reunion to a certain degree.
Summary of the invention
For giving full play to the excellent properties of Graphene-ZnO nano matrix material, make up deficiency when powdery graphite alkene nano composite material is actual to be used, the invention provides a kind of preparation method of spumescence Graphene ZnO nano particulate composite, inhibit the reunion of Graphene, the inventive method can effectively reduce the grain-size of ZnO nano particle simultaneously.
The present invention is by the following technical solutions: a kind of spumescence Graphene-ZnO matrix material, will carry out after soluble in water to material oxidation Graphene and zinc salt mixing being separated, cleaning; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited is obtained after heat treated under air or oxygen a kind of spumescence Graphene-ZnO matrix material.
Described zinc salt is any one in zinc fluoride, zinc chloride, zinc bromide, zinc sulfate, zinc nitrate, zinc acetate or zinc phosphate.
Described thermal treatment temp is at 300-1050 degree Celsius.
Described heat treatment time was at 10 seconds-10 hours.
Described graphene oxide and the mass ratio of zinc salt are 1:10-100:1.
Described freezing dry process comprises and first graphene oxide is become solid-state with the mixing solutions of zinc salt by refrigeration compressor or liquid nitrogen freezing, makes water sublimed obtain graphene oxide-zinc salt foam subsequently under lower pressure.
Beneficial effect of the present invention:
The invention provides a kind of preparation method of spumescence Graphene-ZnO matrix material, products therefrom not only maintains the continuity of matrix material but also maintains the high-ratio surface of Graphene, is conducive to the every potential giving full play to Graphene-ZnO nano matrix material.In addition, to obtain ZnO nano particle size less, nanoparticle size less surface atom ratio is larger, more easily produces unique physical properties.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of the spumescence Graphene-ZnO matrix material that the embodiment of the present invention 1 obtains; Fig. 2 is the transmission electron microscope figure of the spumescence Graphene-ZnO matrix material that the embodiment of the present invention 1 obtains.
Embodiment:
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.According to following embodiment, can better understand the present invention.But concrete material proportion, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1
Material oxidation Graphene and zinc fluoride are respectively got 30mg to be dissolved in 60ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is added 60ml deionized water, and ultrasonic disperse is even again, then solution is carried out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in atmosphere 300 DEG C of insulations and within 10 hours, obtains spumescence Graphene-ZnO matrix material.
Carry out scanning electron microscope sign to product, as shown in Figure 1, visible matrix material is foam porosity to result.Carry out transmission electron microscope sign to product, as shown in Figure 2, visible ZnO nano is particle studded at graphenic surface for result, and ZnO particle size is about 5 nanometers.
Embodiment 2
Getting graphene oxide 10mg and zinc nitrate 20mg is dissolved in 30ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained to be re-dispersed in 30ml deionized water and to stir, then obtaining solution and obtain solid through liquid nitrogen freezing, transferred to subsequently in freeze drier and carry out lyophilize process;
The product obtained is heated in oxygen 500 DEG C of insulations and within 10 minutes, obtains spumescence Graphene-ZnO matrix material.
Gained sample microscopic sdIBM-2+2q.p.approach result is similar to Example 1.
Embodiment 3
Getting graphene oxide 100mg and zinc acetate 10mg is dissolved in 100ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 100ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in atmosphere 1050 DEG C of insulations and within 10 seconds, obtains spumescence Graphene-ZnO matrix material.
Gained sample microscopic sdIBM-2+2q.p.approach result is similar to Example 1.
Claims (4)
1. a preparation method for spumescence Graphene-ZnO matrix material, is characterized in that, will carry out after soluble in water to material oxidation Graphene and zinc salt mixing being separated, cleaning; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited is obtained after heat treated under air or oxygen a kind of spumescence Graphene-ZnO matrix material; Described thermal treatment temp is at 300-1050 degree Celsius.
2. the preparation method of a kind of spumescence Graphene-ZnO matrix material according to claim 1, it is characterized in that, described zinc salt is any one in zinc fluoride, zinc chloride, zinc bromide, zinc sulfate, zinc nitrate, zinc acetate or zinc phosphate.
3. the preparation method of a kind of spumescence Graphene-ZnO matrix material according to claim 1, it is characterized in that, described heat treatment time was at 10 seconds-10 hours.
4. the preparation method of a kind of spumescence Graphene-ZnO matrix material according to claim 1, it is characterized in that, described graphene oxide and the mass ratio of zinc salt are 1:10-100:1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104098089B (en) * | 2014-07-25 | 2015-11-11 | 西南民族大学 | A kind of preparation method of doped graphene foam |
| CN104807861B (en) * | 2015-04-09 | 2017-05-24 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN105967286B (en) * | 2016-06-24 | 2019-04-30 | 华东师范大学 | A kind of preparation method of graphene hydridization cavernous body capacitive desalination electrode |
| CN107236148B (en) * | 2017-05-03 | 2019-06-11 | 中国石油天然气股份有限公司 | A kind of composite material and preparation method of graphene and polyolefin |
| CN108239358B (en) * | 2018-02-26 | 2020-12-18 | 深圳市友晖电子科技有限公司 | Zinc oxide/graphene composite material modified PVC (polyvinyl chloride) profile and preparation method thereof |
| CN108627554B (en) * | 2018-05-09 | 2021-01-12 | 东莞理工学院 | Modified electrode for glucose sensor and preparation method thereof |
| CN114591600B (en) * | 2022-04-11 | 2022-12-13 | 中国科学院兰州化学物理研究所 | Preparation method of super-toughness high-wear-resistance MXene-based composite material |
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| CN103086371A (en) * | 2013-01-24 | 2013-05-08 | 东南大学 | Method for preparing hydrophobic graphene sponge |
| CN103252228A (en) * | 2013-06-08 | 2013-08-21 | 江苏悦达墨特瑞新材料科技有限公司 | Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet |
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