CN103482617A - Method for preparing tin dioxide/graphene composite material - Google Patents

Method for preparing tin dioxide/graphene composite material Download PDF

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CN103482617A
CN103482617A CN201310407762.9A CN201310407762A CN103482617A CN 103482617 A CN103482617 A CN 103482617A CN 201310407762 A CN201310407762 A CN 201310407762A CN 103482617 A CN103482617 A CN 103482617A
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composite material
graphene composite
graphene
tindioxide
graphene oxide
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CN201310407762.9A
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CN103482617B (en
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尹奎波
季静
孙立涛
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Southeast University
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Southeast University
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Abstract

The invention discloses a method for preparing a tin dioxide/graphene composite material. The method comprises the steps of (1) dissolving raw materials, namely graphene oxide and tin tetrachloride, into water according to a certain mass ratio, and mixing uniformly; (2) separating graphene oxide from mixed liquid obtained in the step (1) through centrifugation or suction filtration, and cleanly cleaning graphene oxide by using water or alcohol; (3) dispersing a product obtained in the step (2) into water again, and then, adding a reducing agent for treatment, thereby obtaining the tin dioxide/graphene composite material, wherein the reducing agent contains hydrazine hydrate, sodium borohydride, sodium hydroxide and the like. The method disclosed by the invention has the advantages that the method is simple, energy-saving and environmental-friendly, the cost is low, and the high-temperature heat treatment process is avoided.

Description

A kind of preparation method of tindioxide/graphene composite material
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 a kind of carbon material with bi-dimensional cellular shape structure formed by the monolayer carbon atomic arrangement, has good mechanical property, electric property.Simultaneously, Graphene has high specific surface area, is suitable as very much the carrier of nano material.Tindioxide is a kind of multifunctional material, at aspects such as gas sensing, stored energy, photochemical catalysis, has broad application prospects.The 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, has restricted its practical application.Tin oxide nano particles and Graphene is compound, can suppress the reunion of tin oxide nano particles, the excellent properties that keeps tin oxide nano particles, research at present shows that tindioxide/graphene composite material has higher application potential in the lithium ion battery negative field.
The preparation method of tindioxide/graphene composite material is comparatively complicated at present, usually needs high-temperature water thermal response or high temperature reflux experiment.These techniques are comparatively complicated, and the required equipment cost is higher.
Summary of the invention
In order to reduce the preparation cost of tindioxide/graphene composite material, simplify preparation technology, the invention provides a kind of preparation method of new tindioxide/graphene composite material, not only reduce cost simultaneously but also can guarantee the nano-scale of tindioxide.
The present invention is by the following technical solutions: a kind of preparation method of tindioxide/graphene composite material again is dispersed in water the reduction through reductive agent after being separated, clean after mixing again and obtains tindioxide/graphene composite material feed oxygen functionalized graphene and tin tetrachloride are soluble in water.
Described reductive agent is any 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: pyroreaction link of the present invention, institute all at room temperature carries out in steps, and method is simple, can effectively reduce energy consumption, has reduced production cost, and resulting materials is at nanoscale.
The accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of tindioxide/graphene composite material of obtaining of the embodiment of the present invention 1;
Fig. 2 is the selected area electron diffraction figure of tindioxide/graphene composite material of obtaining of the embodiment of the present invention 2.
Embodiment:
Below in conjunction with embodiment and accompanying drawing, the present invention is done further and explains.According to following embodiment, can better understand the present invention.Yet the described concrete material proportion of embodiment, processing condition and result thereof be only for the present invention is described, and should can not limit the present invention described in detail in claims yet.
A kind of preparation method of tindioxide/graphene composite material, concrete steps are:
Step 1, feed oxygen functionalized graphene and tin tetrachloride are mixed than soluble in water by certain mass;
Step 2, the liquid mixed in step 1 is separated graphene oxide by centrifugal or suction filtration, and water or alcohol clean up;
Step 3, the product obtained in step 2 is re-dispersed in water, then adds reductive agent to process and obtain tindioxide/graphene composite material, wherein said reductive agent comprises: hydrazine hydrate, sodium borohydride, sodium hydroxide etc.
Embodiment 1
Feed oxygen functionalized graphene and tin tetrachloride are respectively got to 10mg and be dissolved in the 20ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained is re-dispersed in the 10ml deionized water, adds after hydrazine hydrate 0.5ml and stir and within 10 minutes, obtain tindioxide/graphene composite material.
Product is carried out to the transmission electron microscope sign, and as shown in Figure 1, visible tin oxide nano particles size is 5 nanometers approximately for result.Product is carried out to selected area electron diffraction analysis, and as shown in Figure 2, the associated diffraction ring is tindioxide crystalline diffraction peak to result, illustrates that the nano particle that present method obtains is the tindioxide crystal.
Embodiment 2
Get graphene oxide 1mg and tin tetrachloride 10mg and be dissolved in the 10ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in the 10ml deionized water, adds after sodium borohydride 50mg and stir and within 30 minutes, obtain tindioxide/graphene composite material.
Products therefrom pattern and structure are similar to Example 1.
Embodiment 3
Get graphene oxide 10mg and tin tetrachloride 1mg and be dissolved in the 20ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in the 20ml deionized water, adds the ultrasonic dispersion of sodium hydroxide 100mg within 20 minutes, to obtain tindioxide/graphene composite material.
Products therefrom pattern and structure are similar to Example 1.

Claims (3)

1. the preparation method of a tindioxide/graphene composite material, it is characterized in that, again be dispersed in water again the reduction through reductive agent after being separated, clean after mixing and obtain tindioxide/graphene composite material feed oxygen functionalized graphene and tin tetrachloride are soluble in water.
2. the preparation method of tindioxide/graphene composite material according to claim 1, it is characterized in that, described reductive agent is any 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.
3. 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.
CN201310407762.9A 2013-09-09 2013-09-09 A kind of preparation method of tindioxide/graphene composite material Active CN103482617B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104852022A (en) * 2015-03-27 2015-08-19 上海大学 Cathode material for lithium ion battery and preparation method thereof
CN105289657A (en) * 2015-11-30 2016-02-03 湘潭大学 Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst
CN107055516A (en) * 2017-04-12 2017-08-18 大连理工大学 A kind of preparation method of graphene/tin dioxide quantal-point composite
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104852022A (en) * 2015-03-27 2015-08-19 上海大学 Cathode material for lithium ion battery and preparation method thereof
CN104852022B (en) * 2015-03-27 2017-03-15 上海大学 A kind of lithium ion battery negative material and preparation method thereof
CN105289657A (en) * 2015-11-30 2016-02-03 湘潭大学 Preparation method for graphene and antimony sulphide nano-rod composite visible light catalyst
CN107055516A (en) * 2017-04-12 2017-08-18 大连理工大学 A kind of preparation method of graphene/tin dioxide quantal-point composite
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

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