CN103482616B - 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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- CN103482616B CN103482616B CN201310407655.6A CN201310407655A CN103482616B CN 103482616 B CN103482616 B CN 103482616B CN 201310407655 A CN201310407655 A CN 201310407655A CN 103482616 B CN103482616 B CN 103482616B
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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 dioxide nanoparticle three-dimensional foam composite material and preparation method thereof.
Background technology
Tindioxide has broad application prospects in gas sensing, stored energy, photochemical catalysis etc., and 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, constrain its practical application.Graphene has excellent mechanical property and electric property, and meanwhile, Graphene has high specific surface area, is the excellent solid support material of nano particle.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.
Current graphene-tin dioxide nanoparticle composite material is mainly Powdered or sheet, dusty material needs bonding or compacting in use, and sheet material portion loses the high-ratio surface performance of Graphene, the present invention is the shortcoming overcoming above-mentioned form matrix material, be prepared into three-dimensional porous structure, not only maintain the continuity of matrix material but also maintain the high-ratio surface of Graphene, be conducive to the every potential giving full play to 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, make up deficiency during Powdered use actual in flake graphite alkene-stannic oxide nanometer matrix material, the preparation method that the invention provides a kind of graphene-tin dioxide nanoparticle composite material can obtain the material of three-dimensional foam shape, only aerobic functionalized graphene and tin tetrachloride two kinds of reagent, without the need to other chemical reagent, both simplified technique and again reduced production cost.
The present invention is by the following technical solutions: a kind of preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material, will carry out after soluble in water to material oxidation Graphene and tin tetrachloride mixing being separated, cleaning; 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 graphene-tin dioxide nanoparticle three-dimensional foam composite material.
Graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
Described freezing dry process comprises and first graphene oxide is become solid-state with the mixing solutions of tin tetrachloride by refrigeration compressor or liquid nitrogen freezing, makes water sublimed obtain graphene oxide-pink salt three-dimensional foam subsequently under lower pressure.
Described thermal treatment temp is at 100-1500 degree Celsius.
Heat treatment time was at 2 seconds-10 hours.
Beneficial effect of the present invention: traditional Graphene-tin dioxide composite material is Powdered or filter paper shape, and product of the present invention is 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.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of the graphene-tin dioxide nanoparticle three-dimensional foam composite material that the embodiment of the present invention 1 obtains;
Fig. 2 is the transmission electron microscope figure of the graphene-tin dioxide nanoparticle three-dimensional foam composite 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 tin tetrachloride are respectively got 20mg to be dissolved in 50ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained is re-dispersed in 50ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in a vacuum 800 DEG C of insulations and obtains graphene-tin dioxide nanoparticle three-dimensional foam composite material in 10 minutes.
Carry out scanning electron microscope sign to product, as shown in Figure 1, visible matrix material is vesicular structure to result.Carry out transmission electron microscope sign to product, result as shown in Figure 2, finds that tin oxide nano particles size is less than 10 nanometers.
Embodiment 2
Getting graphene oxide 10mg and tin tetrachloride 1mg 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, then the container holding solution is immersed in liquid nitrogen and carry out being frozen into solid-state, put into freeze drier subsequently and carry out low-temperature negative-pressure drying treatment;
The product obtained is heated in atmosphere 100 DEG C of insulations and obtains graphene-tin dioxide nanoparticle three-dimensional foam composite material in 10 hours.
Acquired results is similar to Example 1.
Embodiment 3
Getting graphene oxide 1mg and tin tetrachloride 10mg is dissolved in 20ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 10ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in nitrogen environment 1500 DEG C of insulations and obtains graphene-tin dioxide nanoparticle three-dimensional foam composite material in 2 seconds.
Acquired results is similar to Example 1.
Embodiment 4
Getting graphene oxide 100mg and tin tetrachloride 1mg is dissolved in 100ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 50ml deionized water, then carries out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in the hydrogen gas atmosphere 1200 DEG C of insulations and obtains graphene-tin dioxide nanoparticle three-dimensional foam composite material in 5 seconds.
Acquired results is similar to Example 1.
Claims (4)
1. a preparation method for graphene-tin dioxide nanoparticle three-dimensional foam composite material, is characterized in that, will carry out after soluble in water to material oxidation Graphene and tin tetrachloride mixing being separated, cleaning; 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 graphene-tin dioxide nanoparticle three-dimensional foam composite material.
2. the preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material according to claim 1, is characterized in that, graphene oxide and tin tetrachloride mass ratio are 1:10-100:1.
3. the preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material according to claim 1, is characterized in that, described thermal treatment temp is at 100-1500 degree Celsius.
4. the preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material according to claim 1, is characterized in that, heat treatment time was at 2 seconds-10 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310407655.6A CN103482616B (en) | 2013-09-09 | 2013-09-09 | Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material |
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| CN201310407655.6A CN103482616B (en) | 2013-09-09 | 2013-09-09 | Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material |
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| CN103482616B true CN103482616B (en) | 2015-06-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104900859B (en) * | 2015-06-01 | 2017-08-11 | 合肥工业大学 | A kind of porous SnO2Nanosphere/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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| CN102255072B (en) * | 2010-05-17 | 2014-06-18 | 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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