CN106299270B - The preparation and application of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material - Google Patents

The preparation and application of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material Download PDF

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CN106299270B
CN106299270B CN201610705053.2A CN201610705053A CN106299270B CN 106299270 B CN106299270 B CN 106299270B CN 201610705053 A CN201610705053 A CN 201610705053A CN 106299270 B CN106299270 B CN 106299270B
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dimensional grapheme
nano particle
tin
molybdenum
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CN106299270A (en
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何春年
翟朋博
赵乃勤
师春生
刘恩佐
李家俊
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Tianjin University
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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
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 present invention relates to the preparation and application of a kind of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material.The material, by size<The SnO of 10nm2Nano particle uniform load and simultaneously loads on three-dimensional grapheme network<5 layers of MoS2Nanometer sheet forms sandwich structure, and three-dimensional grapheme is with a thickness of 1-10nm, and three-dimensional grapheme network radius is at 1-10 μm.Carbon nanotube prepared by the present invention has excellent electric conductivity.Preparation method process of the present invention is simple, can volume production, the material as lithium ion battery negative material have good charge-discharge performance, high rate performance and stability.

Description

Three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet The preparation and application of material
Technical field
The present invention relates to a kind of three-dimensional grapheme reticular structures to load SnO2Nano particle and MoS2Nanosheet composite material and Preparation and application belong to electrode material of secondary lithium ion battery field.
Background technique
It with the continuous aggravation of energy problem and environmental problem, gets rid of and fossil energy is depended on unduly, gradually utilize electricity Power drive replaces fossil energy to be driven into one main flow direction of today's society.Lithium ion battery as a kind of secondary cell with By means of the advantages that its energy density is big, working range is wide, discharge voltage is high, non-environmental-pollution, memory-less effect, in ni-Cd and ni-mh Show one's talent in the batteries such as battery.Simultaneously because its have extended cycle life, have a safety feature at present be widely used to mobile phone, In the portable devices such as camera, laptop.As hybrid vehicle of new generation (HEV) and pure electric automobile (EV) produce The development of industry has obtained more extensive concern to the research of lithium ion battery.
Graphite is widely applied as negative electrode material in currently used lithium ion battery, theoretical specific capacity 372mAh/g, This lower specific capacity is difficult to meet the needs of high power and energy density electric vehicle.So exploitation has high discharge voltage, High capacity and the novel cathode material for lithium ion battery of long cycle life are particularly important.Wherein, transition metal oxide And sulfide relies on higher theoretical specific capacity, shows one's talent in numerous and complicated negative electrode material.Wherein SnO2Base cathode material Material, theoretical specific capacity are 790mAh/g (Adv.Mater., 2009,21,2536-2539.), simultaneously because having at low cost, peace The advantages that full property is high and receive significant attention, but its fatal weakness be exactly in charge and discharge process due to the insertion of lithium ion and Abjection, can cause the violent expansion (about 340%) of volume itself, to be easy to that active material is caused to occur in cyclic process Dusting, and then cause its cycle performance and high rate performance poor.In addition, MoS2As a kind of typical transient metal sulfide, By higher theoretical specific capacity (670mAh/g), the advantages that excellent stratiform two-dimensional structure, higher Young's modulus and answered For lithium ion battery negative material aspect, but it is similar to other transition metal oxides and sulfide, poor electric conductivity, Biggish volume change limits the performance of its chemical property.
In order to improve these disadvantages of transition metal oxide and sulfide negative electrode material, current main solution has Two：First is that nanosizing, i.e., be crushed it not as far as possible in expansion process in Nano grade the size Control of material, simultaneously The transmission range for shortening electronics and ion improves its electric conductivity；Second is that Composite, mainly by active material and carbon material It carries out compound, compound (different dimensions) including configuration aspects, compound (heterojunction structure) in terms of ingredient, is restricting active material The electric conductivity that carbon material is excellent is utilized while volume expansion；Nanosizing is even more to mention significantly with realization while Composite The performance of high material.A kind of carbon nanomaterial of the carbon nanosheet as two-dimensional structure, since its electric conductivity is excellent, stable structure Property it is good, compared with other zero dimensions, one-dimensional, structure has more active reaction sites, without the best matrix suspected of Composite.And lamella it Between be assembled into three-dimensional grapheme structure then and more could be formed with stereochemical structure conducive to lithium ion and electron-transport, to effectively mention High material chemical property (Adv.Mater., 2012,24:4097).
Summary of the invention
The object of the present invention is to provide a kind of three-dimensional grapheme network structures to load zero dimension SnO2Nano particle and two dimension MoS2 Nanometer sheet material and preparation and application.The material is by structure in carbon covered stannum rice grain uniform load to three-dimensional grapheme network At, preparation method process is simple, can volume production, the material as lithium ion battery negative material have good charge and discharge cycles Performance, high rate performance and stability, have a extensive future.Technical scheme is as follows：
A kind of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material, feature exist In size<The SnO of 10nm2Nano particle uniform load and simultaneously loads on three-dimensional grapheme network<5 layers of MoS2It receives Rice piece forms sandwich structure, and three-dimensional grapheme is with a thickness of 1-10nm, and three-dimensional grapheme network radius is at 1-10 μm.
The three-dimensional grapheme reticular structure carrying tin oxide nano particle of above structure and molybdenum disulfide nano sheet material Preparation method includes the following steps：
(1) with one of citric acid, glucose, sucrose or it is mixed into carbon source, stannous chloride is tin source, and ammonium molybdate is molybdenum Source, thiocarbamide are sulphur source；Wherein the tin molar ratio in the carbon and tin source in carbon source is (50~20):1, tin and NaCl in tin source Mass ratio is (0.01-0.1):1, the molybdenum molar ratio in tin and molybdenum source in tin source is (0.1~1)：1 meter, by carbon source, tin source and NaCl, which is added in deionized water, to be dissolved, while molybdenum source and sulphur source being added in deionized water dissolve respectively, and sulphur is successively added dropwise later Source and molybdenum source solution are uniformly mixed and are placed on refrigerator freezing, then is dried in vacuo, and obtain mixture；
(2) it by mixture grind into powder made from step (1), is laid in Noah's ark, is placed in tube furnace flat-temperature zone and is forged It burns：With N2, He or Ar one kind or mixing be used as inert gas source, be first that 200~400ml/min is passed through indifferent gas with flow Body 10~30 minutes to exclude air；Throughput is fixed as 50~200ml/min later, with the heating speed of 1~10 DEG C/min To 650~800 DEG C, heat preservation 1-8h's degree heating tube furnace is carbonized, and is cooled to room temperature after reaction, obtains calcined product；
(3) calcined product made from collection step (2), it is finely ground, it is washed to until there is no NaCl in calcined product, in temperature It is to be dried at 60~120 DEG C, obtains three-dimensional grapheme network structure load carbon SnO2Nano particle and MoS2Nanometer sheet composite wood Material.
The three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material be applied to lithium from Sub- battery cathode.
The present invention has the following advantages that：The present invention prepares three-dimensional grapheme network structure using raw material cheap and easy to get and loads Carbon SnO2Nano particle and MoS2Nanosheet composite material, low in cost, reaction process is simple, controllability is strong.The material knot simultaneously Structure is uniform, and pattern is excellent, realizes the synergistic effect of multiple material, has excellent performance, and has for negative electrode of lithium ion battery very high Specific capacity and fabulous cycle performance, recycled 100 times under the current density of 2000mA/g and be still able to maintain 750mAh/g or more Specific capacity, and still keep under the high current density of 10A/g the specific capacity of 400mAh/g.
Detailed description of the invention
Fig. 1 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The SEM photograph of piece composite material.From this view it is apparent that three-dimensional grapheme network morphology.
Fig. 2 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The SEM photograph of piece composite material.From this view it is apparent that three-dimensional grapheme piece thickness.
Fig. 3 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The TEM photo of piece composite material.From this view it is apparent that SnO2The smaller size and high dispersion of nano particle.
Fig. 4 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The TEM photo of piece composite material.From this view it is apparent that MoS2 nanometer sheet few number of plies.
Fig. 5 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The HRTEM photo of piece composite material.From this view it is apparent that carbon-coating, SnO2 nano particle and MoS2The sandwich knot of nanometer sheet Structure.
Fig. 6 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The XRD spectrum of piece composite material.
Fig. 7 is that the three-dimensional grapheme network structure that the embodiment of the present invention 1 obtains loads carbon SnO2Nano particle and MoS2Nanometer The Laman map of piece composite material.
Fig. 8 is that the three-dimensional grapheme network structure obtained using the embodiment of the present invention 1 loads carbon SnO2Nano particle and MoS2 The charge-discharge performance figure of negative electrode of lithium ion battery made from nanosheet composite material, in figure：- ■-is charging curve ,- ●-be discharge curve ,-▲-is efficiency curve.
Fig. 9 is that the three-dimensional grapheme network structure obtained using the embodiment of the present invention 1 loads carbon SnO2Nano particle and MoS2 The charge-discharge magnification performance map of negative electrode of lithium ion battery made from nanosheet composite material, in figure：- ■-is charging curve ,- ●-be discharge curve.
Specific embodiment
Particular content of the invention is described as follows combined with specific embodiments below：
Embodiment 1：
2.5g citric acid, 0.394g stannous chloride and 20.0g NaCl are weighed, mixture is dissolved in the deionized water of 80ml In, with the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, while weigh 0.340g ammonium molybdate and 0.352g thiocarbamide is dissolved separately in 10ml deionized water.Ammonium molybdate solution and thiourea solution is successively finally added dropwise with dropper, and Stirring is for 24 hours；The solution mixed is put into refrigerator overnight to freeze, is placed on -50 DEG C of vacuum drying in freeze drier, until Drying obtains mixture.Milled mixtures take the mixed-powder of 10g to be placed in Noah's ark, Noah's ark are put into tube furnace, are passed through The Ar inert gas 20min of 300ml/min excludes air, then with the Ar of 100~200ml/min be protection gas and with 10 DEG C/ The heating rate of min is warming up to 750 DEG C of temperature, and heat preservation 2h carries out carburizing reagent, cooling under Ar atmosphere protection after reaction To room temperature, calcined product is obtained.Calcined product is collected, it is finely ground, it is washed to until there is no NaCl in product, is dried at 80 DEG C, Obtain three-dimensional grapheme network structure load carbon SnO2Nano particle and MoS2Nanosheet composite material, wherein three-dimensional grapheme is thick Degree is 1~10nm, SnO2Nano particle diameter<10nm, MoS2 the nanometer sheet number of plies<5 layers.
With obtained material, PVDF, conductive carbon black mass ratio is 8:1:1 meter is applied to copper sheet as cathode, with 1M's LiPF6Half-cell is made using lithium piece as anode as electrolyte, 100 circles are recycled under the current density of 2000mA/g still The specific capacity of 1000mAh/g or more is kept, as shown in figure 8, and there is excellent circulation performance, in the electric current of 10A/g Still with the specific capacity of 400mAh/g under density, as shown in Figure 9.
Embodiment 2：
1.25g citric acid, 0.197g stannous chloride and 15gNaCl are weighed, mixture is dissolved in the deionized water of 80ml, With the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming；0.227g ammonium molybdate and 0.235g are weighed simultaneously Thiocarbamide is dissolved separately in 10ml deionized water；Ammonium molybdate solution and thiourea solution is successively finally added dropwise with dropper, and stirs 24h；The solution mixed is put into refrigerator overnight to freeze, is placed on -50 DEG C of vacuum drying in freeze drier, until drying Obtain mixture.Milled mixtures take the mixed-powder of 10g to be placed in Noah's ark, Noah's ark are put into tube furnace, are passed through 300ml/ The Ar inert gas 20min of min excludes air, then with the Ar of 100~200ml/min be to protect gas and with the liter of 10 DEG C/min Warm speed is warming up to 750 DEG C of temperature, and heat preservation 2h carries out carburizing reagent, is cooled to room temperature under Ar atmosphere protection after reaction, Obtain calcined product.Calcined product is collected, it is finely ground, it is washed to until there is no NaCl in product, is dried at 80 DEG C, obtain three-dimensional Graphene network structural load carbon SnO2Nano particle and MoS2Nanosheet composite material.
Embodiment 3：
1g citric acid, 0.148g stannous chloride and 15g NaCl are weighed, mixture is dissolved in the deionized water of 80ml, with The magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming, while weighing 0.170g ammonium molybdate and 0.176g sulphur Urea is dissolved separately in 10ml deionized water.Ammonium molybdate solution and thiourea solution is successively finally added dropwise with dropper, and stirs for 24 hours； The solution mixed is put into refrigerator overnight to freeze, is placed on -50 DEG C of vacuum drying in freeze drier, until drying obtains Mixture.Milled mixtures take the mixed-powder of 10g to be placed in Noah's ark, Noah's ark are put into tube furnace, are passed through 300ml/min Ar inert gas 20min exclude air, then with the Ar of 100~200ml/min be protection gas and with the heating of 10 DEG C/min it is fast Degree is warming up to 750 DEG C of temperature, and heat preservation 2h carries out carburizing reagent, is cooled to room temperature, obtains under Ar atmosphere protection after reaction Calcined product.Calcined product is collected, it is finely ground, it is washed to until there is no NaCl in product, is dried at 80 DEG C, obtain three-dimensional graphite Alkene network structure loads carbon SnO2Nano particle and MoS2Nanosheet composite material.

Claims (2)

1. a kind of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material, feature exist In size<The SnO of 10nm2Nano particle uniform load and simultaneously loads on three-dimensional grapheme network<5 layers of MoS2It receives Rice piece forms sandwich structure, and three-dimensional grapheme is with a thickness of 1-10nm, and three-dimensional grapheme network radius is at 1-10 μm, preparation side Method includes the following steps：
(1) with one of citric acid, glucose, sucrose or it being mixed into carbon source, stannous chloride is tin source, and ammonium molybdate is molybdenum source, Thiocarbamide is sulphur source；Wherein the tin molar ratio in the carbon and tin source in carbon source is (50~20):1, the matter of tin and NaCl in tin source Amount is than being (0.01-0.1):1, the molybdenum molar ratio in tin and molybdenum source in tin source is (0.1~1)：1, by carbon source, tin source and NaCl Be added in deionized water and dissolve, while molybdenum source and sulphur source being added in deionized water dissolve respectively, be successively added dropwise later sulphur source and Molybdenum source solution is uniformly mixed and is placed on refrigerator freezing, then is dried in vacuo, and obtains mixture；
(2) it by mixture grind into powder made from step (1), is laid in Noah's ark, is placed in tube furnace flat-temperature zone and is calcined：With N2, He or Ar one kind or mixing be used as inert gas source, first with flow be 200~400ml/min be passed through inert gas 10~ 30 minutes to exclude air；Throughput is fixed as 50~200ml/min later, is heated up with the heating rate of 1~10 DEG C/min To 650~800 DEG C, heat preservation 1-8h's tube furnace is carbonized, and is cooled to room temperature after reaction, obtains calcined product；
(3) calcined product made from collection step (2), it is finely ground, it is washed to until there is no NaCl in calcined product, is 60 in temperature It is dried at~120 DEG C, obtains three-dimensional grapheme network structure load carbon SnO2Nano particle and MoS2Nanosheet composite material.
2. three-dimensional grapheme reticular structure carrying tin oxide nano particle as described in claim 1 and molybdenum disulfide nano sheet material Material is applied to negative electrode of lithium ion battery.
CN201610705053.2A 2016-08-22 2016-08-22 The preparation and application of three-dimensional grapheme reticular structure carrying tin oxide nano particle and molybdenum disulfide nano sheet material Expired - Fee Related CN106299270B (en)

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