CN109859960B - Sulfonated graphene-based carbon-coated lithium titanate composite material and preparation and application thereof - Google Patents
Sulfonated graphene-based carbon-coated lithium titanate composite material and preparation and application thereof Download PDFInfo
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- CN109859960B CN109859960B CN201711238386.XA CN201711238386A CN109859960B CN 109859960 B CN109859960 B CN 109859960B CN 201711238386 A CN201711238386 A CN 201711238386A CN 109859960 B CN109859960 B CN 109859960B
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Abstract
The invention relates to a sulfonated graphene-based carbon-coated lithium titanate composite material and preparation and application thereof, wherein the composite material consists of lithium titanate, carbon and sulfonated graphene, wherein Li is4Ti5O12The mass content of the sulfonated graphene and carbon in the composite material is 92-98%, the mass content of the sulfonated graphene and carbon in the composite material is 2-8%, the mass ratio of the sulfonated graphene to the carbon is (2-4): 1, and the carbon-coated lithium titanate is attached to the sulfonated graphene. Compared with the prior art, the electronic conductivity and the ionic conductivity of the lithium titanate are improved, so that the synthesized sulfonated graphene-based carbon-coated lithium titanate (S-GNS/C @ LTO) has excellent rate capability.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a negative electrode material for a lithium ion supercapacitor.
Background
An electrochemical super capacitor is an energy storage device working based on a double electric layer or a Faraday quasi-capacitance mechanism, and has the advantages of high charging and discharging speed, high power density, long cycle life, wide working temperature range and the like, so that the electrochemical super capacitor is widely concerned. Compared with a lithium ion battery, the electrochemical capacitor has relatively low energy density but long cycle life, and is widely applied to the fields of electric automobile starting devices, pulse power supplies, mobile standby power supplies and the like. With hybrid electric vehicles and their demands for high power density and energy density, lithium ion supercapacitors have gained more and more attention as a new type of energy storage device. However, since the lithium ion supercapacitor uses both electrodes of the lithium ion battery and the supercapacitor, it has dual characteristics, and has advantages of higher energy density than that of a conventional capacitor and higher power density than that of the lithium ion battery. Therefore, the lithium ion super capacitor is expected to be used in the fields of energy type high-power electronic products such as electric automobiles, spaceflight, military affairs and the like.
As a negative electrode material of a lithium ion supercapacitor, lithium titanate has the following advantages: (1) in the process of charging and discharging, along with the insertion and the extraction of lithium ions, lithium titanate hardly undergoes volume change, so that the lithium titanate is called a zero-strain material; (2) due to its lithium insertion platform (1.55V (vs. Li/Li)+) Higher than the reduction potential of most organic electrolytes, so that the safety problems caused by SEI formation and lithium dendrites can be effectively avoided. However, Li4Ti5O12The low conductivity and the small lithium ion diffusion coefficient lead to poor charge and discharge performance under high multiplying power, thereby limiting the wide application of lithium titanate; the graphene with a single layer or a few layers has excellent conductivity, and the conductivity of the graphene can be remarkably improved by compounding the graphene with lithium titanate, so that the rate capability of the graphene is improved. However, graphene is extremely easy to agglomerate in the process of synthesizing the composite material, and the excellent conductivity of graphene cannot be well exerted.
Disclosure of Invention
The invention provides sulfonated graphene-based carbon-coated Li, aiming at solving the problems that the lithium titanate negative electrode material prepared by the existing method is poor in rate capability and graphene is easy to agglomerate in the process of synthesizing a composite material4A Ti5O12 composite anode material and a preparation method thereof.
In order to achieve the above object, the present invention has the following specific technical solutions,
carbon coating of Li on sulfonated graphene4In the Ti5O12 composite anode material, Li4Ti5O12The mass content of the composite negative electrode material is 92-98%, and the total mass content of the sulfonated graphene and the carbon in the composite material is 2-8%. The mass ratio of the sulfonated graphene to the carbon is (2-4:) to 1.
The optimum mass content of each component in the sulfonated graphene-based carbon-coated lithium titanate composite material obtained by the invention is as follows: li4Ti5O1295%, sulfonated graphene and carbon 5%, the ratio of sulfonated graphene to carbon being 3: 1. Among the surfactants used, CTAB is most effective.
The preparation method of the sulfonated graphene and carbon comprises the following steps:
(1) weighing a titanium source and a lithium source according to the mass ratio of the titanium element to the lithium element of 5 (4-5), and dissolving the titanium source and the lithium source in distilled water, wherein the lithium source is one or a mixture of more than two of lithium carbonate, lithium acetate and lithium hydroxide; the titanium source is one or a mixture of tetrabutyl titanate, butyl titanate or tetra-n-butyl titanate; the solvent is one or more of methanol, ethanol, isopropanol and ethylene glycol;
(2) dispersing sulfonated graphene (sulfonated graphene) in distilled water, and carrying out ultrasonic treatment for 0.1-1 h;
(3) adding the solution obtained in the step (2) into a surfactant aqueous solution with a certain mass fraction (0.2-0.8 wt%), stirring and heating for 10-25h at 25-60 ℃;
(4) adding the solution obtained in the step (1) into the solution obtained in the step (3), stirring while adding, transferring the solution into a 30-100mL high-pressure reaction kettle after stirring for 2-5h, and reacting for 10-25h at the temperature of 100-; drying the white precipitate obtained after centrifugation at 60-120 ℃ for 6-12 h; finally calcining for 3-12 h at the temperature of 600-900 ℃ in a reducing atmosphere to obtain the sulfonated graphene-based carbon-coated lithium titanate composite material;
the surfactant is one or more of Dodecyl Trimethyl Ammonium Bromide (DTAB), octadecyl trimethyl ammonium bromide (STAB), hexadecyl trimethyl ammonium bromide (CTAB), Tetradecyl Trimethyl Ammonium Bromide (TTAB), and Dioctadecyl Dimethyl Ammonium Chloride (DDAC).
The mass concentration of the lithium source in the solvent in the step (1) is 10-80g/L, and the mass of the sulfonated graphene in the step (2) accounts for 1-5g/L of the volume of the solvent.
In the step (2), the power of the ultrasonic wave is 200-700W, and the stirring speed in the step (3) is 100-400 rpm.
The reducing atmosphere in the step (3) is H2And inert atmosphere gas, wherein the volume concentration of the hydrogen gas in the total mixed gas is 1-10%, and the inert atmosphere gas is one or more than two of argon, helium or nitrogen.
The sulfonated graphene-based carbon-coated lithium titanate composite material is used as an active ingredient for a negative electrode material of a lithium ion supercapacitor.
The beneficial results of the invention are as follows: 1) compared with the common graphene, the sulfonated graphene can be well dispersed in solvents such as water without external acting force (such as ultrasonic dispersion), so that the steps in material synthesis are simplified. However, during the material synthesis process, the sulfonated graphene may be agglomerated, which may result in insufficient exertion of its excellent conductivity. According to the invention, the sulfonated graphene is subjected to intercalation treatment (surfactant is used as an intercalation agent) aiming at the problem that the sulfonated graphene is easy to agglomerate in the composite material synthesis process, so that the surfactant modified sulfonated graphene with a pillared layer structure is obtained firstly, and the agglomeration phenomenon is not easy to occur when the sulfonated graphene is used for a conductive matrix due to the supporting effect of the surfactant between material layers, so that the uniform dispersion of the composite material on the surface is ensured;
2) in the preparation process, a hydrothermal method is adopted, and a certain amount of high-conductivity substance sulfonated graphene is added into a mixture of a titanium source and a lithium source at the same time, so that Li4Ti5O12The particles grow in situ on the surface of the conductive agent, so that the ionic conductivity is improved, and Li can be effectively prevented4Ti5O12Thereby obtaining a relatively pure phase Li4Ti5O12Smaller particles. The introduced surfactant intercalates the sulfonated graphene, effectively avoids the agglomeration of the sulfonated graphene, and enables Li4Ti5O12The particles can be uniformly grown on the sulfonated graphene sheet layer, and the surfactant is calcined at high temperature and then is added into Li4Ti5O12Forming a conductive carbon layer on the surface of the particles to increase Li4Ti5O12Electron conductivity of (2). In conclusion, the electronic conductivity and the ionic conductivity of the lithium titanate are improved simultaneously, so that the synthesized sulfonated graphene-based carbon-coated lithium titanate (S-GNS/C @ LTO) has excellent rate capability, and the synthesized material can be used in the field of lithium ion supercapacitors.
The sulfonated graphene is used as a conductive matrix of the composite material, so that the ionic conductivity of the material is improved; in addition, the introduced surfactant intercalates the sulfonated grapheneLayer, effectively avoiding agglomeration of sulfonated graphene, so that Li4Ti5O12The particles can be uniformly grown on the sulfonated graphene sheet layer, and the surfactant is calcined at high temperature and then is added into Li4Ti5O12Forming a conductive carbon layer on the surface of the particles to increase Li4Ti5O12Electron conductivity of (2).
Drawings
Fig. 1 is a graph comparing rate performance of lithium ion supercapacitors assembled by the negative electrode materials of example 1, comparative example 1 and comparative example 2.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
Example 1:
the sulfonated graphene-based carbon-coated lithium titanate (S-GNS/C @ LTO) of the present example was prepared by the following steps:
(1) weighing 16.5mL of butyl titanate and 3.46g of lithium acetate, and respectively dispersing in 200mL of distilled water;
(2) weighing 0.309g of sulfonated graphene, placing the sulfonated graphene in a beaker filled with 200mL of distilled water, and carrying out ultrasonic treatment for 0.5h at the power of 600W;
(3) adding the solution obtained in the step (2) into a surfactant CTAB aqueous solution with the mass fraction of 0.4 wt%, stirring and heating at the same time for 24h and at the temperature of 45 ℃;
(4) adding the solution obtained in the step (1) into the solution obtained in the step (3), stirring while adding, transferring the solution into a high-pressure reaction kettle after stirring for 5 hours, and reacting for 15 hours at a certain temperature (120 ℃); drying the white precipitate obtained after centrifugation at 80 ℃ for 12 h; and finally calcining for 10 hours at the temperature of 700 ℃ in a reducing atmosphere to obtain the sulfonated graphene-based carbon-coated lithium titanate composite material which is marked as S-GNS/C @ LTO.
The raw materials used in this example are all commercially available products.
And (3) performance testing:
1) mixing the prepared sulfonated graphene-based carbon-coated lithium titanate material, Super P and PVDF in a ratio of 8:1:1Using N-methyl pyrrolidone as solvent, magnetically stirring at 400rpm for 4h to obtain electrode slurry, coating the electrode slurry on aluminum foil to control the supporting amount to 3.5mg/cm2Vacuum drying at 100 deg.C for 12 hr, and punching into 7.7cm long and 5cm wide electrode sheet with a punching machine.
2) Uniformly mixing the activated carbon, the SuperP and the (CMC + SBR) in a mass ratio of 85:10:5, magnetically stirring for 4 hours at a speed of 400rpm by using water as a solvent to obtain electrode slurry, and coating the electrode slurry on an aluminum foil to control the supporting amount to be 8 mg/cm2Vacuum drying at 100 deg.C for 12 hr, and punching into 7.5cm long and 5cm wide electrode sheet with a punching machine.
3) And folding the positive and negative pole pieces and the polypropylene diaphragm into a rectangular electrode group of the lithium ion supercapacitor, injecting electrolyte, and packaging by using an aluminum plastic film.
The electrolyte used in this example is a commercial lithium ion battery electrolyte, wherein the lithium salt is lithium hexafluorophosphate, and the solvent is a mixed solution of EC, DEC and DMC in a volume ratio of 1:1: 1.
Example 2:
the sulfonated graphene-based carbon-coated lithium titanate composite material and the battery are prepared by the same method as the example 1, except that the content of the sulfonated graphene is 3% by mass.
Example 3: the sulfonated graphene-based carbon-coated lithium titanate composite material and the battery are prepared by the same method as the example 1, except that the content of the surfactant is 0.3% by mass.
Example 4: the same method as in example 1 was used to sulfonate graphene-based carbon-coated lithium titanate composite materials and batteries, except that the content of sulfonated graphene (sulfonated graphene) was 7% by mass.
Comparative example 1: the pure-phase lithium titanate material is used as a negative electrode to assemble the battery, and the preparation method and the battery assembly method of the lithium titanate are the same as those in the embodiment 1.
Comparative example 2: the preparation method of lithium titanate and the battery assembly are the same as those in example 1 by using the unmodified sulfonated graphene/LTO material as a negative electrode to assemble the battery.
Comparative example 3: the same preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material and the battery as in example 1 was adopted, except that the preparation method of the composite material: the solid phase method comprises the following specific steps:
(1) weighing titanium dioxide and lithium carbonate according to the stoichiometric ratio of 5 (4-4.5), taking ethanol as a dispersing agent, and uniformly mixing the weighed titanium source and lithium source;
(2) weighing 0.309g of sulfonated graphene, placing the sulfonated graphene in a beaker filled with 200mL of distilled water, and carrying out ultrasonic treatment for 0.5h at the power of 600W;
(3) adding the solution obtained in the step (2) into a surfactant CTAB aqueous solution with the mass fraction of 0.4 wt%, stirring and heating at the same time for 24h and at the temperature of 45 ℃;
(4) adding the solution obtained in the step (1) into the solution obtained in the step (3), and then placing the solution into a ball mill for ball milling, wherein the ball-to-material ratio is 4:1, and the ball milling time is 12 hours;
(5) and drying the ball-milled slurry at 80 ℃, calcining the dried slurry at 900 ℃ for 24 hours in an argon atmosphere, and obtaining a sample, namely the sulfonated graphene-based carbon-coated lithium titanate composite material, which is marked as S-GNS/C @ LTO-1.
Performance evaluation results and analysis:
the lithium titanate materials obtained in example 1, comparative example 1 and comparative example 2 were subjected to rate capability tests (the three materials were respectively named as S-GNS/C @ LTO, LTO and S-GNS @ LTO), and the test results show that: the rate capability of the CTAB-S-GNS @ LTO material is obviously improved because the specific capacity of other two materials is still 110mAh/g under the discharge rate of 30C. The reason is that after the sulfonated graphene and sulfonated graphene are subjected to intercalation modification by adopting a surfactant CTAB, the conductivity of the sulfonated graphene is fully exerted, lithium titanate can be uniformly dispersed on the sulfonated graphene of a conductive matrix during later synthesis, and after the CTAB is calcined at high temperature, a conductive carbon layer is formed on the surface of LTO particles, so that the electronic conductivity of the LTO material is improved, and the multiplying power performance of the CTAB-S-GNS @ LTO is optimal.
Claims (7)
1. The sulfonated graphene-based carbon-coated lithium titanate composite material is characterized in that: the composite material is composed of lithium titanate, carbon and sulfonated graphene, wherein Li4Ti5O12The mass content of the sulfonated graphene and carbon in the composite material is 92-98%, the mass content of the sulfonated graphene and carbon in the composite material is 2-8%, the mass ratio of the sulfonated graphene to the carbon is (2-4): 1, and the carbon-coated lithium titanate is attached to the sulfonated graphene;
the composite material is prepared by the following steps,
(1) weighing a titanium source and a lithium source according to the mass ratio of the titanium element to the lithium element of 5 (4-5), and dissolving the titanium source and the lithium source in distilled water, wherein the lithium source is one or a mixture of more than two of lithium carbonate, lithium acetate and lithium hydroxide; the titanium source is butyl titanate;
(2) dispersing sulfonated graphene in water, and performing ultrasonic treatment for 0.1-1 h;
(3) adding the solution obtained in the step (2) into an aqueous solution containing 0.2-0.8wt% of a surfactant, stirring and heating for 10-25h at 25-60 ℃, wherein the mass ratio of sulfonated graphene to the surfactant is (1.5-3) to 1;
(3) adding the solution obtained in the step (1) into the solution obtained in the step (3), stirring for 2-5h, transferring the solution into a reaction kettle, and reacting for 10-25h at 100-; drying the white precipitate obtained after centrifugation at 60-120 ℃ for 6-12 h; and finally calcining for 3-12 h at 500-800 ℃ in a reducing atmosphere to obtain the sulfonated graphene-based carbon-coated lithium titanate composite material.
2. The preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material of claim 1, wherein the preparation of the sulfonated graphene-based carbon-coated lithium titanate composite material is performed according to the following steps:
(1) weighing a titanium source and a lithium source according to the mass ratio of the titanium element to the lithium element of 5 (4-5), and dissolving the titanium source and the lithium source in distilled water, wherein the lithium source is one or a mixture of more than two of lithium carbonate, lithium acetate and lithium hydroxide; the titanium source is butyl titanate;
(2) dispersing sulfonated graphene in distilled water, and carrying out ultrasonic treatment for 0.1-1 h; (3) adding the solution obtained in the step (2) into a surfactant aqueous solution with the mass fraction of 0.2-0.8wt%, stirring and heating at 25-60 ℃ for 10-25 h;
(3) adding the solution obtained in the step (1) into the solution obtained in the step (3), stirring while adding, transferring the solution into a reaction kettle after stirring for 2-5h, and reacting for 10-25h at the temperature of 100-; drying the white precipitate obtained after centrifugation at 60-120 ℃ for 6-12 h; and finally calcining for 3-12 h at 500-800 ℃ in a reducing atmosphere to obtain the sulfonated graphene-based carbon-coated lithium titanate composite material.
3. The preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material according to claim 2, characterized in that: the mass concentration of the lithium source in the solvent in the step (1) is 10-80g/L, and the mass of the sulfonated graphene in the step (2) accounts for 1-5g/L of the volume of the solvent.
4. The preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material according to claim 2, characterized in that: in the step (2), the power of the ultrasonic wave is 200-700W, and the stirring speed in the step (3) is 100-400 rpm.
5. The preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material according to claim 2, characterized in that: the reducing atmosphere in the step (3) is H2And inert atmosphere gas, wherein the volume concentration of the hydrogen gas in the total mixed gas is 1-10%, and the inert atmosphere gas is one or more than two of argon, helium or nitrogen.
6. The preparation method of the sulfonated graphene-based carbon-coated lithium titanate composite material according to claim 2, characterized in that: the surfactant is one or more of Dodecyl Trimethyl Ammonium Bromide (DTAB), octadecyl trimethyl ammonium bromide (STAB), hexadecyl trimethyl ammonium bromide (CTAB), Tetradecyl Trimethyl Ammonium Bromide (TTAB), and Dioctadecyl Dimethyl Ammonium Chloride (DDAC).
7. The application of the sulfonated graphene-based carbon-coated lithium titanate composite material of claim 1, is characterized in that: the sulfonated graphene-based carbon-coated lithium titanate composite material is used as an active substance for a negative electrode of a lithium ion supercapacitor.
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| CN101877405A (en) * | 2010-04-20 | 2010-11-03 | 华南理工大学 | Preparation method of lithium titanate-graphene combination electrode material |
| CN103022459A (en) * | 2012-11-27 | 2013-04-03 | 中国科学院大连化学物理研究所 | Preparation method of graphene/lithium titanate composite anode material |
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| CN104393275A (en) * | 2014-12-09 | 2015-03-04 | 江南大学 | Preparation method of carbon-coated lithium titanate battery material |
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| KR101479626B1 (en) * | 2013-05-03 | 2015-01-06 | 삼화콘덴서공업주식회사 | Lithium titanium oxide/carbon composites, lithium titanium oxide/carbon composites manufacturing method, anode active material and hybrid super capacitor using the same |
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| CN101877405A (en) * | 2010-04-20 | 2010-11-03 | 华南理工大学 | Preparation method of lithium titanate-graphene combination electrode material |
| CN103022459A (en) * | 2012-11-27 | 2013-04-03 | 中国科学院大连化学物理研究所 | Preparation method of graphene/lithium titanate composite anode material |
| CN103151505A (en) * | 2013-03-01 | 2013-06-12 | 中国科学院过程工程研究所 | Lithium-titanate composite negative pole material and preparation method thereof |
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