CN103482616A - Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material - Google Patents
Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material Download PDFInfo
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- CN103482616A CN103482616A CN201310407655.6A CN201310407655A CN103482616A CN 103482616 A CN103482616 A CN 103482616A CN 201310407655 A CN201310407655 A CN 201310407655A CN 103482616 A CN103482616 A CN 103482616A
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Abstract
The invention discloses a graphene-tin dioxide nanoparticle three-dimensional foam composite material and a preparation method thereof. The preparation method comprises the following steps: step 1) dissolving raw materials, namely graphene oxide and tin tetrachloride, in water according to a certain mass ratio and uniformly mixing; step 2): separating the graphene oxide from the well mixed liquid, obtained in the step 1, by centrifugation or suction filtration and washing with water or alcohol; step 3) re-dispersing the product, obtained in the step 2, into a water solution, and then performing freeze-drying treatment on the product; and step 4) performing heat treatment on the product, obtained in the step 3, in a vacuum state, air or a specific atmosphere to get the graphene-tin dioxide nanoparticle three-dimensional foam composite material, wherein the specific atmosphere is one of nitrogen, argon or hydrogen, the heat treatment temperature is 100-1500 DEG C, and the heat treatment time is 2s-10h. The product disclosed by the invention is micro-porous and can be used for the fields of energy storage, gas sensing and the like.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of Graphene-tin oxide nano particles three-dimensional foam matrix material and preparation method thereof.
Background technology
Tindioxide has broad application prospects at aspects such as gas sensing, stored energy, photochemical catalysis, and the tin oxide nano particles specific surface area is high, has obvious dimensional effect and quantum tunneling effect, and its properties can be more excellent than macroscopic material.But nano particle is easily reunited usually, has restricted its practical application.Graphene has good mechanical property and electric property, and simultaneously, Graphene has high specific surface area, is the good solid support material of nano particle.Tin oxide nano particles and Graphene is compound, can suppress the reunion of tin oxide nano particles, keep the excellent properties of tin oxide nano particles.
Graphene-tin oxide nano particles matrix material is mainly Powdered or sheet at present, dusty material needs bonding or compacting in use, and flaky material has partly been lost the high-ratio surface performance of Graphene, the present invention is the shortcoming that overcomes above-mentioned form matrix material, it is prepared into to three-dimensional porous structure, not only keep the continuity of matrix material but also safeguarded the high-ratio surface of Graphene, be conducive to give full play to every potential of Graphene-stannic oxide nanometer matrix material.
Summary of the invention
For giving full play to the excellent properties of Graphene-stannic oxide nanometer matrix material, deficiency while making up Powdered and the actual use of flake graphite alkene-stannic oxide nanometer matrix material, the invention provides a kind of Graphene-preparation method of tin oxide nano particles matrix material and can obtain the material of three-dimensional foam shape, two kinds of reagent of aerobic functionalized graphene and tin tetrachloride only, without other chemical reagent, not only simplified technique but also reduced production cost.
The present invention is by the following technical solutions: the preparation method of a kind of Graphene-tin oxide nano particles three-dimensional foam matrix material, separated, clean after mixing feed oxygen functionalized graphene and tin tetrachloride are soluble in water; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited heat treated under vacuum, air, nitrogen, argon gas or hydrogen atmosphere is obtained to Graphene-tin oxide nano particles three-dimensional foam matrix material.
Graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
At first described freezing dry process comprises the mixing solutions of graphene oxide and tin tetrachloride is become to solid-state by refrigeration compressor or liquid nitrogen freezing, under the low pressure condition, makes subsequently water sublimed obtain graphene oxide-pink salt three-dimensional foam.
Described thermal treatment temp is at 100-1500 degree centigrade.
Heat treatment time was at 2 seconds-10 hours.
Beneficial effect of the present invention: traditional Graphene-tindioxide matrix material is Powdered or the filter paper shape, and product of the present invention is the three-dimensional foam shape, has expanded the macroscopic form of Graphene-stannic oxide nanometer matrix material; On the other hand, this preparation method is simple, and required chemical reagent kind is few, environmental protection.
The accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of the Graphene that obtains of the embodiment of the present invention 1-tin oxide nano particles three-dimensional foam matrix material;
Fig. 2 is the transmission electron microscope figure of the Graphene that obtains of the embodiment of the present invention 1-tin oxide nano particles three-dimensional foam matrix material.
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.
Embodiment 1
Feed oxygen functionalized graphene and tin tetrachloride are respectively got to 20mg and be dissolved in the 50ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained is re-dispersed in the 50ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated to 800 ℃ of insulations in a vacuum and within 10 minutes, obtains Graphene-tin oxide nano particles three-dimensional foam matrix material.
Product is carried out to the scanning electron microscope sign, and as shown in Figure 1, visible matrix material is vesicular structure to result.Product is carried out to the transmission electron microscope sign, and result as shown in Figure 2, finds that the tin oxide nano particles size is less than 10 nanometers.
Embodiment 2
Get graphene oxide 10mg and tin tetrachloride 1mg 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, and the container that then will hold solution immerses and to be frozen into solid-stately in liquid nitrogen, puts into subsequently freeze drier and carries out the low-temperature negative-pressure drying treatment;
The product obtained is heated to 100 ℃ of insulations in air and within 10 hours, obtains Graphene-tin oxide nano particles three-dimensional foam matrix material.
Acquired results is similar to Example 1.
Embodiment 3
Get graphene oxide 1mg and tin tetrachloride 10mg 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 10ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated to 1500 ℃ of insulations in nitrogen environment and within 2 seconds, obtains Graphene-tin oxide nano particles three-dimensional foam matrix material.
Acquired results is similar to Example 1.
Embodiment 4
Get graphene oxide 100mg and tin tetrachloride 1mg and be dissolved in the 100ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in the 50ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated to 1200 ℃ of insulations in hydrogen environment and within 5 seconds, obtains Graphene-tin oxide nano particles three-dimensional foam matrix material.
Acquired results is similar to Example 1.
Claims (4)
1. the preparation method of Graphene-tin oxide nano particles three-dimensional foam matrix material, is characterized in that, separated, cleans after mixing feed oxygen functionalized graphene and tin tetrachloride are soluble in water; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited heat treated under vacuum, air, nitrogen, argon gas or hydrogen atmosphere is obtained to Graphene-tin oxide nano particles three-dimensional foam matrix material.
2. the preparation method of Graphene according to claim 1-tin oxide nano particles three-dimensional foam matrix material, is characterized in that, graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
3. the preparation method of Graphene according to claim 1-tin oxide nano particles three-dimensional foam matrix material, is characterized in that, described thermal treatment temp is at 100-1500 degree centigrade.
4. the preparation method of Graphene according to claim 1-tin oxide nano particles three-dimensional foam matrix material, is characterized in that, heat treatment time was at 2 seconds-10 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104900859A (en) * | 2015-06-01 | 2015-09-09 | 合肥工业大学 | Porous SnO2 nano ball/graphene composite material and preparation method thereof |
| CN106990142A (en) * | 2017-05-09 | 2017-07-28 | 大连理工大学 | A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof |
| CN109142627A (en) * | 2018-08-01 | 2019-01-04 | 济南大学 | A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material |
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| 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 |
| CN102324502A (en) * | 2011-09-14 | 2012-01-18 | 重庆大学 | Preparation method of flower-like tin dioxide and graphene composite material |
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2013
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Patent Citations (2)
| 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 |
| CN102324502A (en) * | 2011-09-14 | 2012-01-18 | 重庆大学 | Preparation method of flower-like tin dioxide and graphene composite material |
Non-Patent Citations (3)
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| JUNFEI LIANG ET AL.: "Facile one-step synthesis of a 3D macroscopic SnO2–graphene aerogel and its application as a superior anode material for Li-ion batteries", 《THE ROYAL SOCIETY OF CHEMISTRY》 * |
| ZHIFENG DU ET AL.: "In situ synthesis of SnO2/graphene nanocomposite and their application as anode material for lithium ion battery", 《MATERIALS LETTERS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104900859A (en) * | 2015-06-01 | 2015-09-09 | 合肥工业大学 | Porous SnO2 nano ball/graphene composite material and preparation method thereof |
| CN106990142A (en) * | 2017-05-09 | 2017-07-28 | 大连理工大学 | A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof |
| CN109142627A (en) * | 2018-08-01 | 2019-01-04 | 济南大学 | A kind of preparation method of three-dimensional hierarchical structure graphene composite tin oxide nanosheet gas-sensitive material |
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| CN103482616B (en) | 2015-06-03 |
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