CN102718250A - Method for preparing carbon-material-carrying tin dioxide nanosheet composite material - Google Patents
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Abstract
The invention relates to a method for preparing a carbon-material-carrying tin dioxide nanosheet composite material, belonging to the technical field of functional composite materials. According to the method, a carbon material, tin dichloride dihydrate and sodium citrate dihydrate are taken as raw materials and are subjected to mixing, stirring, hydrothermal synthesis, solid-liquid separation, cleaning and drying, and then, the morphology-controlled carbon-material-carrying tin dioxide nanosheet composite material is prepared. The method provided by the invention is simple and is convenient in operation; and water is taken as a solvent, so that the production cost is lower, the environment is not polluted, and the popularization and the application are facilitated. The carbon-material-carrying tin dioxide nanosheet composite material prepared by adopting the method provided by the invention can be widely applied to new-energy devices such as lithium ion batteries, solar batteries and supercapacitors, and can also be applicable 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 carbon material supported stannic oxide nanometer sheet matrix material.
Background technology
Tindioxide has the positive tetrahedron rutile-type 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.Carbon material is because cheap, excellent conductivity and physical and chemical stability are celebrated; With carbon material as the carrier tindioxide of growing; Not only can the agglomerated phenomenon be curbed, and both complex effects can be more effectively brought into play in the combination of growth in situ.Carbon material and tindioxide recombination energy obviously improve the material electric conductivity, 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 tindioxide and graphene composite material; Like publication number is the patent of CN101969113A " preparation method of graphene-based tindioxide composite lithium ion battery cathode material ", and utilizing hydrothermal method is raw material with stannic chloride pentahydrate, sodium hydroxide and graphene oxide, and ethanol is solvent; Cetyl trimethylammonium bromide is a tensio-active agent; Stir after 30 minutes, carry out hydro-thermal reaction, generated tindioxide and graphene composite material.The main drawback of this method is: (1) ethanol is solvent, and cost is higher; (2) use sodium hydroxide, be unfavorable for environmental protection; (3) stannic oxide particle is easy to reunite in the matrix material.
Summary of the invention
The objective of the invention is the deficiency to existing tindioxide and carbon material composite material and preparation method thereof, a kind of preparation method of carbon material supported stannic oxide nanometer sheet matrix material is provided, it is simple to have method; With water is solvent; Do not use alkaline matter, production cost is lower, and is free from environmental pollution; Output is high, can make the carbon material supported controlled characteristics such as stannic oxide nanometer sheet of pattern that go up.
The technical scheme that realizes the object of the invention is: a kind of preparation method of carbon material supported stannic oxide nanometer sheet matrix material; With carbon material and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder is raw material, through mix stirring, hydro-thermal reaction, solid-liquid separation, clean repeatedly, the exsiccant simple process makes carbon material supported stannic oxide nanometer sheet matrix material.Its concrete steps are following:
(1) mixes stirring
With carbon material (Graphene or carbon nanotube or graphite) and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder is raw material; Water is solvent; Quality (g) in carbon material: the quality of two water tindichloride (g): Sodium Citrate, usp, Dihydrate Powder (g): the ratio of the volume of deionized water (ml) is 1: 1～18: 0.1～50: 50～500 ratio; In container; Add carbon material, two water tindichloride, Sodium Citrate, usp, Dihydrate Powder and deionized water, mix and stirred 2～60 minutes, just obtain the mixing solutions of carbon material and tindioxide precursor.
(2) hydro-thermal reaction
After the completion of (1) step; The mixing solutions that earlier (1) step was made moves in the hydrothermal reaction kettle that liner is a tetrafluoroethylene; Under 140～250 ℃ of temperature, carried out hydro-thermal reaction 2～36 hours, again the mixed solution after the hydro-thermal reaction is positioned in the whizzer; Carry out solid-liquid separation, collect centrifugate and deposition respectively.To deposition, again in sedimentary quality (g): 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 whizzer; Carry out solid-liquid separation, collect centrifugate and deposition once more respectively, so repeat 3～12 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 drying treatment.
(3) drying
(2) step with last deposition of collecting of (2) step, was positioned in the moisture eliminator after accomplishing, 40～160 ℃ dry 4～96 hours down, just prepare carbon material supported stannic oxide nanometer sheet matrix material.
After the present invention adopts technique scheme, mainly contain following effect:
(1) the inventive method can be with stannic oxide nanometer sheet growth in situ on the surface of carbon material; On the structure radical change the combination of carbon material and tindioxide; Make and to be combined into an integral body as the carbon material of carrier and active substance as tindioxide; Be configured to the new function matrix material, fundamentally solved the uniformly dispersed problem of active substance in the carbon material carrier;
(2) material of the present invention has improved specific conductivity, stability and the utilization ratio of active substance tindioxide greatly, and chemical property is superior;
(3) the inventive method is simple, and is easy and simple to handle, and equipment used is simple, and production cost is low, is easy to apply.
The product that adopts the inventive method to prepare can be widely used in new energy devices such as lithium ion battery, ultracapacitor, also goes for having a extensive future in the materials such as conductive and heat-conductive, support of the catalyst, transmitter.
Description of drawings
The SEM Electronic Speculum figure of the graphene-supported stannic oxide nanometer sheet matrix material that Fig. 1 prepares for this instance 1.
Among the figure: 1 is Graphene, and 2 is the stannic oxide nanometer sheet.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
A kind of preparation method of carbon material supported stannic oxide nanometer sheet matrix material, its concrete steps are following:
(1) mixes stirring
With carbon material (Graphene) and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder is raw material; Water is solvent; Quality (g) in Graphene: the quality of two water tindichloride (g): the quality of Sodium Citrate, usp, Dihydrate Powder (g): the ratio of the volume of deionized water (ml) is 1: 9: 29.4: 200 ratio in container, adds Graphene, two water tindichloride, Sodium Citrate, usp, Dihydrate Powder and deionized water; Mix and stirred 20 minutes, just obtain the mixing solutions of Graphene and tindioxide precursor.
(2) hydro-thermal reaction
(1) step went on foot the mixing solutions that makes with (1) earlier and moves in the hydrothermal reaction kettle that liner is a tetrafluoroethylene, under 200 ℃ of temperature after accomplishing; Carried out hydro-thermal reaction 16 hours; Again the mixed solution after the hydro-thermal reaction is positioned in the whizzer, carries out solid-liquid separation, collect centrifugate and deposition respectively.To deposition, again in sedimentary quality (g): 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 whizzer, carries out solid-liquid separation, 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 drying treatment.
(3) drying
(2) step with last lower sediment of collecting of (2) step, was positioned in the moisture eliminator after accomplishing, 60 ℃ dry 36 hours down, just prepare graphene-supported stannic oxide nanometer sheet matrix material.
A kind of preparation method of carbon material supported stannic oxide nanometer sheet matrix material, with embodiment 1, wherein:
In (1) step; Carbon material (carbon nanotube) and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder are raw material; Water is solvent; Quality (g) in carbon nanotube: the quality of two water tindichloride (g): the quality of Sodium Citrate, usp, Dihydrate Powder (g): the ratio of the volume of deionized water (ml) is 1: 1: 0.1: 50 ratio, the mixing churning time in container is 2 minutes.
In (2) step, hydrothermal temperature is 140 ℃, and the hydro-thermal reaction time is 36 hours, sedimentary quality (g): the volume ratio of deionized water (ml) is 1: 40, so repeats 12 times.
In (3) step, drying temperature is 40 ℃, and be 96 hours time of drying.
A kind of preparation method of carbon material supported stannic oxide nanometer sheet matrix material, with embodiment 1, wherein:
In (1) step; Carbon material (graphite) and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder are raw material; Water is solvent; Quality (g) in graphite: the quality of two water tindichloride (g): the quality of Sodium Citrate, usp, Dihydrate Powder (g): the ratio of the volume of deionized water (ml) is 1: 18: 50: 500 ratio, in container, mixing churning time is 60 minutes.
In (2) step, hydrothermal temperature is 250 ℃, and the hydro-thermal reaction time is 2 hours, sedimentary quality (g): the volume ratio of deionized water (ml) is 1: 200, so repeats 3 times.
In (3) step, drying temperature is 160 ℃, and be 4 hours time of drying.
Test-results
Prepare the SEM Electronic Speculum figure of graphene-supported stannic oxide nanometer sheet matrix material with embodiment 1, as shown in Figure 1.
Can know from Fig. 1: the stannic oxide nanometer sheet is carried between the surface and layer and layer of Graphene uniformly, has effectively stoped the reunion of tindioxide and Graphene, thereby has improved the performance of material; The stannic oxide nanometer sheet has superior characteristic more than the tin oxide nano particles that piles up in the matter and energy transmittance process, can shorten carrier or ion transportation path, reduces interface impedance.
Claims (4)
1. the preparation method of a carbon material supported stannic oxide nanometer sheet matrix material is characterized in that its concrete steps are following:
(1) mixes stirring
With carbon material (Graphene or carbon nanotube or graphite) and two water tindichloride and Sodium Citrate, usp, Dihydrate Powder is raw material; Water is solvent; Quality in carbon material: the quality of two water tindichloride: the quality of Sodium Citrate, usp, Dihydrate Powder: the ratio of the volume of deionized water is the ratio of 1g: 1～18g: 0.1～50g: 50～500ml; In container, add carbon material, two water tindichloride, Sodium Citrate, usp, Dihydrate Powder and deionized water, mix and stirred 2～60 minutes;
(2) hydro-thermal reaction
After the completion of (1) step; The mixing solutions that earlier (1) step was made moves in the hydrothermal reaction kettle that liner is a tetrafluoroethylene; Under 140～250 ℃ of temperature, carried out hydro-thermal reaction 2～36 hours, again the mixed solution after the hydro-thermal reaction is positioned in the whizzer; Carry out solid-liquid separation, collect centrifugate and deposition respectively.To deposition, again in sedimentary quality: the volume ratio of deionized water is the ratio of 1g: 40～200ml, adds once more after deionized water and stirring mixes; Be positioned in the whizzer; Carry out solid-liquid separation, collect centrifugate and deposition once more respectively, so repeat 3～12 times.Merge the treated back up to standard discharging of centrifugate of each time collection at last,, be used for next step drying treatment the deposition of last collection;
(3) drying
(2) step with last deposition of collecting of (2) step, was positioned in the moisture eliminator after accomplishing, 40～160 ℃ dry 4～96 hours down.
2. according to the preparation method of the described a kind of carbon material supported stannic oxide nanometer sheet matrix material of claim 1, it is characterized in that:
In (1) step, the quality of Graphene: the quality of two water tindichloride: the quality of Sodium Citrate, usp, Dihydrate Powder: the volume ratio of deionized water is 1g: 9g: 29.4g: 200ml, and the mixing churning time in container is 20 minutes;
In (2) step, hydrothermal temperature is 200 ℃, and the hydro-thermal reaction time is 16 hours, sedimentary quality: the volume ratio of deionized water is 1g: 100ml, so repeats 5 times;
In (3) step, drying temperature is 60 ℃, and be 36 hours time of drying.
3. according to the preparation method of the described a kind of carbon material supported stannic oxide nanometer sheet matrix material of claim 1, it is characterized in that:
In (1) step, the quality of carbon nanotube: the quality of two water tindichloride: the quality of Sodium Citrate, usp, Dihydrate Powder: the volume ratio of deionized water is 1g: 1g: 0.1g: 50ml, and the mixing churning time in container is 2 minutes;
In (2) step, hydrothermal temperature is 140 ℃, and the hydro-thermal reaction time is 36 hours, sedimentary quality: the volume ratio of deionized water is 1g: 40ml, so repeats 12 times;
In (3) step, drying temperature is 40 ℃, and be 96 hours time of drying.
4. according to the preparation method of the described a kind of carbon material supported stannic oxide nanometer sheet matrix material of claim 1, it is characterized in that:
In (1) step, the quality of graphite: the quality of two water tindichloride: the quality of Sodium Citrate, usp, Dihydrate Powder: the ratio of the volume of deionized water is the ratio of 1g: 18g: 50g: 500ml, and in container, mixing churning time is 60 minutes;
In (2) step, hydrothermal temperature is 250 ℃, and the hydro-thermal reaction time is 2 hours, sedimentary quality: the volume ratio of deionized water is 1g: 200ml, so repeats 2 times;
In (3) step, drying temperature is 160 ℃, and be 6 hours time of drying.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112846A (en) * | 2013-02-06 | 2013-05-22 | 华中科技大学 | Preparation method of graphene-carbon nanotube-nano tin dioxide three-dimensional composite material and product thereof |
| CN103833076A (en) * | 2012-11-27 | 2014-06-04 | 王泰林 | Nickel oxide-titanium dioxide nano composite material |
| CN103926278A (en) * | 2014-04-24 | 2014-07-16 | 电子科技大学 | Graphene-based ternary composite film gas sensor and preparation method thereof |
| CN104900850A (en) * | 2014-03-07 | 2015-09-09 | 中国科学院大连化学物理研究所 | Preparation of SnO2/carbon nanotube composite material and application of composite material |
| CN105118965A (en) * | 2015-07-27 | 2015-12-02 | 陕西科技大学 | Preparation method of SnO2/pyrolytic carbon electrode material for sodium-ion battery negative electrode |
| CN105883906A (en) * | 2016-04-11 | 2016-08-24 | 同济大学 | Nano stannic oxide-graphene composite as well as preparation method and application thereof |
| 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 |
| CN107697943A (en) * | 2017-10-31 | 2018-02-16 | 电子科技大学 | A kind of preparation method of flake nano metal oxide |
| CN109179491A (en) * | 2018-11-09 | 2019-01-11 | 五邑大学 | A kind of fast-growth SnO2The method of nanometer sheet |
| CN109879266A (en) * | 2019-03-05 | 2019-06-14 | 中南大学 | A kind of preparation method of porous C-base composte material |
| CN110571063A (en) * | 2019-08-22 | 2019-12-13 | 江苏大学 | Sn2O3Nano-sheet/functional carbon nano-sheet composite material and preparation method thereof |
| CN111453766A (en) * | 2020-04-09 | 2020-07-28 | 吉林大学 | One-dimensional MWCNTs @ SnO2Core-shell structure, preparation method thereof and application of core-shell structure to positive electrode of lead-carbon battery |
| CN111487292A (en) * | 2020-05-18 | 2020-08-04 | 黑龙江省科学院高技术研究院 | Preparation method and application of hemp stalk biomass graphene-based sulfur-doped tin oxide composite gas-sensitive material |
| CN113667196A (en) * | 2021-07-28 | 2021-11-19 | 江门市宏儒电子科技有限公司 | Epoxy type copper-clad plate base material and preparation method and application thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833076A (en) * | 2012-11-27 | 2014-06-04 | 王泰林 | Nickel oxide-titanium dioxide nano composite material |
| CN103112846A (en) * | 2013-02-06 | 2013-05-22 | 华中科技大学 | Preparation method of graphene-carbon nanotube-nano tin dioxide three-dimensional composite material and product thereof |
| CN104900850A (en) * | 2014-03-07 | 2015-09-09 | 中国科学院大连化学物理研究所 | Preparation of SnO2/carbon nanotube composite material and application of composite material |
| CN103926278A (en) * | 2014-04-24 | 2014-07-16 | 电子科技大学 | Graphene-based ternary composite film gas sensor and preparation method thereof |
| CN103926278B (en) * | 2014-04-24 | 2017-01-18 | 电子科技大学 | graphene-based ternary composite film gas sensor and preparation method thereof |
| CN105118965A (en) * | 2015-07-27 | 2015-12-02 | 陕西科技大学 | Preparation method of SnO2/pyrolytic carbon electrode material for sodium-ion battery negative electrode |
| CN105883906A (en) * | 2016-04-11 | 2016-08-24 | 同济大学 | Nano stannic oxide-graphene composite as well as preparation method and application thereof |
| 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 |
| CN107697943A (en) * | 2017-10-31 | 2018-02-16 | 电子科技大学 | A kind of preparation method of flake nano metal oxide |
| CN109179491A (en) * | 2018-11-09 | 2019-01-11 | 五邑大学 | A kind of fast-growth SnO2The method of nanometer sheet |
| CN109879266A (en) * | 2019-03-05 | 2019-06-14 | 中南大学 | A kind of preparation method of porous C-base composte material |
| CN110571063A (en) * | 2019-08-22 | 2019-12-13 | 江苏大学 | Sn2O3Nano-sheet/functional carbon nano-sheet composite material and preparation method thereof |
| CN110571063B (en) * | 2019-08-22 | 2021-11-23 | 江苏大学 | Sn2O3Nano-sheet/functional carbon nano-sheet composite material and preparation method thereof |
| CN111453766A (en) * | 2020-04-09 | 2020-07-28 | 吉林大学 | One-dimensional MWCNTs @ SnO2Core-shell structure, preparation method thereof and application of core-shell structure to positive electrode of lead-carbon battery |
| CN111487292A (en) * | 2020-05-18 | 2020-08-04 | 黑龙江省科学院高技术研究院 | Preparation method and application of hemp stalk biomass graphene-based sulfur-doped tin oxide composite gas-sensitive material |
| CN111487292B (en) * | 2020-05-18 | 2023-03-28 | 黑龙江省科学院高技术研究院 | Preparation method and application of hemp stalk biomass graphene-based sulfur-doped tin oxide composite gas-sensitive material |
| CN113667196A (en) * | 2021-07-28 | 2021-11-19 | 江门市宏儒电子科技有限公司 | Epoxy type copper-clad plate base material and preparation method and application thereof |
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Application publication date: 20121010 |