CN107742701A - Graphene titania aerogel composite and its preparation and application - Google Patents
Graphene titania aerogel composite and its preparation and application Download PDFInfo
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- CN107742701A CN107742701A CN201710856115.4A CN201710856115A CN107742701A CN 107742701 A CN107742701 A CN 107742701A CN 201710856115 A CN201710856115 A CN 201710856115A CN 107742701 A CN107742701 A CN 107742701A
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Abstract
The invention provides a kind of graphene titania aerogel composite and its preparation and application.Described graphene titania aerogel composite, it is characterised in that obtained by in-situ polymerization in graphene oxide layer structure growth titanium dioxide nanoparticle.High-specific surface area of the invention by graphene aerogel, the height ratio capacity of sulphur, and nano titanium oxide prepares porous three-dimensional net structure positive electrode to the strong absorption affinity of more lithium sulfides, the chemical property of the shuttle effect that can effectively solve more lithium sulfides, fully raising lithium-sulfur cell.Dependence test result shows, under 0.5C current density, the first circle specific discharge capacity of the positive electrode is 1520mAh/g, and after the circulation of 100 circles, specific discharge capacity remains at 800mAh/g.The invention provides a kind of easy approach, for preparing lithium sulfur battery anode material, and have a good application prospect.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, and in particular to a kind of graphene-titania aerogel composite
Preparation method and application, the material is a kind of high conductivity, the preferable lithium sulfur battery anode material of strong absorption affinity.
Background technology
With the continuous growth of economics of population, demand of the people to the non-renewable fossil energy such as coal, oil, natural gas
Constantly soaring, thus caused lack of energy and problem of environmental pollution become increasingly conspicuous.Secondary cell be able to will be changed by chemical reaction
Can be converted into electric energy, have higher energy conversion efficiency, progressively turn into focus of concern.In numerous secondary electricity
In pond body system, lithium rechargeable battery is because its operating voltage is high, energy density is big, self discharge is small, long lifespan and pollution-free etc.
Advantage, in recent years, very important role is play in transportation system and portable electric appts.Face new energy technology
Rapid development, constantly increases, people are to this electricity in particular with intelligent communication, Internet technical field market potential demand
The performance of chemical energy storage device proposes higher requirement.Anode material for lithium-ion batteries is mainly the metal compound containing lithium at present
Thing, such as cobalt acid lithium, LiFePO4 etc., height ratio capacity, high ratio modulus these requirements can not be met.Therefore, find next
In generation, has more high-energy-density density, and environmental pollution is low and the positive electrode of rich reserves turns into further lifting lithium ion battery
The key of specific energy density.Elemental sulfur is as positive electrode, the high theoretical specific capacity with 1675mAh/g, it is considered to be most
Potential positive electrode material of lithium secondary cell of future generation.In addition, elemental sulfur also has, toxicity is low, abundant, valency is stored in the earth's crust
The advantages such as lattice are cheap and environment-friendly, therefore the positive electrode by the use of elemental sulfur as lithium secondary battery is extraordinary selection.Lithium
Sulphur battery has high theory than energy, can reach 2600Wh/kg, is conventional lithium ion battery energy density (LiCoO2/ C electricity
The theoretical energy density of pond body system is 387Wh/kg) as many as 5 times, thus in terms of large-scale energy storage and electrokinetic cell have it is huge
Big application prospect.
However, the extensive adaptability of lithium-sulfur cell is also by the low electronic conductivity of various limitations, such as sulphur simple substance at present
With the large volume change of the sulfur electrode during circulation.In addition, in charge and discharge process, sulfur electrode is simultaneously unstable, can generate solvable
Intermediate product --- more lithium sulfides of property, shuttle between negative pole and positive pole, and are chemically reacted with cathode of lithium, cause
The deterioration of battery performance.And the potential safety issue of lithium anode, these all hinder the commercialization hair of lithium-sulfur cell
Exhibition and application.Therefore, how sulphur positive electrode is modified, increases the electron conduction of sulphur and reduce the shuttle of polysulfide
Effect turns into enhancing lithium-sulfur cell cycle life, improves the key point of battery high rate performance.
Therefore, nano titanium oxide is dispersed on graphene sheet layer, original by this problem by a step chemical synthesis
Position is prepared for graphene-titania aerogel composite.By the high-specific surface area high conductivity of graphene, and dioxy
Change the strong absorption affinity of titanium, pass through the dual interface chemical physical action to more lithium sulfides, it is suppressed that its migration and expansion to negative pole
Dissipate, so as to improve the chemical properties such as the cycle efficieny of lithium-sulfur cell, high rate performance and coulombic efficiency.
The content of the invention
It is an object of the invention to provide a kind of preparation process is environmentally friendly, preparation cost is cheap, electrochemical performance stone
Black alkene-titania aerogel composite and its preparation method and application.
In order to achieve the above object, the invention provides a kind of graphene-titania aerogel composite, its feature
It is, is obtained by in-situ polymerization in graphene oxide layer structure growth titanium dioxide nanoparticle.
In order to achieve the above object, the invention provides a kind of preparation of graphene-titania aerogel composite
Method, it is characterised in that including：
Step 1：Graphene oxide solution is prepared using graphene oxide aqueous dispersion liquid and deionized water；
Step 2：Measure butyl titanate to add in absolute ethyl alcohol, be configured to butyl titanate-ethanol solution；
Step 3：Measure butyl titanate-ethanol solution to be added in graphene oxide solution, obtained mixed solution is stirred
Mix, be put into hydrothermal reaction kettle and carry out home position polymerization reaction, by in-situ polymerization in graphene oxide layer structure growth nanometer
Titanium dioxide granule, taken out after being cooled to room temperature, obtain titanium dioxide-graphene hydrogel；
Step 4：Above-mentioned titanium dioxide-graphene hydrogel is washed into 2~3 times with deionized water and absolute ethyl alcohol respectively to remove
Decontamination, it is put into freeze drier and is freeze-dried afterwards, takes out, obtain graphene-titania aerogel composite.
Preferably, the concentration of described graphene oxide solution is 1-3mg/mL.
Preferably, described butyl titanate-ethanol solution concentration is 0.005-0.015mol/L.
Preferably, the volume ratio of butyl titanate-ethanol solution and graphene oxide solution is 1: 15- in described step 3
25。
Preferably, the mixing time in described step 3 is 2-4h.
Preferably, the reaction temperature in described step 3 is 150-200 DEG C, reaction time 8-16h.
Preferably, the temperature of described freeze-drying is -30~-50 DEG C, and freeze-drying vacuumizes simultaneously, and vacuum is
0.1~0.15 support, drying time are 24~72h.
Present invention also offers above-mentioned graphene-titania aerogel composite to make the electrode of lithium-sulfur cell
Application in material.
The present invention realizes nano-metal-oxide titanium dioxide by the method for in-situ polymerization in graphene base body material
It is scattered, by controlling reactant concentration, reaction temperature and time, realize pattern of the titanium dioxide in graphene base body material surface
With the regulation and control of structure.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) preparation process of the present invention is simple and environmentally-friendly, easily operated, is a kind of Green Chemistry preparation method.
(2) experimental design of the present invention is ingenious, using highly conductive graphene as matrix, by one-step synthesis in graphene
Superficial growth nano titanium oxide prepares the aeroge combination electrode material with excellent electrochemical activity, while makes full use of gas
The continuous three-dimensional net structure that gel rubber material is connected with each other, change the pattern and dispersed of reaction condition regulation and control nano titanium oxide
Condition.
(3) graphene-titania aerogel composite prepared by the present invention has higher electric conductivity, stronger
Adsorption capacity, and stable cycle performance and high rate performance, it is the ideal electrode material of lithium-sulfur cell.
(4) present invention is by the high-specific surface area of graphene aerogel, the height ratio capacity of sulphur, and nano titanium oxide pair
The strong absorption affinity of more lithium sulfides prepares porous three-dimensional net structure positive electrode, can effectively solve the shuttle effect of more lithium sulfides
Should, the abundant chemical property for improving lithium-sulfur cell.Dependence test result shows, under 0.5C current density, the positive pole material
The first circle specific discharge capacity of material is 1520mAh/g, and after the circulation of 100 circles, specific discharge capacity remains at 800mAh/g.This
Invention provides a kind of easy approach, for preparing lithium sulfur battery anode material, and has a good application prospect.
Brief description of the drawings
Fig. 1 is the SEM figures of graphene-titania aerogel in the present invention.(a, b TiO2- GA, c, d TiO2-GA-
1, e, f TiO2-GA-2)；
Fig. 2 is the TEM figures of graphene in the present invention-titania aerogel composite, and titanium dioxide nano-particle is equal
It is even to be dispersed on graphene sheet layer.(a, b TiO2- GA, c, d TiO2- GA-1, e, f TiO2-GA-2)
Fig. 3 is the XRD of graphene in the present invention-titania aerogel composite.
Fig. 4 is the CV curves of graphene in the present invention-titania aerogel composite.
Fig. 5 is that discharge and recharge of graphene in the present invention-titania aerogel composite under 0.5C current densities is bent
Line chart.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
A kind of graphene-titania aerogel composite, by using in-situ polymerization in graphene oxide layer knot
Structure growth of nano titanium dioxide particle obtains.
The preparation method of above-mentioned graphene-titania aerogel composite, is concretely comprised the following steps：
Step 1：Weigh 10g graphene oxides aqueous dispersion liquid (on carbon paddy wish, GO-1,10mg/g) and add beaker, and
40mL deionized waters are measured in beaker, are made into 2mg/mL graphene oxide solutions；
Step 2：Measure butyl titanate to add in absolute ethyl alcohol, be configured to butyl titanate-second that concentration is 0.010mol/L
Alcoholic solution；
Step 3：Measure 1mL butyl titanates-ethanol solution to be slowly added into 20mL graphene oxide solutions, by what is obtained
Mixed solution is sufficiently stirred 3h on magnetic stirrer, is put into hydrothermal reaction kettle and carries out home position polymerization reaction, and reaction temperature is
180 DEG C, reaction time 12h, by in-situ polymerization in graphene oxide layer structure growth titanium dioxide nanoparticle, cooling
Taken out after to room temperature, obtain titanium dioxide-graphene hydrogel；
Step 4：Above-mentioned titanium dioxide-graphene hydrogel is washed into 2~3 times with deionized water and absolute ethyl alcohol respectively to remove
Decontamination, it is put into freeze drier and is freeze-dried afterwards, the temperature of freeze-drying is -40 DEG C, and freeze-drying vacuumizes simultaneously,
Vacuum is 0.1 support, drying time 48h, takes out, obtains graphene-titania aerogel composite, be designated as TiO2-
GA。
Embodiment 2
20mg glucose will be added in graphene oxide solution in step 1 in embodiment 1, remaining is with embodiment 1, most
The composite obtained eventually, is designated as TiO2-GA-1。
Embodiment 3
The concentration of butyl titanate-ethanol solution in embodiment 1 is changed to 0.05mol/L, remaining is with embodiment 1, most
The composite obtained eventually, is designated as TiO2-GA-2。
Use SEM (SEM), transmission electron microscope (TEM), X-ray diffractometer (XRD), battery testing
System characterizes the pattern of the preparation-obtained graphene-titania aerogel composite of the present invention and structure and as lithium
The chemical property of the positive electrode of sulphur battery, its result are as follows：
(1) SEM test results show：The accordion graphite with layer structure can be observed under relatively low enlargement ratio
Alkene lamella, this lamellar structure have good electric conductivity and chemical property.(accompanying drawing 1) is in addition, can be clearly visible stone in figure
Three-dimensional porous structure is presented in black alkene-titania aerogel, and this structure can provide the passage that electronics quickly transmits, be advantageous to electricity
Solve the quick diffusion of liquid and lithium ion, it is most important that macroporous structure can effectively adsorb caused more lithium sulfides, suppress its
Transfer and diffusion between both positive and negative polarity.
(2) TEM test results show：It can be seen that graphene film Rotating fields thin and full of fold in low power lens picture.
(accompanying drawing 2) high power lens picture, which can be clearly observed graphene-titania aerogel and contain, to be largely dispersed on graphene sheet layer
Titanium dioxide nano-particle, size is in 3-5nm or so, and the interplanar distance of titanium dioxide nano-particle is 0.35nm, right
Should be in (101) crystal face of anatase titania.
(3) XRD test results show：Occurs (101) crystallographic plane diffraction peak of anatase titania in 2 θ=25.3 °.It is (attached
Fig. 3)
(4) Electrochemical results show：It was found from cyclic voltammetry curve, in the reduction process first of positive pole, 2.01V
With occur two reduction peaks at 2.25V, correspond respectively to two discharge platforms of sulfur electrode.Reduction peak at 2.25V be by
Ring-type S8It is converted into long-chain Li2Sx(4≤x≤8) are formed, and second reduction peak is in 2.01V or so, corresponding to the Li of liquid phase2Sx
It is converted into the Li of solid phase2S2And Li2S.It is basically identical that cyclic voltammetry curve can be seen that by the circulation of 5 times, illustrate the material
Electrochemical process has good stability.(accompanying drawing 4) under 0.5C current density, the first circle of positive electrode electric discharge specific volume
Measure as 1520mAh/g, after the circulation of 100 circles, specific discharge capacity remains at 800mAh/g.(accompanying drawing 5) is compared to tradition
Sulphur carbon electrode, the capability retention of graphene-titania aerogel composite increases.
Claims (9)
1. a kind of graphene-titania aerogel composite, it is characterised in that by in-situ polymerization in graphene oxide sheet
Rotating fields growth of nano titanium dioxide particle obtains.
2. the preparation method of graphene-titania aerogel composite described in claim 1, it is characterised in that including：
Step 1：Graphene oxide solution is prepared using graphene oxide aqueous dispersion liquid and deionized water；
Step 2：Measure butyl titanate to add in absolute ethyl alcohol, be configured to butyl titanate-ethanol solution；
Step 3：Measure butyl titanate-ethanol solution to be added in graphene oxide solution, obtained mixed solution is stirred, put
Enter and home position polymerization reaction is carried out in hydrothermal reaction kettle, by in-situ polymerization in graphene oxide layer structure growth nanometer titanium dioxide
Titanium particle, taken out after being cooled to room temperature, obtain titanium dioxide-graphene hydrogel；
Step 4：Above-mentioned titanium dioxide-graphene hydrogel is washed 2~3 times with deionized water and absolute ethyl alcohol respectively and removes impurity elimination
Matter, it is put into freeze drier and is freeze-dried afterwards, takes out, obtain graphene-titania aerogel composite.
3. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
The concentration for the graphene oxide solution stated is 1-3mg/mL.
4. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
Butyl titanate-the ethanol solution concentration stated is 0.005-0.015mol/L.
5. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
The volume ratio of butyl titanate-ethanol solution and graphene oxide solution is 1: 15-25 in the step 3 stated.
6. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
Mixing time in the step 3 stated is 2-4h.
7. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
Reaction temperature in the step 3 stated is 150-200 DEG C, reaction time 8-16h.
8. the preparation method of graphene as claimed in claim 2-titania aerogel composite, it is characterised in that institute
The temperature for the freeze-drying stated is -30~-50 DEG C, and freeze-drying vacuumizes simultaneously, and vacuum is 0.1~0.15 support, when drying
Between be 24~72h.
9. graphene-titania aerogel composite described in claim 1 is in the electrode material for making lithium-sulfur cell
Application.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108493422A (en) * | 2018-04-02 | 2018-09-04 | 清华大学深圳研究生院 | A kind of sulfur functionalization porous graphene macroscopic view block materials and preparation method thereof |
| CN109037657A (en) * | 2018-08-18 | 2018-12-18 | 复旦大学 | A kind of lithium sulfur battery anode material and preparation method thereof |
| CN109860476A (en) * | 2018-12-11 | 2019-06-07 | 华南师范大学 | Lithium-sulfur cell colloidal tio 2 modified diaphragm and preparation method thereof and lithium-sulfur cell |
| CN110164697A (en) * | 2018-03-01 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of preparation method for the graphene-based composite material can be used for photoelectric conversion |
| CN111454691A (en) * | 2020-04-14 | 2020-07-28 | 大连理工大学 | Graphene/amorphous titanium dioxide nanorod composite material, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109860476A (en) * | 2018-12-11 | 2019-06-07 | 华南师范大学 | Lithium-sulfur cell colloidal tio 2 modified diaphragm and preparation method thereof and lithium-sulfur cell |
| CN111454691A (en) * | 2020-04-14 | 2020-07-28 | 大连理工大学 | Graphene/amorphous titanium dioxide nanorod composite material, preparation method and application thereof |
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