CN109286009B - Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material - Google Patents

Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material Download PDF

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CN109286009B
CN109286009B CN201811119950.0A CN201811119950A CN109286009B CN 109286009 B CN109286009 B CN 109286009B CN 201811119950 A CN201811119950 A CN 201811119950A CN 109286009 B CN109286009 B CN 109286009B
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殷立雄
蔺英
程如亮
张浩繁
黄剑锋
白培杰
李慧敏
宋佳琪
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
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    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
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    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • H01M4/5815Sulfides
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method of a nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material, which comprises the steps of preserving heat of melamine for 2-6 h at the temperature of 450-650 ℃, grinding for later use when the melamine is naturally cooled to room temperature, dispersing the melamine in ethanol to obtain a suspension, centrifuging the suspension, washing the suspension for a plurality of times by using deionized water and absolute ethyl alcohol, and then drying in vacuum to obtain a product g-C3N4The product g-C3N4Dissolving in deionized water, stirring, ultrasonic dispersing to obtain suspension A, adding PVP into suspension A, stirring to completely dissolve to obtain solution B, adding TAA and SnCl4·2H2Adding O into the solution B, uniformly stirring to form a solution C, carrying out microwave hydrothermal reaction on the solution C, obtaining a precursor after the reaction is finished, respectively centrifugally washing the precursor for a plurality of times by deionized water and absolute ethyl alcohol, and then carrying out vacuum drying to obtain the nanosheet self-assembled three-dimensional nanoflower SnS2/g‑C3N4A battery material.

Description

Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material
Technical Field
The invention relates to a preparation method of a lithium ion battery cathode material, in particular to a preparation method of a nanosheet self-assembled three-dimensional nanoflower tin sulfide/graphitized carbon nitride lithium ion battery cathode material.
Background
A lithium ion battery, as a rechargeable secondary battery, mainly operates by deintercalation of lithium ions between a positive electrode and a negative electrode. In addition, the lithium ion battery has the advantages of high working voltage, long cycle life, large specific capacity, good safety performance, small self-discharge, no memory effect and the like. This advantage makes it widely used in portable devices such as mobile phones, cameras, notebook computers, etc. In recent years, the use of lithium ion batteries in the fields of new energy automobiles, electric tools, aerospace, energy storage and the like has been gradually expanded through continuous development and improvement in the aspects of charge and discharge capacity, rate characteristics, cycle performance and the like of the lithium ion batteries. Therefore, lithium ion batteries can become a main direction of development of secondary batteries in the future. The negative electrode material of the lithium ion battery is an important component of the lithium ion battery, and the composition and the structure of the negative electrode material have decisive influence on the electrochemical performance of the lithium ion battery. This has therefore made the development of suitable battery materials important.
SnS2Is a binary compound belonging to the IV: VI main group and is composed of hexagonal basic units CdI2The layered crystal structure (unit cell parameters: a: 0.3648nm, c: 0.5899nm) is composed of a sandwich structure (S-Sn-S) of two layers of hexagonally close-packed sulfide ions with tin ions added in the middle. One tin ion is inserted into every six sulfide ions to form a regular octahedral coordination, and weak van der waals forces exist between layers and are bound by covalent bonds. In addition, the layered structure has many crystal vacancies, which can be used as the host lattice of intercalation. This unique layered structure gives it excellent photovoltaic characteristics. Currently, researchers prepare SnS with different structures or sizes through different methods2The main structure of the nano-composite material is tin disulfide nano-particles, nanospheres, nano-sheets, nano-tubes and nano-tubesZero-dimensional, one-dimensional, two-dimensional or three-dimensional nanostructures such as plates, and even more complex multilevel micro-nano structures. The unique properties of these different structures are utilized to prepare semiconductor materials, photocatalytic materials, solar cell materials, photoelectric conversion system materials, lithium ion battery materials, and the like. Unique performance and wide application of SnS2Materials have become one of the most promising materials. Moreover, SnS2Due to its high theoretical capacity (690 mAh. g)-1) The lithium ion battery cathode material has the advantages of abundant natural resources, no toxicity and low cost, is considered as a promising candidate of a new generation of cathode material, but has the defects of poor conductivity, large volume expansion in the charge and discharge process and the like of most cathode materials, and the development of the lithium ion battery cathode material is limited. In view of its major drawbacks, we have compounded it with highly conductive materials or electrode designs to improve their electrochemical cycling performance.
g-C3N4Is a carbon material with a two-dimensional (2D) graphene structure, which is a nitrogen heteroatom substituted graphite skeleton and is sp-substituted by single atoms of carbon and nitrogen2Hybrid formation, with a unique planar structure, has attracted considerable attention due to its abundant porous structure, high nitrogen content, large surface area, cost-effective availability and remarkable physical and chemical properties. And the preparation process is simple and the cost is lower. Therefore, the object is to provide a conductive material containing g-C3N4As support material in charging and discharging processes with SnS2The conductivity and the structural stability of the composite material are improved, and the electrochemical performance of the composite material as a lithium ion battery cathode material is further improved. At present, many scholars pass through the complex g-C3And N is compounded to prepare the novel composite electrode material so as to improve the electrochemical performance of the battery.
At present, Li et al [ Li X, Feng Y, Li M, et al2GeO4Nanoparticles and Ultrathin g-C3N4Layers:Synergistic Lithium Storage and Excellent Electrochemical Performance[J].Advanced Functional Materials,2016,25(44):6858-6866.]Prepared Zn2GeO4/g-C3N4The compound is at 200mA g-1The capacity of the capacitor reaches 1370mAh g after the capacitor is cycled for 140 times under the current density-1At a high current density of 2000mA g-1Has excellent rate capability and capacity of 950 mAh.g-1(ii) a Senthil et al [ Chenrayan, K.S.Chandra, S.Manickam, Ultrathin MoS2sheets supported on N-rich carbon nitride nanospheres with enhanced lithium storage properties,Applied Surface Science,410(2017)215-224.]Prepare MoS2/g-C3N4The nanosphere is used as a negative electrode material, and the composite material has excellent electrochemical performance at 100 mA.g-1The reversible capacity after 50 cycles under the current density is 857mAh g -1; the current preparation method mainly comprises a solvothermal method [ Enzho Liu, Jibing Chen a, Yongning Ma., et al2/g-C3N4heterojunction with enhanced H2evolution during photocatalytic water splitting,Journal of Colloid and Interface Science[J].524(2018)313–324Journal of Catalysis,352(2017)532-541.]Ion exchange method [ Liu Y, Chen P, Chen Y, et al. in situ ion-exchange synthesis of SnS2/g-C3N4nanosheets heterojunction for enhancing photocatalytic activity[J].Rsc Advances,2016,6(13).]. The solvent thermal reaction method is an improved hydrothermal reaction method, an organic solvent is used for replacing the traditional water as a solvent, but the condition of solvent heat is strictly controlled in the reaction process; the ion exchange method can generate excessive regeneration waste liquid, the period is longer, the salt consumption is large, and the ion exchange resin is polluted by the existence of organic matters.
Disclosure of Invention
The invention aims to provide a preparation method of a nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material, which overcomes the defects in the prior art2/g-C3N4The size of the battery cathode material reaches about fifty nanometers, the purity is high, the crystallinity is strong, the appearance is uniform, and the battery cathode material has excellent charge-discharge rate performance when being applied to a lithium ion battery cathodeCan be used.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material comprises the following steps:
1) keeping the temperature of melamine at the temperature of 450-650 ℃ for 2-6 h, and grinding for later use when the melamine is naturally cooled to room temperature;
2) dispersing the product obtained in the step 1) in ethanol to obtain a suspension, centrifuging the suspension, washing the suspension for a plurality of times by using deionized water and absolute ethyl alcohol, and then drying the suspension in vacuum to obtain the product g-C3N4
3) The product g-C3N4Dissolving in deionized water, stirring, and performing ultrasonic dispersion to form a suspension A;
4) PVP is added to suspension A and stirred until completely dissolved to form solution B, in which the product g-C3N4The mass ratio of PVP to PVP is (30 mg-50 mg): (0.4 g-0.6 g);
5) according to the element mole ratio nS:nSn=2 (0.5-2) adding TAA and SnCl4·5H2Adding O into the solution B, and uniformly stirring to form a solution C;
6) carrying out microwave hydrothermal reaction on the solution C, and obtaining a precursor after the reaction is finished;
7) respectively centrifugally washing the precursor for a plurality of times by deionized water and absolute ethyl alcohol, and then drying in vacuum to obtain the nano-sheet self-assembled three-dimensional nano flower SnS2/g-C3N4A battery material.
Further, in the step 2), 30-50 mg of the product obtained in the step 1) is dispersed in 40-60 mL of ethanol.
Further, the vacuum drying temperature in the step 2) is 60-100 ℃, and the time is 8-14 h.
Further, 30-50 mg of product g-C is dissolved in every 40-60 mL of deionized water in the step 3)3N4
Further, in the step 5), 1-2.85 g of SnCl is added into every 40-60 mL of the solution B4·5H2O。
Further, the microwave hydrothermal reaction in the step 6) is specifically as follows: and (3) sealing the solution C in a microwave hydrothermal reaction kettle, controlling the filling ratio to be 40-60%, placing the solution C in a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 160-200 ℃ and the reaction time to be 1-5 h.
Further, the vacuum drying temperature in the step 7) is 80 ℃, and the time is 12 hours.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention has the advantages of faster reaction rate, full and thorough reaction, controllable grain growth, uniform size distribution and the like due to the assistance of microwaves and the full and uniform mixing of a hydrothermal method, and overcomes the defects of high energy consumption, difficult reaction control, impure products and the like of the traditional method2/g-C3N4The lithium ion battery cathode material has the particle size of about several nanometers, and has the advantages of low preparation cost, high controllable degree, low energy consumption, high production efficiency and high yield, and the g-C coated on the surface of stannous sulfide3N4Can relieve SnS2The volume change and the charge and discharge performance in the charge and discharge process are excellent, the first discharge capacity can reach about 640.2mAh/g under the current density of 100mA/g, the capacity can be kept about 440.6mAh/g after circulation for 40 times, and the high-stability lithium ion battery has high stability under the high current density.
Drawings
FIG. 1 is SnS prepared according to example 2 of the present invention2/g-C3N4SEM image of battery negative electrode material;
FIG. 2 is SnS prepared according to example 2 of the present invention2/g-C3N4A TEM image of the battery anode material;
FIG. 3 shows the nano-sheet self-assembled three-dimensional nano flower-like SnS prepared in example 3 of the present invention2/g-C3N4A rate performance diagram of the lithium ion battery cathode composite material.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of a nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material comprises the following steps:
1) placing 5-15 g of melamine in a crucible with a cover, placing the crucible in a muffle furnace, preserving heat for 2-6 h at the temperature of 450-650 ℃, keeping the temperature rise rate at 2 ℃/min, and placing a yellow product in a mortar for grinding when the yellow product is naturally cooled to room temperature;
2) and then dispersing the mixture in ethanol for 2 hours under vigorous stirring, and dispersing 30-50 mg of the product obtained in the step 1) in every 40-60 mL of ethanol. And then, centrifuging the suspension, washing the suspension for several times by using deionized water and absolute ethyl alcohol, and then drying the suspension for 8-14 h in vacuum at the temperature of 60-100 ℃. The yellow product g-C is finally obtained3N4
3) 30-50 mg g-C3N4Dissolving in 40-60 ml of deionized water, stirring strongly for 5 hours, and carrying out ultrasonic dispersion for 3 hours. Forming a suspension A;
4) then slowly adding 0.4-0.6 g of PVP (polyvinylpyrrolidone) into the suspension A, and magnetically stirring for 10 minutes until the PVP is completely dissolved to form a solution B;
5) according to the element mole ratio nS:nSn2 (0.5-2) mixing TAA (thioacetamide) and SnCl4·5H2Adding O into the solution B, and adding 1-2.85 g SnCl into every 40-60 mL of the solution B4·5H2O, magnetically stirring for 30min to form a solution C;
6) putting the solution C into a microwave hydrothermal reaction kettle, sealing, controlling the filling ratio to be 40-60%, putting into a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 160-200 ℃ and controlling the reaction time to be 1-5 h;
7) after the reaction is finished, taking out the precursor, respectively centrifugally washing the precursor for 3 times by deionized water and absolute ethyl alcohol, and drying the precursor for 12 hours in vacuum at the temperature of 80 ℃ to obtain the SnS2/g-C3N4And (3) precursor.
The present invention is described in further detail below with reference to examples:
example 1
1) Placing 5g of melamine in a crucible with a cover, placing the crucible in a muffle furnace, preserving heat for 2h at 450 ℃, keeping the heating rate at 2 ℃/min, and placing a yellow product in a mortar for grinding when the melamine is naturally cooled to room temperature;
2) it is subsequently dispersed in ethanol for 2 hours with vigorous stirring, with 30mg of product from step 1) per 40mL of ethanol. Subsequently, the suspension was centrifuged and washed several times with deionized water and absolute ethanol, and then dried under vacuum at 60 ℃ for 8 h. The yellow product g-C is finally obtained3N4
3) 30mg of g-C3N4Dissolving in 40ml deionized water, stirring vigorously for 5h, and ultrasonic dispersing for 3 h. Forming a suspension A;
4) then 0.4g PVP (polyvinylpyrrolidone) is slowly added into the suspension A, and the mixture is magnetically stirred for 10 minutes until the mixture is completely dissolved to form a solution B;
5) according to the element mole ratio nS:nSn2:0.5 TAA (thioacetamide) and SnCl4·2H2O was added to the above solution B, 1g of SnCl was added per 40mL of the solution B4·5H2O, magnetically stirring for 30min to form a solution C;
6) putting the solution C into a microwave hydrothermal reaction kettle, sealing, controlling the filling ratio to be 40%, putting into a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 160 ℃ and the reaction time to be 1 h;
7) after the reaction is finished, taking out the precursor, respectively centrifugally washing the precursor for 3 times by deionized water and absolute ethyl alcohol, and drying the precursor for 12 hours in vacuum at the temperature of 80 ℃ to obtain the SnS2/g-C3N4And (3) precursor.
Example 2
1) Placing 10g of melamine in a crucible with a cover, placing the crucible in a muffle furnace, preserving heat for 4h at 550 ℃, keeping the heating rate at 2 ℃/min, and placing a yellow product in a mortar for grinding when the melamine is naturally cooled to room temperature;
2) it is subsequently dispersed in ethanol for 2 hours with vigorous stirring, 40mg of the product obtained in step 1) being dispersed per 50mL of ethanol. Subsequently, the suspension was centrifuged and washed several times with deionized water and absolute ethanol, and then dried under vacuum at 80 ℃ for 12 h. The yellow product g-C is finally obtained3N4
3) Will be provided with40mg g-C3N4Dissolving in 50ml deionized water, stirring vigorously for 5h, and ultrasonic dispersing for 3 h. Forming a suspension A;
4) then 0.5g PVP (polyvinylpyrrolidone) is slowly added into the suspension A, and the mixture is magnetically stirred for 10 minutes until the mixture is completely dissolved to form a solution B;
5) according to the element mole ratio nS:nSn=2:1 reaction of TAA (Thioacetamide) with SnCl4·2H2O was added to the above solution B, 2.85g of SnCl was added per 60mL of the solution B4·5H2O, magnetically stirring for 30min to form a solution C;
6) putting the solution C into a microwave hydrothermal reaction kettle, sealing, controlling the filling ratio to be 50%, putting into a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 180 ℃ and the reaction time to be 3 h;
7) after the reaction is finished, taking out the precursor, respectively centrifugally washing the precursor for 3 times by deionized water and absolute ethyl alcohol, and drying the precursor for 12 hours in vacuum at the temperature of 80 ℃ to obtain the SnS2/g-C3N4And (3) precursor.
From FIG. 1, it can be seen that SnS is prepared2/g-C3N4The battery cathode material is a nano-sheet self-assembly three-dimensional nanoflower, the thickness of the nano-sheet is about 50nm, the size of the nano-sheet self-assembly three-dimensional nanoflower is about 500nm, the result is consistent with SEM (scanning electron microscope) as shown in figure 2, and SnS with a nano-sheet self-assembly three-dimensional nanoflower-shaped structure can be shown in figure 32/g-C3N4The lithium ion battery cathode composite material has slow capacity attenuation of the battery under different current densities and has certain cycle stability.
Example 3
1) Placing 15g of melamine in a crucible with a cover, placing the crucible in a muffle furnace, preserving heat for 6h at 650 ℃, keeping the temperature rise rate at 2 ℃/min, and placing a yellow product in a mortar for grinding when the melamine is naturally cooled to room temperature;
2) it is subsequently dispersed in ethanol for 2 hours with vigorous stirring, with 50mg of the product obtained in step 1) per 60mL of ethanol. Subsequently, the suspension was centrifuged and washed several times with deionized water and absolute ethanol, and then vacuumed at 100 ℃And drying for 14 h. The yellow product g-C is finally obtained3N4
3) 50mg of g-C3N4Dissolving in 60ml deionized water, stirring strongly for 5h, and ultrasonic dispersing for 3 h. Forming a suspension A;
4) then 0.6g PVP (polyvinylpyrrolidone) is slowly added into the suspension A, and the mixture is magnetically stirred for 10 minutes until the mixture is completely dissolved to form a solution B;
5) according to the element mole ratio nS:nSn=2:2 reaction of TAA (Thioacetamide) with SnCl4·2H2O was added to the above solution B, 2g of SnCl was added per 50mL of the solution B4·5H2O, magnetically stirring for 30min to form a solution C;
6) putting the solution C into a microwave hydrothermal reaction kettle, sealing, controlling the filling ratio to be 60%, putting into a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 200 ℃ and the reaction time to be 5 hours;
7) after the reaction is finished, taking out the precursor, respectively centrifugally washing the precursor for 3 times by deionized water and absolute ethyl alcohol, and drying the precursor for 12 hours in vacuum at the temperature of 80 ℃ to obtain the SnS2/g-C3N4And (3) precursor.

Claims (1)

1. A preparation method of a nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material is characterized by comprising the following steps:
1) keeping the temperature of melamine at the temperature of 450-650 ℃ for 2-6 h, and grinding for later use when the melamine is naturally cooled to room temperature;
2) dispersing the product obtained in the step 1) in ethanol to obtain a suspension, dispersing 30-50 mg of the product obtained in the step 1) in 40-60 mL of ethanol, centrifuging the suspension, washing the suspension for several times by using deionized water and absolute ethyl alcohol, and then drying in vacuum to obtain a product g-C3N4(ii) a The vacuum drying temperature is 60-100 ℃, and the time is 8-14 h;
3) the product g-C3N4Dissolving the mixture in deionized water, and dissolving 30-50 mg of product g-C in every 40-60 mL of deionized water3N4Stirring and then ultrasonically dispersing to form a suspension A;
4) PVP is added to suspension A and stirred until completely dissolved to form solution B, in which the product g-C3N4The dosage ratio of PVP to PVP is (30 mg-50 mg): (0.4 g-0.6 g);
5) according to the element mole ratio nS:nSn=2 (0.5-2) adding TAA and SnCl4·5H2Adding O into the solution B, and adding 1-2.85 g of SnCl into every 40-60 mL of the solution B4·5H2O, uniformly stirring to form a solution C;
6) putting the solution C into a microwave hydrothermal reaction kettle, sealing, controlling the filling ratio to be 40-60%, putting into a microwave hydrothermal reaction instrument, controlling the reaction temperature to be 160-200 ℃, controlling the reaction time to be 1-5 h, and obtaining a precursor after the reaction is finished;
7) respectively centrifugally washing the precursor for several times by deionized water and absolute ethyl alcohol, and then drying in vacuum at 80 ℃ for 12h to obtain the nanosheet self-assembled three-dimensional nanoflower SnS2/g-C3N4A battery material.
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