CN102142549B - Graphene nano sheet and SnS2 composite nano material and synthesis method thereof - Google Patents
Graphene nano sheet and SnS2 composite nano material and synthesis method thereof Download PDFInfo
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- CN102142549B CN102142549B CN201110046471.2A CN201110046471A CN102142549B CN 102142549 B CN102142549 B CN 102142549B CN 201110046471 A CN201110046471 A CN 201110046471A CN 102142549 B CN102142549 B CN 102142549B
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Abstract
The invention discloses a graphene nano sheet and SnS2 composite nano material and a synthesis method thereof. The composite material is characterized by being formed by compounding a graphene nano sheet and a SnS2 nano material, wherein the substance amount ratio of the graphene nano sheet to the SnS2 nano material is 1:1-4:1. The preparation method comprises the following steps of: preparing a graphite oxide nano sheet from graphite by using a chemical oxidation method, then dissolving L-cysteine into deionized water, adding stannic chloride, and dissolving the stannic chloride with full stirring, wherein the molar ratio of the L-cysteine to the stannic chloride in the solution is 6:1-12:1; and adding the graphite oxide nano sheet into the solution, performing ultrasonic treatment so that the graphite oxide nano sheet is fully dispersed in the hydrothermal reaction solution, and synthesizing the graphene nano sheet and SnS2 composite nano material by a one-step hydrothermal method, wherein the mass ratio of the graphene nano sheet to the SnS2 nano material in the composite material is 1:1-4:1. The method has the characteristics of mild reaction condition and simple process. The synthesized graphene nano sheet and SnS2 composite nano material serving as an electrode material of a new energy battery or serving as other materials has wide application.
Description
Technical field
The present invention relates to composite nano materials and preparation thereof, relate in particular to graphene nanometer sheet and SnS
2composite nano materials and preparation method thereof, belong to inorganic composite nano material, new energy materials and preparation field thereof.
Background technology
Graphene nanometer sheet has the performances such as physics, chemistry and mechanics of numerous uniquenesses with its unique two-dimensional nano chip architecture, have important scientific research meaning and application prospect widely.The finder of grapheme material obtains the Nobel Prize in 2010 and has excited especially the very big interest of people to grapheme material research.Graphene nanometer sheet has high specific area, high conduction and heat conductivility, superpower mechanical property.Recently people have carried out research widely to graphene nanometer sheet as the application of the electrode material of micro-nano electronic device, new forms of energy battery, kollag and novel catalyst carrier.
SnS
2the structure with layered crystal, it forms octahedral coordination by two-layer compact arranged S atom and the sandwich sandwich structure forming of Sn cation, combines between layers with weak Van der Waals force.SnS
2as lithium ion battery negative material, there is good electrochemistry seasoning lithium performance.SnS
2electrochemical lithiation theoretical capacity be 645mAh/g, so the theoretical capacity of large graphite 372mAh/g.Therefore, SnS
2also can be used as a kind of potential lithium ion battery negative material of alternative graphite material.[Momma T, Shiraishi N, Yoshizawa A, et al., the SnS such as Momma
2anode for rechargeable lithium battery.Journalof Power Sources, 2001,97-98:198～200] use SnCl
4the SnS synthetic with thioacetamide method
2product is after 400 ℃ of processing, and its electrochemistry storage lithium reversible capacity reaches 600mAh/g, but after circulation 25 times, capacity is less than 400mAh/g.Therefore, its cycle performance is to be further improved in addition.[Seo JW, Jang JT, Park SW, et al., the Two-Dimensional SnS such as Seo JW
2nanoplates withExtraordinary High Discharge Capacity for Lithium Ion Batteries.Advanced Materials.2008,20 (22): 4269～4273] by by organic Sn presoma pyrolyzing synthesis SnS
2nanocrystal, result shows SnS
2more than the electrochemistry storage lithium capacity of nanocrystal can reach 600mAh/g, and there is good cycle performance, shown SnS
2nanocrystal has a good application prospect as lithium ion battery negative material.
Due to graphene nanometer sheet and SnS
2it is all the electrode material of very promising new forms of energy battery.If graphene nanometer sheet and SnS
2the corresponding composite nano materials of the compound preparation of nano material, the high conduction performance of graphene nanometer sheet can further improve the electric conductivity of composite material, be conducive to the electronics transmission in electrochemical electrode reaction and catalytic reaction process, the chemical property of reinforced composite electrode.Graphene nanometer sheet and SnS in addition
2compound, due to large ∏ key and the SnS of graphene nanometer sheet
2the interaction of Electronic Structure, can form the electronic structure between a kind of new different material.This graphene nanometer sheet and SnS
2the performance that composite nano materials has having a wide range of applications and strengthens as new forms of energy electrode material.But graphene nanometer sheet and SnS
2the research synthetic and chemical property of composite nano materials have not been reported.
The application of biological micromolecule in nano material is synthetic recently obtained people's extensive concern.Cys contains a plurality of functional group (as: NH
2,-COOH and-SH), these functional groups can provide coordination atom and metal cation to form coordinate bond.Cys has obtained application in synthetic transient metal sulfide nano material.Document [Zhang B, Ye XC, Hou WY, Zhao Y, Xie Y.Biomolecule-assistedsynthesis and electrochemical hydrogen storage of Bi
2s
3flowerlike patterns withwell-aligned nanorods.Journal of Physical Chemistry B, 2006,110 (18) 8978～8985] with Cys, synthesized the Bi of floriform appearance
2s
3nano structural material.But up to the present, with Cys, come synthesizing graphite alkene nanometer sheet and SnS
2the research of composite nano materials yet there are no report publicly.
Summary of the invention
The object of the present invention is to provide a kind of graphene nanometer sheet and SnS
2composite nano materials and preparation method thereof, it is characterized in that composite material is by graphene nanometer sheet and SnS
2the compound formation of nano material, graphene nanometer sheet and SnS
2between nano material, the ratio of amount is 1: 1-4: 1.
A kind of graphene nanometer sheet provided by the invention and SnS
2its preparation method of composite nano materials, it is characterized in that the method carries out as follows:
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 0.015-0.072g graphite powder is distributed in the 20-25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be graphite 3-4 doubly, stir 30-60 minute, temperature rises to 30-35 ℃ of left and right, adds 40-50ml deionized water, stirs 20-30 minute, adds the H of 10-15ml mass concentration 30%
2o
2, stir 5-20 minute, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
2) Cys is dissolved in deionized water, then adds butter of tin (SnCl
45H
2o) and fully stir and make its dissolving, in solution, the mol ratio of Cys and butter of tin was at 6: 1～12: 1, again by by the 1st) the graphite oxide nanometer sheet for preparing of step adds in this solution, the 1st) step graphite raw material amount used is 1: 1～4: 1 with the ratio of the amount of butter of tin, ultrasonic processing 1-2h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, this mixture is proceeded in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene and seal, at 180-200 ℃ of reaction 20-36h, the product centrifugation obtaining, and with deionized water and absolute ethanol washing, dry, obtain graphene nanometer sheet and SnS
2composite nano materials.
Method of the present invention has advantages of following outstanding compared with the prior art:
(1) because graphene nanometer sheet has the excellent properties such as high specific area, superpower mechanical property, high conduction and heat conduction, therefore, graphene nanometer sheet of the present invention and SnS
2composite nano materials have and strengthen mechanical property, conduction and heat conductivility, be conducive to it as the electrode reaction of new forms of energy battery electrode material, electronics transmission in catalytic reaction process, strengthen chemical property and the catalytic performance of composite nano materials.And the superpower mechanical property of graphene nanometer sheet has also strengthened the mechanical property of composite nano materials, can improve it as the tribological property of kollag.Graphene nanometer sheet and SnS in addition
2compound, due to large ∏ key and the SnS of graphene nanometer sheet
2the interaction of Electronic Structure, can form the electronic structure between a kind of new different material, and the electrons height delocalization of participation role, is conducive to the quick transmission of electronics in chemical reaction process.This graphene nanometer sheet and SnS
2composite nano materials as electrode material electrochemistry storage lithium, electrochemistry storage magnesium and catalyst carrier etc., have a wide range of applications and strengthen the performance of improvement.
(2) in course of reaction of the present invention, stannic oxide/graphene nano sheet in-situ reducing becomes graphene nanometer sheet, and reacts the stannic disulfide nano material forming with Situ Hydrothermal and be compounded to form composite material.Its advantage is: graphite oxide nanometer sheet contains abundant oxygen-containing functional group (as: hydroxyl, carbonyl and carboxyl etc.), in hydro-thermal reaction solution, after ultrasonic dispersion, no longer easily again reunited or be deposited in together, and the functional group on graphite oxide surface can be adsorbed on tin ion on the surface of graphite oxide nanometer sheet by complexing, in reproducibility hydrothermal reaction process, can be that generated in-situ graphene nanometer sheet and stannic disulfide nano material height are evenly compound.
(3) Cys contains a plurality of functional group (as: NH
2,-COOH and-SH), these functional groups can provide coordination atom and ion to form coordinate bond.Therefore, Cys can with solution in tin ion form coordination.While is due to the existence of stannic oxide/graphene nano sheet in solution, just formed the coordination mode of stannic oxide/graphene nano sheet-tin ion-Cys, can be evenly compound nano material of generated in-situ graphene nanometer sheet and stannic disulfide nano material height in reproducibility hydrothermal reaction process.
(4) synthesizing graphite alkene nanometer sheet of the present invention and SnS
2the method of composite nano materials be also advantageous in that: by adjusting the ratio of synthetic solvent Raw, can obtain graphene nanometer sheet and the SnS of different proportion
2composite nano materials, graphene nanometer sheet and SnS
2the difference of nano material ratio can be adjusted SnS
2the degree of crystallinity of nano material, makes the application of its applicable different field.
(5) for the present invention, stannic oxide/graphene nano sheet, Cys etc. are raw material, adopt Situ Hydrothermal reducing process to synthesize graphene nanometer sheet and SnS
2composite nano materials, this has the simple feature of reaction condition mild process.Synthesizing graphite alkene nanometer sheet of the present invention and SnS
2composite nano materials as the electrode material of new forms of energy battery lithium ion battery, electrochemistry storage Development of Magnesium Electrode Materials catalyst carrier, have a wide range of applications.
Accompanying drawing explanation
Fig. 1 graphene nanometer sheet and SnS
2the SEM of composite nano materials and TEM pattern.
(a) SnS of embodiment 1 preparation
2the SEM of nano material and TEM pattern;
(b) graphene nanometer sheet and the SnS of embodiment 1 preparation
2the SEM of composite nano materials and TEM pattern, graphene nanometer sheet and SnS
2the ratio of amount is 2: 1.
Fig. 2 graphene nanometer sheet and SnS
2the XRD figure of composite nano materials.
(a) XRD of the synthetic graphene nanometer sheet of embodiment 1 comparative example;
(b) graphene nanometer sheet and the SnS of embodiment 1 preparation
2the XRD figure of composite nano materials, graphene nanometer sheet and SnS
2the ratio of amount is 2: 1;
(c) the synthetic SnS of embodiment 1 comparative example
2the XRD figure of nano material.
Embodiment
Embodiment 1: graphene nanometer sheet and SnS
2its preparation method of composite nano materials:
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 4.0mmol (0.048g) graphite powder is distributed in the 20mL concentrated sulfuric acid, adds 0.03g KMnO under stirring
4, institute adds KMnO
4quality be 3 times of graphite, stir 30 minutes, temperature rises to 30 ℃ of left and right, adds 45ml deionized water, stirs 20 minutes, adds the H of 10ml mass concentration 30%
2o
2, stir 5 minutes, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
2) 1.94g (16mmol) Cys is dissolved in 160ml deionized water, then adds 0.70g (2mmol) butter of tin (SnCl
45H
2o), and stir it is dissolved, Cys and SnCl in mixed solution
4mol ratio be 8: 1.Then by the 1st) the prepared graphite oxide nanometer sheet of graphite of 4.0mmol for step (0.048g) adds in this solution, in the amount of substance of graphite raw material used and solution, butter of tin amount ratio is 2: 1, ultrasonic processing 1.0h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, then this mixture is transferred in hydrothermal reaction kettle, at 180 ℃, hydro-thermal reaction is 12 hours, naturally cooling, centrifugation, with deionized water, fully wash rear collection dry, obtain graphene nanometer sheet and SnS
2composite nano materials, graphene nanometer sheet and SnS in composite nano materials
2the ratio of amount be 2: 1.SEM and XRD analysis show that composite material is graphene nanometer sheet and SnS
2composite nano materials.SEM and XRD figure are shown in respectively Fig. 1 and Fig. 2.
With similar hydrothermal method, graphene nanometer sheet and SnS have been synthesized respectively as a comparison
2nano material, and carried out characterizing (seeing Fig. 1 and Fig. 2) with SEM and XRD.
Embodiment 2: graphene nanometer sheet and SnS
2its preparation method of composite nano materials:
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 2.0mmol (0.024g) graphite powder is distributed in the 25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be 4 times of graphite, stir 40 minutes, temperature rises to 33 ℃ of left and right, adds .50ml deionized water, stirs 25 minutes, adds the H of 12ml mass concentration 30%
2o
2, stir 5-10 minute, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
2) 1.22g (10mmol) Cys is dissolved in 150ml deionized water, then adds 0.70g (2mmol) butter of tin (SnCl
45H
2o), and stir it is dissolved, Cys and SnCl in mixed solution
4mol ratio be 5: 1, then by the 1st) the prepared graphite oxide nanometer sheet of graphite of 2.0mmol for step (0.024g) adds in this solution, in the amount of substance of graphite raw material used and solution, the amount ratio of butter of tin is 1: 1, ultrasonic processing 1.5h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, then this mixture is transferred in hydrothermal reaction kettle, reactor is incubated 16 hours at 190 ℃, naturally cooling, centrifugation, with deionized water, fully wash rear collection dry, obtain graphene nanometer sheet and SnS
2composite nano materials, graphene nanometer sheet and SnS in composite nano materials
2the ratio of amount be 1: 1.SEM and XRD analysis show that composite material is graphene nanometer sheet and SnS
2composite nano materials.
Embodiment 3: graphene nanometer sheet and SnS
2its preparation method of composite nano materials
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 4.5mmol (0.054g) graphite powder is distributed in the 25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be 4 times of graphite, stir 50 minutes, temperature rises to 35 ℃ of left and right, adds 50ml deionized water, stirs 30 minutes, adds the H of 20ml mass concentration 30%
2o
2, stir 15 minutes, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
2) 1.454g (12mmol) Cys is dissolved in 150ml deionized water, then adds 0.52g (1.5mmol) butter of tin (SnCl
45H
2o), and stir it is dissolved, Cys and SnCl in mixed solution
4mol ratio be 8: 1, then by the 1st) the prepared graphite oxide nanometer sheet of graphite of 4.5mmol for step (0.054g) adds in this solution, in the amount of substance of graphite raw material used and solution, the ratio of butter of tin is 3: 1, ultrasonic processing 2.0h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, then this mixture is transferred in hydrothermal reaction kettle, reactor is incubated 20 hours at 200 ℃, naturally cooling, centrifugation, with deionized water, fully wash rear collection dry, obtain graphene nanometer sheet and SnS
2composite nano materials, graphene nanometer sheet and SnS in composite nano materials
2the ratio of amount be 3: 1.SEM and XRD analysis show that composite material is graphene nanometer sheet and SnS
2composite nano materials.
Embodiment 4: graphene nanometer sheet and SnS
2its preparation method of composite nano materials:
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 8.0mmol (0.096g) graphite powder is distributed in the 25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be 4 times of graphite, stir 52 minutes, temperature rises to 32 ℃ of left and right, adds 40ml deionized water, stirs 15 minutes, adds the H of 15ml mass concentration 30%
2o
2, stir 8 minutes, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
1) 2.423g (20mmol) Cys is dissolved in 150ml deionized water, then adds 0.70g (2mmol) butter of tin (SnCl
45H
2o), and stir it is dissolved, Cys and SnCl in mixed solution
4mol ratio be 10: 1, then by the 1st) the prepared graphite oxide nanometer sheet of graphite of 8.0mmol for step (0.096g) adds in this solution, in the amount of graphite raw material used and solution, the amount ratio of butter of tin is 4: 1, ultrasonic processing 2.0h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, then this mixture is transferred in hydrothermal reaction kettle, reactor is incubated 18 hours at 200 ℃, naturally cooling, centrifugation, with deionized water, fully wash rear collection dry, obtain graphene nanometer sheet and SnS
2composite nano materials, graphene nanometer sheet and SnS in composite nano materials
2the ratio of amount be 4: 1.SEM and XRD analysis show that composite material is graphene nanometer sheet and SnS
2composite nano materials.
Embodiment 5: graphene nanometer sheet and SnS
2its preparation method of composite nano materials:
1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 10.0mmol (0.12g) graphite powder is distributed in the 25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be 4 times of graphite, stir 40 minutes, temperature rises to 33 ℃ of left and right, adds 50ml deionized water, stirs 25 minutes, adds the H of 12ml mass concentration 30%
2o
2, stir 5-10 minute, through centrifugation, with obtaining graphite oxide nanometer sheet after mass concentration 5%HCl solution, deionized water and acetone cyclic washing;
2) 1.22g (10mmol) Cys is dissolved in 150ml deionized water, then adds 3.50g (10mmol) butter of tin (SnCl
45H
2o), and stir it is dissolved, Cys and SnCl in mixed solution
4mol ratio be 1: 1, then by the 1st) the prepared graphite oxide nanometer sheet of graphite of 10.0mmol for step (0.12g) adds in this solution, in the amount of substance of graphite raw material used and solution, the amount ratio of butter of tin is 1: 1, ultrasonic processing 2.0h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, then this mixture is transferred in hydrothermal reaction kettle, reactor is incubated 20 hours at 200 ℃, naturally cooling, centrifugation, with deionized water, fully wash rear collection dry, obtain graphene nanometer sheet and SnS
2composite nano materials, graphene nanometer sheet and SnS in composite nano materials
2the ratio of amount be 1: 1.SEM and XRD analysis show that composite material is graphene nanometer sheet and SnS
2composite nano materials.
Claims (1)
1. a graphene nanometer sheet and SnS
2composite nano materials, it is characterized in that composite material is by graphene nanometer sheet and SnS
2the compound formation of nano material, graphene nanometer sheet and SnS
2between nano material, the ratio of amount is 1: 1-4: 1;
Described graphene nanometer sheet and SnS
2the preparation method of composite nano materials carry out as follows: the 1) preparation of graphite oxide nanometer sheet: under 0 ℃ of ice bath, 0.015-0.072g graphite powder is distributed in the 20-25mL concentrated sulfuric acid, adds KMnO under stirring
4, institute adds KMnO
4quality be graphite powder 3-4 doubly, stir 30-60 minute, temperature rises to 30-35 ℃, adds 40-50ml deionized water, stirs 20-30 minute, adds the H of 10-15ml mass concentration 30%
2o
2, stir 5-20 minute, through centrifugation, after HCl solution, deionized water and acetone cyclic washing by mass concentration 5%, obtain graphite oxide nanometer sheet;
2) Cys is dissolved in deionized water, then add butter of tin and fully stir and make its dissolving, in solution, the mol ratio of Cys and butter of tin was at 6: 1～12: 1, again by by the 1st) the graphite oxide nanometer sheet for preparing of step adds in this solution, the 1st) step graphite powder amount used is 1: 1～4: 1 with the ratio of the amount of butter of tin, ultrasonic processing 1-2h, graphite oxide nanometer sheet is well dispersed in hydro-thermal reaction solution, this mixture is proceeded in the hydrothermal reaction kettle of inner liner polytetrafluoroethylene and seal, at 180-200 ℃ of reaction 20-36h, the product obtaining is through centrifugation, and with deionized water and absolute ethanol washing, dry, obtain graphene nanometer sheet and SnS
2composite nano materials.
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| CN102522543A (en) * | 2011-12-15 | 2012-06-27 | 清华大学 | Method for preparing nanometer compound of tin disulfide-graphene |
| CN102931402A (en) * | 2012-11-06 | 2013-02-13 | 西北工业大学 | Preparation of rare earth metal-tin sulfide/grapheme negative electrode material for lithium ion batteries |
| CN102969501A (en) * | 2012-11-19 | 2013-03-13 | 上海交通大学 | Application method of binary metal sulfides in chargeable magnesium battery |
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| CN103872375B (en) * | 2014-03-07 | 2017-05-24 | 上海交通大学 | Application method of disulfide in rechargeable magnesium battery |
| CN104646032A (en) * | 2015-02-07 | 2015-05-27 | 南昌航空大学 | Method for preparing SnS2/ZnFe2O4 graphene compound photocatalyst through hydrothermal method |
| CN105869893B (en) * | 2016-04-11 | 2018-06-01 | 河南师范大学 | One step hydrothermal synthesis graphene-SnS2The method of combined counter electrode material |
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| CN108786849B (en) * | 2018-06-08 | 2021-08-17 | 西北师范大学 | Preparation and application of tin sulfide/titanium dioxide composite material |
| CN110010870A (en) * | 2019-04-03 | 2019-07-12 | 山东星火科学技术研究院 | A kind of preparation method of the lithium ion battery negative material of novel graphene/SnS2 composite material |
| CN110194482A (en) * | 2019-06-21 | 2019-09-03 | 安阳师范学院 | Three-dimensional ultra-thin carbon dots/Copper-cladding Aluminum Bar stannic disulfide composite Nano piece preparation method |
| CN111252806B (en) * | 2020-02-14 | 2021-08-13 | 西安交通大学 | Tin disulfide-black phosphorus composite material, preparation method and application thereof |
| CN112133899B (en) * | 2020-09-27 | 2023-03-03 | 南开大学 | Preparation method of tin-antimony sulfide/graphene composite material and application of tin-antimony sulfide/graphene composite material in sodium ion battery cathode |
| CN112786858A (en) * | 2021-01-19 | 2021-05-11 | 安徽光特新材料科技有限公司 | SnS2Preparation method of nano-sheet loaded graphene-based nano composite material |
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| CN101420023B (en) * | 2008-12-11 | 2010-06-09 | 浙江大学 | Electrochemical lithium ionic insertion/deinsertion electrode and production method thereof |
| CN101609884B (en) * | 2009-07-20 | 2011-01-05 | 北京理工大学 | Method for preparing negative pole material SnS2 of lithium ion battery |
| CN101728535A (en) * | 2009-10-30 | 2010-06-09 | 北京化工大学 | Lithium ion battery conducting material and preparation method and application thereof |
| CN101811696B (en) * | 2010-04-28 | 2013-01-02 | 东南大学 | Graphene-supported cobaltosic oxide nano composite material and preparation method thereof |
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