CN102324502A - Preparation method of flower-like tin dioxide and graphene composite material - Google Patents
Preparation method of flower-like tin dioxide and graphene composite material Download PDFInfo
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- CN102324502A CN102324502A CN201110271670A CN201110271670A CN102324502A CN 102324502 A CN102324502 A CN 102324502A CN 201110271670 A CN201110271670 A CN 201110271670A CN 201110271670 A CN201110271670 A CN 201110271670A CN 102324502 A CN102324502 A CN 102324502A
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Abstract
The invention discloses a preparation method of a flower-like tin dioxide and graphene composite material, belonging to the technical field of functional composite materials. According to the preparation method disclosed by the invention, the flower-like tin dioxide and graphene composite material with controllable morphology is prepared from graphene oxide, tin chloride pentahydrate and sodium hydroxide as raw materials by adopting the steps of mixed stirring, hydro-thermal synthesis, solid-liquid separation, cleaning and drying. The method disclosed by the invention has the advantages of simpleness, convenience for operation, lower production cost, no influence on the environment and convenience for popularization and application; and in the method, water is used as solvent and no surfactant is used. The flower-like tin dioxide and graphene composite material prepared by adopting the method can be widely applied to new energy source devices such as a lithium ion battery, a solar cell, a super capacitor and the like, or can be applied to the fields of catalyst carriers, information materials and the like.
Description
Technical field
The invention belongs to the functional composite material technical field, be specifically related to the preparation method of flower-shaped tin ash and graphene composite material.
Background technology
Tin ash has the positive tetrahedron Rutile structure, and physics, chemical property are stablized, and be cheap, pollution-free, is a kind of semiconductor material with wide forbidden band that receives extensive attention.Graphene is by SP
2The two-dimensional material that the hydridization carbon atom is formed has bigger specific area, excellent conduction, heat conduction, mechanics, performances such as magnetics.Tin ash and Graphene recombination energy obviously improve the hardness of material, conductance, and performances such as electrochemistry capacitance can be widely used in fields such as lithium ion battery, solar cell, fuel cell, ultracapacitor and information material.
The preparation method of existing tin ash and graphene composite material; Like publication number is the patent of CN 101969113A " preparation method of graphene-based tin ash composite lithium ion battery cathode material ", and utilizing hydro thermal method is raw material with stannic chloride pentahydrate, NaOH and graphene oxide, and ethanol is solvent; Softex kw is a surfactant; Stir after 30 minutes, carry out hydro-thermal reaction, generated tin ash and graphene composite material.The major defect of this method is: (1) ethanol is solvent, and cost is higher; (2) use softex kw to be surfactant, be unfavorable for environmental protection and increase cost." the electrochemistry journal " of Britain " tin ash of high power capacity/graphene nano composite material is made the negative pole of lithium ion battery " (Electrochimica Acta and for example; 2011,56 (12): 4532-4539) disclosed Hydrothermal Preparation stannic oxide particle and the compound technology of Graphene in the literary composition.This method is a raw material with stannic chloride pentahydrate, ammoniacal liquor and graphene oxide, and ethylene glycol is solvent, and hydro-thermal reaction is carried out in ultrasonic dispersion after 6 hours, generated tin ash and graphene composite material.The major defect of this method is: (1) ethylene glycol is organic solvent, and cost is higher, and is unfavorable for environmental protection; (2) sonic oscillation is 6 hours, and jitter time is long; (3) the composite material output that generates is low excessively, and stannic oxide particle is easy to reunite, and causes poor performance, is unfavorable for suitability for industrialized production.
Summary of the invention
The objective of the invention is the deficiency to existing tin ash and graphene composite material preparation method, the preparation method of a kind of flower-shaped tin ash and graphene composite material is provided, it is simple to have method; With water is solvent; Do not use surfactant, production cost is lower, and is free from environmental pollution; Output is high, can make the graphene-supported controlled characteristics such as flower-shaped tin ash of pattern that go up.
The technical scheme that realizes the object of the invention is: the preparation method of a kind of flower-shaped tin ash and graphene composite material; With stannic chloride pentahydrate and NaOH and graphene oxide is raw material, through mix stirring, hydro-thermal reaction, Separation of Solid and Liquid, clean repeatedly, dry simple process makes flower-shaped tin ash and graphene composite material.Its concrete steps are following:
(1) mixes stirring
With stannic chloride pentahydrate and NaOH and graphene oxide is raw material; Water is solvent; Quality (g) in stannic chloride pentahydrate: the quality of NaOH (g): the quality of graphene oxide (g): the ratio of the volume of deionized water (ml) is 1: 1.2～1.6: 0.001～0.4: 30～45 ratio, in container, adds stannic chloride pentahydrate, NaOH, graphene oxide and deionized water; Mix and stirred 2～60 minutes, just obtain the mixed solution of graphene oxide and tin ash predecessor.
(2) hydro-thermal reaction
After the completion of (1) step; The mixed solution that earlier (1) step was made moves in the hydrothermal reaction kettle that liner is a polytetrafluoroethylene; Under 160～250 ℃ of temperature, carried out hydro-thermal reaction 2～36 hours, again the mixed liquor after the hydro-thermal reaction is positioned in the centrifuge; Carry out Separation of Solid and Liquid, collect centrifugate and deposition respectively.To deposition, again by the quality (g) that precipitates: the volume ratio of deionized water (ml) is 1: 40～200 ratio, adds once more after deionized water and stirring mixes; Be positioned in the centrifuge; Carry out Separation of Solid and Liquid, collect centrifugate and deposition once more respectively, so repeat 2～10 times.Merge the treated back up to standard discharging of centrifugate of each time collection at last; To the deposition of last collection, be used for next step dried.
(3) drying
(2) step with last deposition of collecting of (2) step, was positioned in the drier after accomplishing, 40～150 ℃ dry 6～96 hours down, just prepare flower-shaped tin ash and graphene composite material product.
After the present invention adopts technique scheme, mainly contain following effect:
1, the present invention is solvent with water, does not use surfactant, and is with low cost.It is short to mix mixing time, mixes.Each step does not produce poisonous and harmful substance in the preparation process, helps environmental protection.
2, the flower-shaped tin ash of preparing and the output of graphene composite material are high; The controlled flower-shaped tin ash of pattern is uniformly dispersed on the Graphene surface; The nanometer rods of forming flower-shaped tin ash has superior characteristic more than the tin oxide nano particles that piles up in the matter and energy transmittance process, become the express passway that matter and energy transmits; Reduce interface impedance, thereby improve the performance of material.
3, the inventive method is simple, and is easy and simple to handle, and device therefor is simple, is easy to apply.
The flower-shaped tin ash and the graphene composite material that adopt the inventive method to prepare can be widely used in new energy devices such as lithium ion battery, solar cell, ultracapacitor; Also, have a extensive future applicable to fields such as catalyst carrier, information materials.
Description of drawings
The SEM Electronic Speculum figure of flower-shaped tin ash that Fig. 1 prepares for this instance 1 and graphene composite material.
Among the figure: 1 is flower-shaped tin ash, and 2 is Graphene.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
The preparation method of a kind of flower-shaped tin ash and graphene composite material, its concrete steps are following:
(1) mixes stirring
With stannic chloride pentahydrate and NaOH and graphene oxide is raw material; Water is solvent; Quality (g) in stannic chloride pentahydrate: the quality of NaOH (g): the quality of graphene oxide (g): the ratio of the volume of deionized water (ml) is 1: 1.4: 0.1: 40 ratio in container, adds stannic chloride pentahydrate, NaOH, graphene oxide and deionized water; Mix and stirred 20 minutes, just obtain the mixed solution of graphene oxide and tin ash predecessor.
(2) hydro-thermal reaction
(1) step went on foot the mixed solution that makes with (1) earlier and moves in the hydrothermal reaction kettle that liner is a polytetrafluoroethylene, under 200 ℃ of temperature after accomplishing; Carried out hydro-thermal reaction 16 hours; Again the mixed liquor after the hydro-thermal reaction is positioned in the centrifuge, carries out Separation of Solid and Liquid, collect centrifugate and deposition respectively.To deposition, again by the quality (g) that precipitates: the volume ratio of deionized water (ml) is 1: 100 a ratio, adds once more after deionized water and stirring mixes, and is positioned in the centrifuge, carries out Separation of Solid and Liquid, collects centrifugate and deposition once more respectively, so repeats 5 times.Merge the treated back up to standard discharging of centrifugate of each time collection at last; To the deposition of last collection, be used for next step dried.
(3) drying
(2) step with last lower sediment of collecting of (2) step, was positioned in the drier after accomplishing, 70 ℃ dry 36 hours down, just prepare flower-shaped tin ash and graphene composite material product.
The preparation method of a kind of flower-shaped tin ash and graphene composite material, with embodiment 1, wherein:
In (1) step, the quality of stannic chloride pentahydrate (g): the quality of NaOH (g): the quality of graphene oxide (g): the ratio of the volume of deionized water (ml) is 1: 1.2: 0.001: 30, and the mixing mixing time in container is 2 minutes.
In (2) step, hydrothermal temperature is 160 ℃, and the hydro-thermal reaction time is 36 hours, the quality of deposition (g): the volume ratio of deionized water (ml) is 1: 40, so repeats 10 times.
In (3) step, baking temperature is 40 ℃, and be 96 hours drying time.
The preparation method of a kind of flower-shaped tin ash and graphene composite material, with embodiment 1, wherein:
In (1) step, the quality of stannic chloride pentahydrate (g): the quality of NaOH (g): the quality of graphene oxide (g): the ratio of the volume of deionized water (ml) is 1: 1.6: 0.4: 45, and in container, mixing mixing time is 60 minutes.
In (2) step, hydrothermal temperature is 250 ℃, and the hydro-thermal reaction time is 2 hours, the quality of deposition (g): the volume ratio of deionized water (ml) is 1: 200, so repeats 2 times.
In (3) step, baking temperature is 150 ℃, and be 6 hours drying time.
Result of the test
Prepare flower-shaped tin ash and graphene composite material with embodiment 1 and take the SEM figure of gained through field emission scanning electron microscope, as shown in Figure 1.
Can know from Fig. 1: by the flower-shaped tin ash that nanometer tin dioxide rod constituted; Its particle diameter is at 500nm～1 μ m; Flower-shaped tin ash is carried between the surface and layer and layer of Graphene uniformly, has effectively stoped the reunion of tin ash and Graphene, thereby has improved the performance of material; The nanometer rods of forming flower-shaped tin ash has superior characteristic more than the tin oxide nano particles that piles up in the matter and energy transmittance process, become the express passway that matter and energy transmits, and reduces interface impedance, further improves the performance of material.
Claims (4)
1. method for preparing flower-shaped tin ash and graphene composite material is characterized in that its concrete steps are following:
(1) mixes stirring
With stannic chloride pentahydrate and NaOH and graphene oxide is raw material; Water is solvent; Quality in stannic chloride pentahydrate: the quality of NaOH: the quality of graphene oxide: the ratio of the volume of deionized water is the ratio of 1g: 1.2～1.6g: 0.001～0.4g: 30～45ml; In container, add stannic chloride pentahydrate, NaOH, graphene oxide and deionized water, mix and stirred 2～60 minutes;
(2) hydro-thermal reaction
(1) step went on foot the mixed solution that makes with (1) earlier and moves in the hydrothermal reaction kettle that liner is a polytetrafluoroethylene, under 160～250 ℃ of temperature after accomplishing; Carry out hydro-thermal reaction 2～36 hours, and again the mixed liquor after the hydro-thermal reaction was positioned in the centrifuge, carry out Separation of Solid and Liquid; Collect centrifugate and deposition respectively, to deposition, again in the quality that precipitates: the volume ratio of deionized water is the ratio of 1g: 40～200ml; Add once more after deionized water and stirring mixes, be positioned in the centrifuge, carry out Separation of Solid and Liquid; Collect centrifugate and deposition once more respectively, so repeat 2～10 times, merge the centrifugate of each time collection at last;
(3) drying
(2) step with last deposition of collecting of (2) step, was positioned in the drier after accomplishing, 40～150 ℃ dry 6～96 hours down.
2. according to the described a kind of method for preparing flower-shaped tin ash and graphene composite material of claim 1, it is characterized in that:
In (1) step, the quality of stannic chloride pentahydrate: the quality of NaOH: the quality of graphene oxide: the ratio of the volume of deionized water is 1g: 1.4g: 0.1g: 40ml, and the mixing mixing time in container is 20 minutes;
In (2) step, hydrothermal temperature is 200 ℃, and the hydro-thermal reaction time is 16 hours, the quality of deposition: the volume ratio of deionized water is 1g: 100ml, so repeats 5 times;
In (3) step, baking temperature is 70 ℃, and be 36 hours drying time.
3. according to the described a kind of method for preparing flower-shaped tin ash and graphene composite material of claim 1, it is characterized in that:
In (1) step, the quality of stannic chloride pentahydrate: the quality of NaOH: the quality of graphene oxide: the ratio of the volume of deionized water is 1g: 1.2g: 0.001g: 30ml, and the mixing mixing time in container is 2 minutes;
In (2) step, hydrothermal temperature is 160 ℃, and the hydro-thermal reaction time is 36 hours, the quality of deposition: the volume ratio of deionized water is 1g: 40ml, so repeats 10 times;
In (3) step, baking temperature is 40 ℃, and be 96 hours drying time.
4. according to the described a kind of method for preparing flower-shaped tin ash and graphene composite material of claim 1, it is characterized in that:
In (1) step, the quality of stannic chloride pentahydrate: the quality of NaOH: the quality of graphene oxide: the ratio of the volume of deionized water is 1g: 1.6g: 0.4g: 45ml, and in container, mixing mixing time is 60 minutes;
In (2) step, hydrothermal temperature is 250 ℃, and the hydro-thermal reaction time is 2 hours, the quality of deposition: the volume ratio of deionized water is 1g: 200ml, so repeats 2 times;
In (3) step, baking temperature is 150 ℃, and be 6 hours drying time.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674439A (en) * | 2012-05-28 | 2012-09-19 | 重庆大学 | Method for preparing stannic oxide porous microsphere |
| CN102891319A (en) * | 2012-09-24 | 2013-01-23 | 上海锦众信息科技有限公司 | Preparation method of graphite composite material of lithium ion battery |
| 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 |
| CN103482616A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material |
| CN105470484A (en) * | 2015-12-04 | 2016-04-06 | 厦门大学 | Preparation method of graphene/stannic oxide composite nanofiber membrane and application |
| CN106549166A (en) * | 2016-12-07 | 2017-03-29 | 黄河科技学院 | The carrier and its preparation method of the electrode catalyst of one proton exchanging film fuel battery |
| CN108091844A (en) * | 2017-12-11 | 2018-05-29 | 合肥国轩电池材料有限公司 | A kind of composite cathode material of lithium ion battery stannic oxide/graphene and preparation method thereof |
| CN108807962A (en) * | 2018-07-31 | 2018-11-13 | 澳洋集团有限公司 | A kind of preparation method of stannic oxide-graphene negative material |
| CN110429179A (en) * | 2019-07-15 | 2019-11-08 | 河南大学 | A kind of AZO/ titanium dioxide/stannic oxide-graphene oxide film and utilize its perovskite solar battery obtained |
| CN112499669A (en) * | 2020-12-31 | 2021-03-16 | 广西科技大学 | Novel tin dioxide graphite grading nano heteroplasmon with morphology structure and preparation method thereof |
| CN113511670A (en) * | 2021-07-26 | 2021-10-19 | 湖北工程学院 | Three-dimensional flower bunch-shaped structure nano material compounded with zinc sulfide on graphene oxide, application and preparation method |
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| CN101693552A (en) * | 2009-10-22 | 2010-04-14 | 浙江大学 | Method for preparing tin dioxide nanostructure material with floriform appearance by hydrothermal synthesis |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674439A (en) * | 2012-05-28 | 2012-09-19 | 重庆大学 | Method for preparing stannic oxide porous microsphere |
| CN102891319A (en) * | 2012-09-24 | 2013-01-23 | 上海锦众信息科技有限公司 | Preparation method of graphite composite material of lithium ion battery |
| 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 |
| CN103326007B (en) * | 2013-06-25 | 2015-12-09 | 上海交通大学 | The preparation method of three-dimensional graphite thiazolinyl tin dioxide composite material and application thereof |
| CN103482616A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Preparation method of graphene-tin dioxide nanoparticle three-dimensional foam composite material |
| CN105470484A (en) * | 2015-12-04 | 2016-04-06 | 厦门大学 | Preparation method of graphene/stannic oxide composite nanofiber membrane and application |
| CN106549166A (en) * | 2016-12-07 | 2017-03-29 | 黄河科技学院 | The carrier and its preparation method of the electrode catalyst of one proton exchanging film fuel battery |
| CN108091844A (en) * | 2017-12-11 | 2018-05-29 | 合肥国轩电池材料有限公司 | A kind of composite cathode material of lithium ion battery stannic oxide/graphene and preparation method thereof |
| CN108807962A (en) * | 2018-07-31 | 2018-11-13 | 澳洋集团有限公司 | A kind of preparation method of stannic oxide-graphene negative material |
| CN110429179A (en) * | 2019-07-15 | 2019-11-08 | 河南大学 | A kind of AZO/ titanium dioxide/stannic oxide-graphene oxide film and utilize its perovskite solar battery obtained |
| CN110429179B (en) * | 2019-07-15 | 2021-04-27 | 河南大学 | AZO/titanium dioxide/tin dioxide-graphene oxide film and perovskite solar cell prepared by using same |
| CN112499669A (en) * | 2020-12-31 | 2021-03-16 | 广西科技大学 | Novel tin dioxide graphite grading nano heteroplasmon with morphology structure and preparation method thereof |
| CN113511670A (en) * | 2021-07-26 | 2021-10-19 | 湖北工程学院 | Three-dimensional flower bunch-shaped structure nano material compounded with zinc sulfide on graphene oxide, application and preparation method |
| CN113511670B (en) * | 2021-07-26 | 2022-05-03 | 湖北工程学院 | Three-dimensional flower bunch-shaped structure nano material compounded with zinc sulfide on graphene oxide, application and preparation method |
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Application publication date: 20120118 |