CN103482617B - A kind of preparation method of tindioxide/graphene composite material - Google Patents
A kind of preparation method of tindioxide/graphene composite material Download PDFInfo
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- CN103482617B CN103482617B CN201310407762.9A CN201310407762A CN103482617B CN 103482617 B CN103482617 B CN 103482617B CN 201310407762 A CN201310407762 A CN 201310407762A CN 103482617 B CN103482617 B CN 103482617B
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Abstract
The present invention discloses a kind of preparation method of tindioxide/graphene composite material, comprises the following steps: step one, material oxidation Graphene and tin tetrachloride 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, be re-dispersed in water by the product obtained in step 2, then add reductive agent process and obtain tindioxide/graphene composite material, wherein said reductive agent comprises: hydrazine hydrate, sodium borohydride, sodium hydroxide etc.Preparation method of the present invention is simple, with low cost, avoids high-temperature heat treatment process, energy-conserving and environment-protective.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of preparation method of tindioxide/graphene composite material.
Background technology
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, is suitable as very much the carrier of nano material.Tindioxide is a kind of multifunctional material, has broad application prospects in gas sensing, stored energy, photochemical catalysis etc.Tin oxide nano particles specific surface area is high, has dimensional effect and quantum tunneling effect, and its every property can be more excellent than macroscopic material.But nano particle is easily reunited usually, constrain its practical application.By tin oxide nano particles and Graphene compound, the reunion of tin oxide nano particles can be suppressed, keep the excellent properties of tin oxide nano particles, research at present shows that tindioxide/graphene composite material has higher application potential in lithium ion battery negative field.
The preparation method of current tindioxide/graphene composite material is comparatively complicated, usually needs high-temperature water thermal response or high temperature reflux experiment.These techniques are comparatively complicated, and required equipment cost is higher.
Summary of the invention
In order to reduce the preparation cost of tindioxide/graphene composite material, simplifying preparation technology, the invention provides a kind of preparation method of new tindioxide/graphene composite material, not only reduced cost simultaneously but also the nano-scale of tindioxide can be ensured.
The present invention is by the following technical solutions: a kind of preparation method of tindioxide/graphene composite material, obtains tindioxide/graphene composite material by being again dispersed in water after carrying out after soluble in water to material oxidation Graphene and tin tetrachloride mixing being separated, cleaning through reductive agent reduction again.
Described reductive agent is any one in hydrazine hydrate, sodium borohydride, sodium hydroxide, and the quality of reductive agent and the mass ratio of graphene oxide are 0.5:10-50:1.
Graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
Beneficial effect of the present invention: present invention, avoiding pyroreaction link, institute all at room temperature carries out in steps, and method is simple, and effectively can reduce energy consumption, reduce production cost, resulting materials is at nanoscale.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of tindioxide/graphene composite material that the embodiment of the present invention 1 obtains;
Fig. 2 is the selected area electron diffraction figure of tindioxide/graphene composite material that the embodiment of the present invention 2 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.
A preparation method for tindioxide/graphene composite material, concrete steps are:
Step one, material oxidation Graphene and tin tetrachloride to be 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, be re-dispersed in water by the product obtained in step 2, then add reductive agent process and obtain tindioxide/graphene composite material, wherein said reductive agent comprises: hydrazine hydrate, sodium borohydride, sodium hydroxide etc.
Embodiment 1
Material oxidation Graphene and tin tetrachloride are respectively got 10mg to be dissolved in 20ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained is re-dispersed in 10ml deionized water, stirs after adding hydrazine hydrate 0.5ml and obtain tindioxide/graphene composite material in 10 minutes.
Transmission electron microscope sign is carried out to product, result as shown in Figure 1, visible tin oxide nano particles size about 5 nanometer.Carry out selected area electron diffraction analysis to product, as shown in Figure 2, associated diffraction ring is tindioxide crystalline diffraction peak to result, illustrates that the nano particle that present method obtains is tindioxide crystal.
Embodiment 2
Getting graphene oxide 1mg and tin tetrachloride 10mg is dissolved in 10ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 10ml deionized water, stirs after adding sodium borohydride 50mg and obtain tindioxide/graphene composite material in 30 minutes.
Products therefrom pattern and structure similar to Example 1.
Embodiment 3
Getting graphene oxide 10mg and tin tetrachloride 1mg is dissolved in 20ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 20ml deionized water, adds sodium hydroxide 100mg ultrasonic disperse and obtain tindioxide/graphene composite material in 20 minutes.
Products therefrom pattern and structure similar to Example 1.
Claims (2)
1. the preparation method of tindioxide/graphene composite material, it is characterized in that, under room temperature, obtain tindioxide/graphene composite material by being again dispersed in water again after carrying out after soluble in water to material oxidation Graphene and tin tetrachloride mixing being separated, cleaning through reductive agent reduction; Described reductive agent is any one in hydrazine hydrate, sodium borohydride, sodium hydroxide, and the quality of reductive agent and the mass ratio of graphene oxide are 0.5:10-50:1.
2. the preparation method of tindioxide/graphene composite material according to claim 1, is characterized in that, graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
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| CN201310407762.9A CN103482617B (en) | 2013-09-09 | 2013-09-09 | A kind of preparation method of tindioxide/graphene composite material |
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| CN201310407762.9A CN103482617B (en) | 2013-09-09 | 2013-09-09 | A kind of preparation method of tindioxide/graphene composite material |
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| CN103482617B true CN103482617B (en) | 2016-01-13 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104852022B (en) * | 2015-03-27 | 2017-03-15 | 上海大学 | A kind of lithium ion battery negative material and preparation method thereof |
| CN105289657B (en) * | 2015-11-30 | 2018-02-06 | 湘潭大学 | The preparation method of graphene antimony sulfide nano rod composite visible light catalyst |
| CN107055516B (en) * | 2017-04-12 | 2019-04-12 | 大连理工大学 | A kind of preparation method of graphene/tin dioxide quantal-point composite material |
| CN107522895A (en) * | 2017-08-08 | 2017-12-29 | 东南大学 | A kind of gentle method for preparing graphene polyurethane sponge composite |
| CN112573508A (en) * | 2020-12-28 | 2021-03-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of graphene-coated core-shell stannous oxide @ tin oxide material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255072A (en) * | 2010-05-17 | 2011-11-23 | 国家纳米科学中心 | Preparation method of stannic oxide or metallic tin and grapheme lamella composite material |
| CN102778478A (en) * | 2012-05-15 | 2012-11-14 | 中国科学技术大学 | Graphene-modified doped tin oxide composite material and preparation method thereof |
| CN103094539A (en) * | 2012-11-28 | 2013-05-08 | 上海大学 | Preparation method of tin dioxide quantum dot graphene sheet composite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255072A (en) * | 2010-05-17 | 2011-11-23 | 国家纳米科学中心 | Preparation method of stannic oxide or metallic tin and grapheme lamella composite material |
| CN102778478A (en) * | 2012-05-15 | 2012-11-14 | 中国科学技术大学 | Graphene-modified doped tin oxide composite material and preparation method thereof |
| CN103094539A (en) * | 2012-11-28 | 2013-05-08 | 上海大学 | Preparation method of tin dioxide quantum dot graphene sheet composite |
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