CN103035916A - Preparation method of nano tin dioxide-graphene composite material and product thereof - Google Patents
Preparation method of nano tin dioxide-graphene composite material and product thereof Download PDFInfo
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- CN103035916A CN103035916A CN2012104946210A CN201210494621A CN103035916A CN 103035916 A CN103035916 A CN 103035916A CN 2012104946210 A CN2012104946210 A CN 2012104946210A CN 201210494621 A CN201210494621 A CN 201210494621A CN 103035916 A CN103035916 A CN 103035916A
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Abstract
The invention discloses a method for preparing a nano tin dioxide-graphene composite material, which comprises the following steps: (a) sequentially adding graphene oxide and stannous dichloride into deionized water, and mixing, thereby obtaining a graphene oxide-tin dioxide precursor mixed solution, wherein 57-374mg of graphene oxide and 10-24mg of stannous dichloride are added to every 100ml of deionized water; (b) carrying out ultrasonic reaction on the mixed solution at a certain temperature, wherein the ultrasonic power is 100-300W; and (c) carrying out vacuum filtration and cleaning on the suspension subjected to ultrasonic treatment, thereby obtaining the composite material product. The invention also discloses a corresponding composite material product and main application thereof. The invention can effectively avoid environmental pollution in the production process, lowers the production cost and energy consumption, and is beneficial to enhancing the reaction efficiency and enabling the reaction process to be more sufficient; and the prepared composite material product has better comprehensive properties.
Description
Technical field
The invention belongs to the Nano-composite materials field, more specifically, relate to preparation method of a kind of nano-stannic oxide-graphene composite material and products thereof.
Background technology
Graphene be carbon atom with the tightly packed cellular Colloidal particles carbon nanomaterial that forms of sp2 hybrid systems, it has good electricity, mechanics and thermal property, is the energy storage material that has at present potentiality.Graphene-based composite material refers to utilize surface modifier, conducting polymer or transition metal oxide particle etc., by surface reaction Graphene is carried out the composite material that obtains after the finishing, its source is abundant and embody good performance index, is the electrode material of the element first-selection such as ultracapacitor.Studies show that, to possess positive tetrahedron Rutile structure, tin ash that physicochemical properties are stable and evenly be attached to the hardness that composite material that the Graphene particle surface consists of can obviously improve material, and strengthen the performances such as electrochemistry capacitance, conductance, therefore obtained in a plurality of fields such as ultracapacitor, information material, lithium ion battery, solar cell and fuel cells to use more and more widely.
Method for the preparation of tin ash-graphene composite material of the prior art for example comprises the preparation method of disclosed a kind of flower-like tin dioxide and graphene composite material among the CN102324502A, wherein utilize hydro thermal method take stannic chloride pentahydrate, NaOH and graphene oxide as raw material, water is solvent, stir and carry out hydro-thermal reaction after 60 minutes, generated thus tin ash and graphene composite material.Among the CN101927979A a kind of tin oxide/graphene nanometer composite and its preparation method and application is disclosed and for example, the method is take stannic chloride pentahydrate or two hydration stannous chloride, NaOH and graphene oxide as raw material, methyl-sulfoxide is solvent, stir and carry out hydro-thermal reaction after 2.5 hours, generated tin ash and graphene composite material.Above-mentioned preparation method's defective mainly is: (1) has used the materials such as alkaline NaOH or methyl-sulfoxide in preparation process, is unfavorable for environmental protection and increases production cost; (2) hydro-thermal reaction needs the high-temperature heating of long period, and energy consumption height and production efficiency are on the low side.
In addition; a kind of tin ash or metallic tin and graphene sheet layer composite manufacture method are also disclosed among the CN102255072A; wherein with organic solvent, the graphene oxide lamella hydrosol and after pink salt mixes; at 60-200 ℃ of lower heating 0.5-12h; obtain solid matter; the gained solid matter is heated 0.5-10h under the inert gas shielding under 400-700 ℃ temperature, thereby making tin ash and graphene sheet layer composite material.The defective of the method mainly is: (1) equally with an organic solvent, it is unfavorable for environmental protection and has increased production cost in preparation process; (2) owing to need to react under higher reaction temperature condition, energy consumption is higher and stricter to equipment requirement; (3) whole reaction will be carried out under inert gas shielding, the corresponding requirement that improves the production control aspect, and further improved manufacturing cost.Therefore, the preparation method who exists in association area tin ash-graphene composite material makes further improved technical need.
Summary of the invention
Above defective and/or technical need for prior art, the object of the present invention is to provide preparation method of a kind of nano-stannic oxide-graphene composite material and products thereof, it is by research and improvement to key reaction thing and reaction condition thereof, can be beneficial to environmental protection, be convenient to quality control and high efficiency mode prepares tin ash-graphene composite material product, and its prepared product stannic oxide particle average diameter is 5-8nm and is uniformly distributed in the Graphene surface, and electric capacity possesses better cycle performance simultaneously up to more than the 120F/g.
According to one aspect of the present invention, a kind of method for the preparation of nano-stannic oxide-graphene composite material is provided, it is characterized in that the method comprises the following steps:
(a) take deionized water as solvent, priority adds as the graphene oxide of solute and the inferior tin of dichloro and carries out mix and blend, charge ratio is controlled to be in every 100ml deionized water, the mass ratio of the inferior tin of graphene oxide and dichloro is 57~374mg:10~24mg, obtains thus the mixed solution of graphene oxide-tin ash presoma;
(b) with the mixed solution that obtains ultrasonic reaction 1~2 hour under 25 ℃~40 ℃ temperature, ultrasonic power is set to 100~300W;
(c) carry out suction filtration and process process resulting suspension through step (b), and resulting filter cake after adopting the washed with de-ionized water suction filtration to process, make thus the nano-stannic oxide that is chondritic-graphene composite material product.
By above design, owing to adopt graphene oxide and the inferior tin of dichloro to carry out oxidation-reduction reaction, Sn in course of reaction as the crucial thing of reaction
2+At first oxidized Graphene be adsorbed on its surface and by its oxidation, meanwhile graphene oxide is reduced into Graphene, in the set of Graphene adsorption the stannic oxide particle of nanometer scale is arranged like this, thereby make required tin ash=graphene composite material product.This course of reaction compared with prior art can effectively be avoided using there is the organic substance that pollutes in environment, and reduce production costs and improve reaction efficiency, and the stannic oxide particle that is adsorbed on the Graphene surface is evenly distributed, and its average-size is about 5-8nm; In addition, owing to adopt ultrasonic wave to process, with the hydro-thermal reaction phase specific energy raising reaction efficiency of prior art, and it is more abundant that whole course of reaction is carried out, and is conducive to reduce efficiency, and stannic oxide particle obtains on the Graphene surface to distribute more uniformly.
As further preferably, in step (c) afterwards, can also process the freeze drying of carrying out 12~72 hours through resulting solid after the washed with de-ionized water.
According to another aspect of the present invention, also provide corresponding nano-stannic oxide-graphene composite material product.
As further preferably, the average diameter of particles of nano-stannic oxide is about 5-8nm in the described composite products.
According to another aspect of the present invention, also provide prepared nano-stannic oxide-graphene composite material product in the purposes of the aspects such as ultracapacitor, field-effect transistor, lithium ion battery or fuel cell for example.
In general, according to preparation method of nano-stannic oxide-graphene composite material of the present invention and products thereof compared with prior art, mainly possess following technological merit:
1, by adopting the inferior tin of graphene oxide and dichloro to prepare tin ash-graphene composite material as the crucial thing of reaction and by the ultrasonic reaction mode, can effectively avoid using there is the organic substance that pollutes in environment, reduce production costs and energy consumption, help simultaneously to improve reaction efficiency, and so that course of reaction is more abundant;
2, by the aspects such as the charge ratio in the course of reaction, response parameter are selected, can form the stannic oxide particle of nanometer scale on the Graphene surface and be evenly distributed, prepared composite products shows better combination property;
3, whole preparation method's economy, environmental protection, and be convenient to quality control, and can be used for the large-scale industrialization batch production, therefore be particularly useful for making the purposes such as ultracapacitor, lithium ion battery negative, fuel cell electrode or field-effect transistor.
Description of drawings
Fig. 1 is according to the method flow diagram of the present invention for the preparation of nano-stannic oxide-graphene composite material;
Fig. 2 a is the transmission electron microscope photo according to the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product;
Fig. 2 b sweeps cyclic voltammetry curve under the speed according to the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product in difference;
Fig. 2 c is according to the constant current charge-discharge curve chart of the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product under the 1mA/mg current density;
Fig. 2 d is according to the constant current charge-discharge curve chart of the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product under the 2mA/mg current density;
Fig. 2 e is the X ray diffracting spectrum according to the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Fig. 1 is according to the method flow diagram of the present invention for the preparation of nano-stannic oxide-graphene composite material.As shown in fig. 1, in order to prepare tin ash-graphene composite material product, at first, take deionized water as solvent, priority adds as the graphene oxide of solute and the inferior tin of dichloro and carries out mix and blend, wherein charge ratio is controlled to be in every 100ml deionized water, and the mass ratio of the inferior tin of graphene oxide and dichloro is 57~374mg:10~24mg, obtains thus the mixed solution of graphene oxide-tin ash presoma; Then, with the mixed solution that obtains ultrasonic reaction 1~2 hour under 25 ℃~40 ℃ temperature, ultrasonic power is set to 100~300W; At last, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and resulting filter cake after adopting the washed with de-ionized water suction filtration to process, make thus the nano-stannic oxide that is chondritic-graphene composite material product.After making this composite products, can also process the freeze drying that this solid was carried out 12-72 hour.
Embodiment 1
In reaction vessel, add deionized water 80ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 106.7mg and 18.7mg as solute, then mix and blend obtains the mixed solution of graphene oxide and tin ash predecessor about 1 minute thus;
Then, be to carry out ultrasonic response 1.5 hours under the condition of 120W at 25 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 12 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
Embodiment 2
In reaction vessel, add deionized water 100ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 160mg and 10mg as solute, then mix and blend is 60 minutes, obtains thus the mixed solution of graphene oxide and tin ash predecessor;
Then, be to carry out ultrasonic response 2 hours under the condition of 280W at 40 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 60 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
In reaction vessel, add deionized water 80ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 372mg and 23.3mg as solute, then mix and blend is 60 minutes, obtains thus the mixed solution of graphene oxide and tin ash predecessor;
Then, be to carry out ultrasonic response 2 hours under the condition of 300W at 30 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 72 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
Embodiment 4
In reaction vessel, add deionized water 100ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 57mg and 10mg as solute, then mix and blend is 60 minutes, obtains thus the mixed solution of graphene oxide and tin ash predecessor;
Then, be to carry out ultrasonic response 1.5 hours under the condition of 100W at 35 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 72 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
Embodiment 5
In reaction vessel, add deionized water 80ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 45.7mg and 8mg as solute, then mix and blend is 60 minutes, obtains thus the mixed solution of graphene oxide and tin ash predecessor;
Then, be to carry out ultrasonic response 1 hour under the condition of 150W at 28 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 72 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
Embodiment 6
In reaction vessel, add deionized water 100ml as solvent, then to the inferior tin of the dichloro of the graphene oxide that wherein successively adds 57.1mg and 10mg as solute, then mix and blend is 30 minutes, obtains thus the mixed solution of graphene oxide and tin ash predecessor;
Then, be to carry out ultrasonic response 2 hours under the condition of 200W at 35 ℃, ultrasonic power with this mixed solution;
Then, process carrying out suction filtration through the resulting suspension of ultrasonic processing, and adopt the washed with de-ionized water suction filtration to process the rear resulting tin ash-Graphene that includes at interior filter cake, at last resulting solid freeze drying was processed 12 hours, made thus the nano-stannic oxide that substantially is chondritic-graphene composite material product.
The below will be take embodiment 1 prepared sample as example, introduces the composite products that obtains according to the present invention is analyzed and the process of Performance Detection.At first the nickel foam of sheet can be cut into about 1*2cm
2Size, then nickel foam is cleaned and activates: nickel foam was carried out ultrasonic cleaning 10 minutes with ethanol, then nickel foam was carried out ultrasonic cleaning 10 minutes with deionized water.After wash phase is finished, change nickel foam over to baking oven and under 100 ℃ condition, dried by the fire 30 minutes, remove the moisture of nickel foam absorption.Nano-stannic oxide-the graphene composite material that makes is downcut small pieces with blade, grind alms bowl at agate and mill, the sample bottle of packing into after evenly to be ground.On the nickel foam after assay balance takes by weighing this composite material 1.0mg and it is transferred to previous processed (for example, can under the pressure of 20Mpa, composite material be pressed onto on the nickel foam with infrared tablet press machine, the sheet active material difficult drop-off that this pressure is pressed also is difficult for nickel foam is broken simultaneously).Then just can adopt conventional three-electrode system, carry out the scanning of cyclic voltammetry scan and constant current charge-discharge.The nickel foam of composite material load is as work electrode, and the Pt electrode of light is as auxiliary electrode, and calomel electrode is as reference electrode.Electrolyte adopts the KOH solution of 0.1mol/L.For cyclic voltammetry scan, sweep speed is to test under the condition of 10mV/s, 20mV/s, 50mV/s, 100mV/s and 200mV/s.For constant current charge-discharge, under the condition of 1mA/mg and 2mA/mg, test.
Fig. 2 b is the cyclic voltammetry curve of this material, in sweep speed be to test under the condition of 10mV/s, 20mV/s, 50mV/s, 100mV/s and 200mV/s, its curve near the invertibity of rectangle illustrative material and capacitive character than more excellent.Galvanostatic charge/discharge is one of method of test capacitors capacity, in according to the constant current charge-discharge result of the prepared tin ash-graphene composite material of preparation method of the present invention by Fig. 2 c and 2d, can find out, this composite material single discharges and recharges the isosceles triangle that is approximate test and has reasonable symmetry, it is substantially constant that in time linear variation of voltage repeatedly discharges and recharges rear curve, this explanation electrode charge and discharge stable performance good reversibility electrode and electrolyte contact-making surface form reasonable charge accumulated and release, calculate the ratio electric capacity of electrode material for being about 212F/g according to discharge curve and formula.
Fig. 2 a and 2e are respectively transmission electron microscope photo (TEM) and the X ray diffracting spectrums (XRD) according to the embodiment of the invention 1 prepared nano-stannic oxide-graphene composite material product.Can find out that from 2a figure the average diameter of particles of nano-stannic oxide is about 5-8nm in this composite material.And be dispersed in uniformly on the Graphene surface.In addition, the XRD test of Fig. 2 e has proved that prepared composite material thing is in 2 θ=34.6 ° (101), 38.5 ° (200) and 52.1 ° (211) have located to occur the characteristic diffraction peak of tin ash different crystal forms of the correspondence of standard, these external 2 θ=26.6 ° of characteristic diffraction peaks that Graphene occurs.Integral composite presents good performance index.For example, when its as super capacitor material the time, its than electric capacity greater than traditional pure material with carbon element; When its during as lithium ion battery negative, possess the advantages such as charge/discharge capacity height, cycle performance; This composite material also can be used as the electrode, field-effect transistor of fuel cell etc., therefore possesses the potentiality of replacing the traditional devices material and application prospect widely.
Those skilled in the art will readily understand; the above only is preferred embodiment of the present invention; not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the method for the preparation of nano-stannic oxide-graphene composite material is characterized in that the method comprises the following steps:
(a) take deionized water as solvent, priority adds as the graphene oxide of solute and the inferior tin of dichloro and carries out mix and blend, charge ratio is controlled to be in every 100ml deionized water, the mass ratio of the inferior tin of graphene oxide and dichloro is 57~374mg:10~24mg, obtains thus the mixed solution of graphene oxide-tin ash presoma;
(b) with the mixed solution that obtains ultrasonic reaction 1~2 hour under 25 ℃~40 ℃ temperature, ultrasonic power is set to 100~300W;
(c) carry out suction filtration and process process resulting suspension through step (b), and resulting filter cake after adopting the washed with de-ionized water suction filtration to process, make thus the nano-stannic oxide that is chondritic-graphene composite material product.
2. the method for claim 1 is characterized in that, in step (c) afterwards, can also process carry out for example 12~72 hours freeze drying through resulting solid after the washed with de-ionized water.
3. the prepared nano-stannic oxide of method as claimed in claim 1 or 2-graphene composite material product.
4. composite products as claimed in claim 3 is characterized in that, wherein the average diameter of particles of nano-stannic oxide is about 5-8nm.
Such as claim 3 or 4 described nano-stannic oxide-graphene composite material products in the purposes of the aspects such as ultracapacitor, field-effect transistor, lithium ion battery or fuel cell for example.
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CN103326007A (en) * | 2013-06-25 | 2013-09-25 | 上海交通大学 | Preparation method and application of three-dimensional graphene-based stannic oxide composite material |
CN103995088A (en) * | 2014-05-26 | 2014-08-20 | 太原理工大学 | Preparation method and application of graphene/tin oxide nano composite material |
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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 |
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CN107124778A (en) * | 2017-05-03 | 2017-09-01 | 广州厨霸电器有限公司 | Far-infrared electrothermal film, the manufacture craft of far-infrared electrothermal film and electric heater |
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