CN107732211A - A kind of silica nanosphere/graphene composite material and preparation method thereof - Google Patents

A kind of silica nanosphere/graphene composite material and preparation method thereof Download PDF

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Publication number
CN107732211A
CN107732211A CN201710993220.2A CN201710993220A CN107732211A CN 107732211 A CN107732211 A CN 107732211A CN 201710993220 A CN201710993220 A CN 201710993220A CN 107732211 A CN107732211 A CN 107732211A
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nanosphere
reaction solution
sio
composite material
mixed
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杨友文
高远皓
刘继广
方晓刚
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Hefei University of Technology
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Hefei University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a kind of silica nanosphere/graphene composite material and preparation method thereof, its be using tetraethyl orthosilicate as silicon source, under alkaline solution, high temperature hydro-thermal reaction reduction-oxidation graphite, fabricated in situ SiO2Nanosphere/graphene composite material, wherein SiO2The diameter of nanosphere is between 150 250nm.The raw material that the present invention uses is cheap, easily operated, and step is less, and equipment is simple, is easy to industrialized production.

Description

A kind of silica nanosphere/graphene composite material and preparation method thereof
Technical field
The invention belongs to technical field of function materials, and in particular to SiO2The preparation of nanosphere/graphene composite material.
Background technology
Silica (SiO2) a kind of acid nonmetal oxide is used as, its existence form mainly has two kinds：Crystalline state SiO2 With amorphous state (unformed) SiO2.The SiO of crystal habit2Be primarily present among quartz mine, generally with quartz, cristobalite and Phosphorus quartz variant is stored within ore, amorphous Si O2It is primarily present within diatomite and flint.SiO2Existence form is not Together, key factor is in SiO2In Si-O keys composition form it is different.Crystal form SiO2Chemical property it is relatively stable, be because Its space structure forms covalent bond between Si and O and forms orderly state, and the bond energy of Si-O keys is higher, it is difficult to be broken. And amorphous SiO2Space structure be then random continuous network structure, inflated shape is not of uniform size in network structure Hole, Si-O keys have longer bond distance so that its bond energy is relatively low, therefore amorphous SiO2Compared to the SiO of crystalline state2Have Higher activity.
At present, SiO2It is mainly used in electronic package material, resin composite materials, coating etc..Led because itself is relatively low Electrical property, SiO2It is considered as being difficult as among electrode material always.With technological progress, research finds to influence SiO2Electrochemistry The main reason for performance is SiO2The granular size and crystal structure of itself.Work as SiO2Scantling is reduced to nanoscale even 100 nanometers are less than, its electron energy level and band structure can all change.Meanwhile with the reduction of size, SiO2Surface is former The ratio regular meeting of son increases therewith, so as to increase the specific surface area of material so that the surface energy and activity of material have largely Enhancing.SiO is worked as in the discoveries such as Otto Zhou2, can be in 0-1.0V (vs.Li when the yardstick of particle reaches Nano grade+/ Li) area It is interior to be reacted with lithium ion, and there is about 400mAhg-1Reversible capacity.Aishui Yu seminars pass through in SiO2Table Bread covers one layer of carbon film, forms a kind of nano material of clad structure, applied to steady with good circulation in lithium ion battery It is qualitative.Amorphous SiO is made using hydro-thermal method in Zhaoxiang Wang seminars2With C (HC/SiO2) nano composite material, make Good performance is also shown for lithium ion battery negative material.Guiyun Yi etc. are with tetraethyl orthosilicate (TEOS) and oxidation Graphite is raw material, and SiO is prepared into an acidic solution using hydro-thermal method2Nanoparticle/graphene composite material, and present good Good absorption property.Xiucheng Zheng etc. prepare the amorphous Si O of 3D structures using one pot of hydro-thermal method2/ graphene is compound Aeroge, and because of the design feature such as its is porous, specific surface area is big, improve the chemical property of material.
The present invention intends structure SiO2Nanosphere/graphene composite structure material, using graphite oxide as raw material, positive silicic acid tetrem Ester is that silicon source, ethanol and deionized water are solvent, NaOH control solution ph, and high temperature hydro-thermal reaction prepares SiO2/ graphene Nano composite structure.Raman test results can show that graphene has the less number of plies, test structure table in composite construction Face, the composite prepared possess preferable cycle performance and high rate performance.
The content of the invention
A kind of the present invention is intended to provide SiO2Nanosphere/graphene composite material and preparation method thereof, it is intended to using hydro-thermal Method combination calcination processing obtains SiO2Nanosphere/graphene composite material.
The present invention solves technical problem, adopts the following technical scheme that：
Silica nanosphere/graphene composite material of the present invention, is that amorphous state is closely attached with graphene SiO2Nanosphere, the SiO2A diameter of 150nm~250nm of nanosphere.
The preparation method of inventive silica nanosphere/graphene composite material, it is to carry out as follows：
A, measure 30mL ethanol and 3mL deionized water is sufficiently mixed, be configured to ethanol/water mixed solution；By 30mg Graphite oxide be added in the ethanol/water mixed solution, add 25mg surfactant sodium dodecyl base benzene sulfonic acid sodium salt (SDS) mixed reaction solution A, is obtained；
The mixed reaction solution A is placed in 0 DEG C of ice bath to ultrasonic, the oxidation stone in the mixed reaction solution A Ink is completely dissolved, and obtains mixed reaction solution B；
B, 25mL tetraethyl orthosilicate (Si (OC are measured2H5)4), it is slowly dropped in the mixed reaction solution B, then 3mg NaOH is added, ultrasonic 15min, obtains mixed reaction solution C；
By the mixed reaction solution C magnetic stirrer 2h, the mixed reaction solution C transfers after being then sufficiently stirred Into 100mL ptfe autoclave liner, 160 DEG C of pyroreaction 12h；
C, after reaction terminates, reactor is cooled to room temperature, gained black product is stirred with ethanol, centrifuged, cleaned, then is passed through 60 DEG C of dry 12h, that is, obtain target product SiO2Nanosphere/graphene composite material.
Using composite obtained by the present invention as active material, carrying out the method for electrochemical property test is：By preparation After active material, conductive black and Kynoar (PVDF) in mass ratio 7: 2: 1 mix, 1-METHYLPYRROLIDONE is added (NMP) uniform slurry is mixed and made into, is evenly coated on copper foil, after drying, is washed into 10mm or so circular electric pole piece.Then it is electric Pond is assembled into button cell using lithium metal as being microporous polypropylene membrane (Celgard2300) to electrode, barrier film.The perseverance of battery Stream charge-discharge test is carried out on the new prestige multichannel battery charging and discharging tester in Shenzhen.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, the present invention is raw materials used cheap, and the solvent used is deionized water and ethanol, greatly reduces cost；
2nd, the present invention in hydro-thermal reaction and subsequent processes, do not increase any additive, reduce production process and Production equipment, and hydro-thermal reaction and calcination processing time are shorter, reduce energy consumption；
3rd, the SiO obtained by the present invention in composite2Nanosphere is relatively large in diameter, and pattern is complete, and between composite It is tightly combined；
4th, present invention gained composite possesses preferable cycle performance and high rate performance.
5th, the inventive method is simple and environmentally-friendly, is easy to large-scale production.
Brief description of the drawings
Fig. 1 is native graphite (a), graphite oxide (b) and SiO2The X-ray diffraction of nanosphere/graphene composite material (c) Collection of illustrative plates (XRD).
Fig. 2 is graphite oxide (b) and SiO2The laser Raman spectroscopy (Raman) of nanosphere/graphene composite material (a), There are two obvious characteristic peaks in two Raman spectrum, be D peaks and G peaks respectively.
Fig. 3 is SiO2The FE-SEM figures of nanosphere/graphene composite material.
Fig. 4 is SiO2The thermal analysis curue (TG) of nanosphere/graphene composite material.
Fig. 5 is SiO2The nitrogen adsorption desorption curve and graph of pore diameter distribution of nanosphere/graphene composite material.
Fig. 6 is SiO2The constant current cycle performance curve of nanosphere/graphene composite material.
Embodiment
Careful explanation is carried out to technical scheme below by embodiment and accompanying drawing.
Embodiment 1
The present embodiment SiO2The specific preparation process of nanosphere/graphene composite material is as follows：
1st, graphite oxide is prepared using Hummers methods：By improved Hummers methods, 1g graphite is weighed, is put into vacuum Drying box dries 12h, by the concentrated sulfuric acid (the dense H of the concentration 98% of dried graphite and 46mL2SO4) pour into three-necked flask, put 30min is stirred in ice bath to stirring；Then 3g potassium permanganate (KMnO is slowly added in 2h4), continue to stir Mix 4h (during pay attention to keep reaction temperature at 0 DEG C or so).Reaction temperature is raised, keeps bath temperature to maintain 30-35 DEG C, 2h is reacted, is during which stirred continuously；After reaction terminates, 46mL deionized waters are slowly added dropwise into solution, it is stirring while adding, promote Ionized water fully dissolves；Continue to raise reaction temperature, keep bath temperature to maintain 90-95 DEG C, react 15min；Finally stop Heating, deionized water is added dropwise into solution with dilute solution, and the hydrogen peroxide solution that appropriate concentration is 3% is added dropwise until solution It is constant in golden yellow and holding.It is 1 with volume ratio after solution is filtered：10 aqueous hydrochloric acid solution fully washs, and filters three It is secondary.Obtained product is washed with deionized and repeatedly rises to 5 to solution ph, it is abundant that solution finally is put into vacuum drying chamber After drying, obtained product is graphite oxide.
2nd, solution is prepared：Measure 30mL ethanol and 3mL deionized water is sufficiently mixed, it is molten to be configured to ethanol/water mixing Liquid；30mg graphite oxide is added in ethanol/water mixed solution, adds 25mg surfactant sodium dodecyl base benzene sulphur Sour sodium, obtain mixed reaction solution A；
Mixed reaction solution A is placed on ultrasound in 0 DEG C of ice bath, until the graphite oxide in mixed reaction solution A is completely molten Solution, obtain mixed reaction solution B；
25mL tetraethyl orthosilicate is measured, is slowly dropped in mixed reaction solution B, then adds 3mg NaOH, is surpassed Sound 15min, obtain mixed reaction solution C；
By mixed reaction solution C magnetic stirrer 2h, well mixed solution is obtained.
3rd, hydro-thermal reaction：Mixed reaction solution C after being sufficiently stirred is transferred to 100mL ptfe autoclave liner In, 160 DEG C of pyroreaction 12h；
4th, after reaction terminates, reactor is cooled to room temperature, gained black product is stirred with ethanol, centrifuged, cleaned three times, Again through 60 DEG C of dry 12h, that is, obtain target product SiO2Nanosphere/graphene composite material.
Appearance structure characterizes：
A, X-ray diffraction (XRD) is analyzed：XRD analysis have been carried out to sample using D/MAX-2500V types X-ray diffractometer, Cu-K α radiation sourcesScanning range is 10-80 °.
B, field emission scanning electron microscope (FESEM) is analyzed：The sample ultrasonic of gained is scattered in ethanol solution, dripped On silicon chip, then naturally dry at room temperature.Silicon chip is pasted onto to the pattern that sample is observed on SEM sample stages with conducting resinl.
C, laser Raman spectroscopy (Raman) is analyzed：Instrument uses excitation wavelength 532nm visible laser, scanning range 0- 4000cm-1。
D, thermogravimetric (TG) is analyzed：There are many materials that matter often occurs during heating or cooling to some temperature Amount change, passes through the mass change in different temperatures scope, it is possible to authenticate the material composition of sample and quantitative analysis material Mass ratio, it is the important means of COMPOSITE MATERIALS heat endurance.Sample is positioned under nitrogen protective condition, with 10 DEG C/min Heating rate be heated to 1000 DEG C from room temperature and tested.
E, specific surface area and pore structure (BET) analysis：Specific surface area is the gross area possessed by unit mass material, porous Nano material has higher specific surface area, and instrument analyzes sample under -196 DEG C of liquid nitrogen temperatures.
Fig. 1 is native graphite (a), graphite oxide (b) and SiO2The X-ray diffraction of nanosphere/graphene composite material (c) Collection of illustrative plates (XRD).SiO is can be seen that from Fig. 1 c2The XRD of nanosphere/graphene composite material is at θ=22.5 ° of the angle of diffraction 2 There is a wider disperse peak, this is the SiO of amorphous state2Characteristic peak, be amorphous structure so as to prove obtained sample.
Fig. 2 is graphite oxide (b) and SiO2The laser Raman spectroscopy (Raman) of nanosphere/graphene composite material (a). Compare two and scheme it can be found that the intensity at two peaks of composite is all significantly improved, while the position at two peaks Also there occurs slight skew.The D peaks of graphite oxide are located at 1323cm-1, G peaks are located at 1586cm-1, and the D peak positions of composite In 1343cm-1, G peaks are located at 1584cm-1。
Fig. 3 is SiO2The FE-SEM figures of nanosphere/graphene composite material.As can be seen from Figure, shape in composite Into SiO2Pattern be chondritic, average diameter is about 200nm, SiO2Nanosphere being adhered to each other tightly.
Fig. 4 is SiO2The thermal analysis curue (TG) of nanosphere/graphene composite material.It is main from 300 DEG C to 1000 DEG C in section The mass loss wanted comes from graphene and thermally decomposed, to remaining weight at 1000 DEG C than 42.52% be mainly SiO2。
Fig. 5 is SiO2The nitrogen adsorption desorption curve and graph of pore diameter distribution of nanosphere/graphene composite material, can be with from figure Find out that the hysteresis loop of the nitrogen adsorption desorption curve map of composite is larger, H4 types are presented.The ratio of material is calculated by BET method Surface area is 480.880m2/ g, hole average diameter are 2.587nm.
Fig. 6 is SiO2The constant current cycle performance curve of nanosphere/graphene composite material.It is from figure it can be found that multiple The cycle performance of condensation material is relatively stable, and in second of cyclic process, coulombic efficiency has just risen to 91.4%.50 circulations Afterwards, irreversible capacity is down to 222.3mAg-1, coulombic efficiency is then 99.19%.
The exemplary embodiment of the present invention is these are only, is not intended to limit the invention, all spirit in the present invention With all any modification, equivalent and improvement made within principle etc., it should be included in the scope of the protection.

Claims (2)

  1. A kind of 1. silica nanosphere/graphene composite material, it is characterised in that：The composite is tightened in graphene It is close to be attached with amorphous Si O2Nanosphere, the SiO2A diameter of 150nm~250nm of nanosphere.
  2. 2. the preparation method of silica nanosphere/graphene composite material described in a kind of claim 1, it is characterised in that press Following steps are carried out：
    A, measure 30mL ethanol and 3mL deionized water is sufficiently mixed, be configured to ethanol/water mixed solution；By 30mg oxygen Graphite is added in the ethanol/water mixed solution, is added 25mg surfactant sodium dodecyl base benzene sulfonic acid sodium salt, is obtained mixed Close reaction solution A；
    The mixed reaction solution A is placed on ultrasound in 0 DEG C of ice bath, until the graphite oxide in the mixed reaction solution A is complete Fully dissolved, obtain mixed reaction solution B；
    B, 25mL tetraethyl orthosilicate is measured, is slowly dropped in the mixed reaction solution B, then adds 3mg NaOH, Ultrasonic 15min, obtain mixed reaction solution C；
    By the mixed reaction solution C magnetic stirrer 2h, the mixed reaction solution C after being then sufficiently stirred is transferred to In 100mL ptfe autoclave liner, 160 DEG C of pyroreaction 12h；
    C, after reaction terminates, reactor is cooled to room temperature, gained black product is stirred with ethanol, centrifuged, cleaned, then through 60 DEG C 12h is dried, that is, obtains target product SiO2Nanosphere/graphene composite material.
CN201710993220.2A 2017-10-23 2017-10-23 A kind of silica nanosphere/graphene composite material and preparation method thereof Pending CN107732211A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109244412A (en) * 2018-09-21 2019-01-18 上海理工大学 The preparation method of fold silica/graphene composite powder particle and its composite material, fold silica

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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
CN106328892A (en) * 2016-08-30 2017-01-11 安徽师范大学 Preparation method of silicon dioxide/graphene nanocomposite, negative electrode of lithium ion battery and lithium ion battery

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Publication number Priority date Publication date Assignee Title
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
CN106328892A (en) * 2016-08-30 2017-01-11 安徽师范大学 Preparation method of silicon dioxide/graphene nanocomposite, negative electrode of lithium ion battery and lithium ion battery

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN109244412A (en) * 2018-09-21 2019-01-18 上海理工大学 The preparation method of fold silica/graphene composite powder particle and its composite material, fold silica
CN109244412B (en) * 2018-09-21 2021-09-28 上海理工大学 Folded silicon dioxide/graphene composite powder particle, composite material thereof and preparation method of folded silicon dioxide

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