CN106299270A - Three-dimensional grapheme network structure carrying tin oxide nano-particle and the preparation and application of molybdenum disulfide nano sheet material - Google Patents
Three-dimensional grapheme network structure carrying tin oxide nano-particle and the preparation and application of molybdenum disulfide nano sheet material Download PDFInfo
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Abstract
The present invention relates to a kind of three-dimensional grapheme network structure carrying tin oxide nano-particle and the preparation and application of molybdenum disulfide nano sheet material.This material, by the size < SnO of 10nm2Nano-particle uniform load is on three-dimensional grapheme network, with < the MoS of 5 layers loaded simultaneously2Nanometer sheet forms sandwich structure, and three-dimensional grapheme thickness is 1 10nm, and three-dimensional grapheme network radius is in 1 10 μm.CNT prepared by the present invention, has the electric conductivity of excellence.Preparation method process of the present invention is simple, can volume production, this material has good charge-discharge performance, high rate performance and stability as lithium ion battery negative material.
Description
Technical field
The present invention relates to a kind of three-dimensional grapheme network structure load SnO2Nano-particle and MoS2Nanosheet composite material and
Preparation and application, belong to electrode material of secondary lithium ion battery field.
Background technology
Along with energy problem and the continuous aggravation of environmental problem, break away from and fossil energy is depended on unduly, progressively utilize electricity
Power drives replacement fossil energy to be driven into one main flow direction of society.Lithium ion battery as a kind of secondary cell with
The advantage such as big, working range width, discharge voltage height, non-environmental-pollution, memory-less effect by means of its energy density, at NI-G and ni-mh
The batteries such as battery are shown one's talent.Simultaneously because its have extended cycle life, security performance is widely used to mobile phone the most at present,
In the portable set such as photographing unit, notebook computer.Along with a new generation's hybrid vehicle (HEV) and pure electric automobile (EV) produce
The development of industry, the research to lithium ion battery has obtained paying close attention to more widely.
Currently used lithium ion battery extensively applies graphite as negative material, and its theoretical specific capacity is 372mAh/g,
This relatively low specific capacity is difficult to meet high power and the demand of energy density electric motor car.So, exploitation has high discharge voltage,
The Novel cathode material for lithium ion battery of high power capacity and long cycle life is particularly important.Wherein, transition metal oxide
And sulfide is by higher theoretical specific capacity, shows one's talent in the negative material of numerous and complicated.Wherein SnO2Base negative pole material
Material, theoretical specific capacity is 790mAh/g (Adv.Mater., 2009,21,2,536 2539.), simultaneously because have low cost, peace
Full property advantages of higher and receive significant attention, but its fatal weakness be exactly in charge and discharge process due to lithium ion embedding and
Abjection, can cause volume own acutely expands (about 340%), thus is prone to cause active material to occur in cyclic process
Efflorescence, and then cause its cycle performance and high rate performance poor.Additionally, MoS2As the typical transient metal sulfide of one,
By higher theoretical specific capacity (670mAh/g), excellent stratiform two-dimensional structure, the advantage such as 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,
Bigger change in volume, limits the performance of its chemical property.
In order to improve these shortcomings of transition metal oxide and sulfide negative material, solution currently mainly has
Two: one is nanorize, will the size Control of material at Nano grade so that it is do not crush, simultaneously in expansion process as far as possible
Shorten the transmission range of electronics and ion, improve its electric conductivity；Two is Composite, mainly by active material and material with carbon element
It is combined, including compound (heterojunction structure) in terms of compound (different dimensions) of configuration aspects, composition, at restriction active material
The electric conductivity that material with carbon element is excellent is utilized while volumetric expansion；Realize can significantly carrying especially while nanorize and Composite
The performance of high material.Carbon nanosheet is as the carbon nanomaterial of a kind of two-dimensional structure, owing to its electric conductivity is excellent, Stability Analysis of Structures
Property is good, and compared with other zero dimensions, one-dimensional, structure has more active reaction sites, is the optimal matrix of Composite undoubtedly.And lamella it
Between be assembled into three-dimensional grapheme structure and the most more could be formed with beneficially lithium ion and the stereochemical structure of electric transmission, thus effectively carry
The chemical property (Adv.Mater., 2012,24:4097) of high material.
Summary of the invention
It is an object of the invention to provide a kind of three-dimensional grapheme network structure load zero dimension SnO2Nano-particle and two dimension MoS2
Nanometer sheet material and preparation and application.This material is structure by carbon covered stannum rice grain uniform load to three-dimensional grapheme network
Becoming, its preparation method process is simple, can volume production, this material has good charge and discharge cycles as lithium ion battery negative material
Performance, high rate performance and stability, have a extensive future.Technical scheme is as follows:
A kind of three-dimensional grapheme network structure carrying tin oxide nano-particle and molybdenum disulfide nano sheet material, its feature exists
In, the size < SnO of 10nm2Nano-particle uniform load is on three-dimensional grapheme network, with < the MoS of 5 layers loaded simultaneously2Receive
Rice sheet forms sandwich structure, and three-dimensional grapheme thickness is 1-10nm, and three-dimensional grapheme network radius is in 1-10 μm.
The three-dimensional grapheme network structure carrying tin oxide nano-particle of said structure and molybdenum disulfide nano sheet material
Preparation method, comprises the following steps:
(1) with the one in citric acid, glucose, sucrose or be mixed into carbon source, stannous chloride is Xi Yuan, and ammonium molybdate is molybdenum
Source, thiourea is sulfur source；Wherein the carbon in carbon source is (50～20) with the stannum mol ratio in stannum source: 1, and the stannum in stannum source is with NaCl's
Mass ratio is (0.01-0.1): 1, and the molybdenum mol ratio in the stannum in stannum source and molybdenum source be (0.1～1): 1 counts, by carbon source, Xi Yuan and
NaCl adds in deionized water and dissolves, and the most respectively molybdenum source and sulfur source is added in deionized water and is dissolved, afterwards successively dropping sulfur
Source and molybdenum source solution, it is freezing that mix homogeneously is placed on refrigerator, then is vacuum dried, and obtains mixture；
(2) mixture grind into powder step (1) prepared, is laid in Noah's ark, is placed in tube furnace flat-temperature zone and forges
Burn: with N2, the one of He or Ar or mixing as inert gas source, be first 200～400ml/min to be passed through indifferent gas with flow
Body 10～30 minutes are to get rid of air；Afterwards throughput is fixed as 50～200ml/min, with the intensification speed of 1～10 DEG C/min
Degree intensification tube furnace is to 650～800 DEG C, and insulation 1-8h carries out carbonization, and reaction is cooled to room temperature after terminating, obtains calcined product；
(3) calcined product that step (2) prepares is collected, finely ground, till being washed to calcined product does not has NaCl, in temperature
It is to dry at 60～120 DEG C, obtains three-dimensional grapheme network structure load carbon SnO2Nano-particle and MoS2Nanometer sheet composite wood
Material.
This three-dimensional grapheme network structure carrying tin oxide nano-particle and molybdenum disulfide nano sheet materials application in lithium from
Sub-battery cathode.
The invention have the advantages that the present invention utilizes raw material cheap and easy to get to prepare the load of three-dimensional grapheme network structure
Carbon SnO2Nano-particle and MoS2Nanosheet composite material, with low cost, course of reaction is simple, controllability is strong.This material knot simultaneously
Structure is homogeneous, and pattern is excellent, achieve the cooperative effect of multiple material, and excellent performance has the highest for lithium ion battery negative
Specific capacity and fabulous cycle performance, under the electric current density of 2000mA/g, circulation remains to for 100 times keep more than 750mAh/g
Specific capacity, and under the high current density of 10A/g, still keep the specific capacity of 400mAh/g.
Accompanying drawing explanation
Fig. 1 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The SEM photograph of sheet composite.From this view it is apparent that three-dimensional grapheme network morphology.
Fig. 2 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The SEM photograph of sheet composite.From this view it is apparent that three-dimensional grapheme sheet thickness.
Fig. 3 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The TEM photo of sheet composite.From this view it is apparent that SnO2The reduced size of nano-particle and high dispersion.
Fig. 4 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The TEM photo of sheet composite.From the few number of plies that this view it is apparent that MoS2 nanometer sheet.
Fig. 5 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The HRTEM photo of sheet composite.From this view it is apparent that carbon-coating, SnO2 nano-particle and MoS2The sandwich knot of nanometer sheet
Structure.
Fig. 6 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The XRD figure spectrum of sheet composite.
Fig. 7 is the three-dimensional grapheme network structure load carbon SnO that the embodiment of the present invention 1 obtains2Nano-particle and MoS2Nanometer
The Laman collection of illustrative plates of sheet composite.
Fig. 8 is the three-dimensional grapheme network structure load carbon SnO using the embodiment of the present invention 1 to obtain2Nano-particle and MoS2
The charge-discharge performance figure of the lithium ion battery negative that nanosheet composite material prepares, in figure: ■ is charging curve,
● for discharge curve, ▲ for efficiency curve.
Fig. 9 is the three-dimensional grapheme network structure load carbon SnO using the embodiment of the present invention 1 to obtain2Nano-particle and MoS2
The charge-discharge magnification performance map of the lithium ion battery negative that nanosheet composite material prepares, in figure: ■ is charging curve,
● for discharge curve.
Detailed description of the invention
Below in conjunction with specific embodiment, the particular content of the present invention is described as follows:
Embodiment 1:
Weigh 2.5g citric acid, 0.394g stannous chloride and 20.0g NaCl, 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, weigh simultaneously 0.340g ammonium molybdate and
0.352g thiourea is dissolved separately in 10ml deionized water.Finally with dropper successively dropping ammonium molybdate solution and thiourea solution, and
Stirring 24h；The solution mixed is put into refrigerator overnight freeze, be placed on-50 DEG C of vacuum drying in freezer dryer, until
Drying obtains mixture.Milled mixtures, the mixed-powder taking 10g is placed in Noah's ark, is put into by Noah's ark in tube furnace, is passed through
The Ar noble gas 20min of 300ml/min gets rid of air, then with 100～200ml/min Ar for protection gas and with 10 DEG C/
The programming rate of min is warming up to temperature 750 DEG C, and insulation 2h carries out carburizing reagent, and reaction cools down after terminating under Ar atmosphere protection
To room temperature, obtain calcined product.Collect calcined product, finely ground, till being washed to product does not has NaCl, dry 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, the MoS2 nanometer sheet number of plies < 5 layers.
With obtained material, PVDF, conductive carbon black mass ratio is that 8:1:1 meter is applied to copper sheet as negative pole, with 1M's
LiPF6As electrolyte, using lithium sheet as positive pole, preparing half-cell, it circulates 100 circles still under the electric current density of 2000mA/g
Keep the specific capacity of more than 1000mAh/g, as shown in Figure 8, and there is excellent circulation performance, at the electric current of 10A/g
Still there is the specific capacity of 400mAh/g, as shown in Figure 9 under density.
Embodiment 2:
Weigh 1.25g citric acid, 0.197g stannous chloride and 15gNaCl, mixture be dissolved in the deionized water of 80ml,
With the magnetic stirring apparatus of mixing speed 300r/min, stirring and dissolving wiring solution-forming；Weigh 0.227g ammonium molybdate and 0.235g simultaneously
Thiourea is dissolved separately in 10ml deionized water；Finally with dropper successively dropping ammonium molybdate solution and thiourea solution, and stir
24h；The solution mixed is put into refrigerator overnight freeze, be placed on-50 DEG C of vacuum drying in freezer dryer, until drying
Obtain mixture.Milled mixtures, the mixed-powder taking 10g is placed in Noah's ark, is put into by Noah's ark in tube furnace, is passed through 300ml/
The Ar noble gas 20min of min gets rid of air, then with 100～200ml/min Ar for protection gas and with the liter of 10 DEG C/min
Temperature speed is warming up to temperature 750 DEG C, and insulation 2h carries out carburizing reagent, and reaction is cooled to room temperature after terminating under Ar atmosphere protection,
Obtain calcined product.Collect calcined product, finely ground, till being washed to product does not has NaCl, dry at 80 DEG C, obtain three-dimensional
Graphene network structural load carbon SnO2Nano-particle and MoS2Nanosheet composite material.
Embodiment 3:
Weigh 1g citric acid, 0.148g stannous chloride and 15g NaCl, 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, weigh 0.170g ammonium molybdate and 0.176g sulfur simultaneously
Urea is dissolved separately in 10ml deionized water.Finally with dropper successively dropping ammonium molybdate solution and thiourea solution, and stir 24h；
The solution mixed being put into refrigerator overnight freeze, be placed on-50 DEG C of vacuum drying in freezer dryer, obtaining until drying
Mixture.Milled mixtures, the mixed-powder taking 10g is placed in Noah's ark, is put into by Noah's ark in tube furnace, is passed through 300ml/min
Ar noble gas 20min get rid of air, then with 100～200ml/min Ar for protection gas and with the intensification of 10 DEG C/min speed
Degree is warming up to temperature 750 DEG C, and insulation 2h carries out carburizing reagent, and reaction is cooled to room temperature under Ar atmosphere protection after terminating, obtains
Calcined product.Collect calcined product, finely ground, till being washed to product does not has NaCl, dry at 80 DEG C, obtain three-dimensional graphite
Alkene network structure load carbon SnO2Nano-particle and MoS2Nanosheet composite material.
Claims (3)
1. three-dimensional grapheme network structure carrying tin oxide nano-particle and a molybdenum disulfide nano sheet material, its feature exists
In, the size < SnO of 10nm2Nano-particle uniform load is on three-dimensional grapheme network, with < the MoS of 5 layers loaded simultaneously2Receive
Rice sheet forms sandwich structure, and three-dimensional grapheme thickness is 1-10nm, and three-dimensional grapheme network radius is in 1-10 μm.
2. the three-dimensional grapheme network structure carrying tin oxide nano-particle of said structure and the system of molybdenum disulfide nano sheet material
Preparation Method, comprises the following steps:
(1) with the one in citric acid, glucose, sucrose or be mixed into carbon source, stannous chloride is Xi Yuan, and ammonium molybdate is molybdenum source,
Thiourea is sulfur source；Wherein the carbon in carbon source is (50～20) with the stannum mol ratio in stannum source: 1, the stannum in stannum source and the matter of NaCl
Amount is than for (0.01-0.1): 1, and the stannum in stannum source be (0.1～1) with the molybdenum mol ratio in molybdenum source: 1 counts, by carbon source, Xi Yuan and
NaCl adds in deionized water and dissolves, and the most respectively molybdenum source and sulfur source is added in deionized water and is dissolved, afterwards successively dropping sulfur
Source and molybdenum source solution, it is freezing that mix homogeneously is placed on refrigerator, then is vacuum dried, and obtains mixture；
(2) mixture grind into powder step (1) prepared, is laid in Noah's ark, is placed in tube furnace flat-temperature zone and calcines: with
N2, the one of He or Ar or mixing as inert gas source, first with flow be 200～400ml/min be passed through noble gas 10～
30 minutes to get rid of air；Afterwards throughput is fixed as 50～200ml/min, heats up with the programming rate of 1～10 DEG C/min
Tube furnace is to 650～800 DEG C, and insulation 1-8h carries out carbonization, and reaction is cooled to room temperature after terminating, obtains calcined product；
(3) calcined product that step (2) prepares is collected, finely ground, till being washed to calcined product does not has NaCl, it is 60 in temperature
～dry at 120 DEG C, obtain three-dimensional grapheme network structure load carbon SnO2Nano-particle and MoS2Nanosheet composite material.
3. this three-dimensional grapheme network structure carrying tin oxide nano-particle and molybdenum disulfide nano sheet materials application are in lithium ion
Battery cathode.
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| CN107774282A (en) * | 2017-09-05 | 2018-03-09 | 天津大学 | Three-dimensional grapheme network structure loads the preparation and application of molybdenum disulfide nano material |
| CN108091841A (en) * | 2017-12-05 | 2018-05-29 | 陕西科技大学 | A kind of method for preparing porous carbon load tin dioxide composite material |
| CN108448091A (en) * | 2018-03-20 | 2018-08-24 | 济南大学 | A kind of MoO2/SnS2Nanocomposite and preparation method thereof |
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| CN112038626A (en) * | 2020-08-25 | 2020-12-04 | 哈尔滨工业大学（深圳） | Tin-carbon composite material for lithium ion battery cathode and preparation method thereof |
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