CN108346783A - A kind of layered structure MoSxSe2-x/ graphene negative material and preparation method thereof - Google Patents
A kind of layered structure MoSxSe2-x/ graphene negative material and preparation method thereof Download PDFInfo
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- CN108346783A CN108346783A CN201810027259.3A CN201810027259A CN108346783A CN 108346783 A CN108346783 A CN 108346783A CN 201810027259 A CN201810027259 A CN 201810027259A CN 108346783 A CN108346783 A CN 108346783A
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- H01M4/00—Electrodes
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- 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
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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
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a kind of layered structure MoSxSe2‑x/ graphene（0.5≤x≤1.5）Negative material and preparation method thereof belongs to electrochemistry and new energy materials field.The electrode material is multilayer lamination structure, the space of bigger is provided for the insertion of lithium, sodium ion, the present invention will obtain MoS after graphene oxide solution, ammonium molybdate and thiocarbamide hydro-thermal2/ grapheme material, is then uniformly mixed with elemental selenium, is calcined in nitrogen.Selenium atom replaces part sulphur atom, forms layered structure MoSxSe2‑x/ graphene（0.5≤x≤1.5）Composite material.The present invention passes through simple hydro-thermal method and calcination method, prepares layered structure MoSxSe2‑x/ graphene（0.5≤x≤1.5）Composite material, can not only improve the specific capacity and lithium ion diffusion rate of material, and can overcome reunion and the overlap problem of nano particle, have great application prospect as lithium, anode material of lithium-ion battery.
Description
Technical field
The invention discloses a kind of layering MoSxSe2-x/ graphene（0.5≤x≤1.5）Negative material and preparation method thereof,
Belong to electrochemistry and new energy materials field.
Background technology
Come in the past few decades, the rechargeable battery including lithium ion battery and sodium-ion battery is close due to its high-energy
Degree, long-life and memoryless function and be widely studied the most promising portable energy for electronic equipment and electric vehicle
Source.However, for the energy density of rechargeable battery, rate capability, the further improvement in terms of durability and safety is still
It is of great significance.Therefore, more and more researchers are dedicated to exploring new electrode material, to realize high power capacity, quickly
Charging and durable cycle.
Two-dimensional layered structure molybdenum sulfide is as one of transient metal sulfide, single layer MoS2Upper and lower two layers are sulphur atom, in
Between one layer be molybdenum atom, this layer structure is conducive to the insertion of lithium, sodium ion, and the sky of bigger can be provided for ion insertion
Between.But since layer and layer have Van der Waals force, the constantly embedded abjection of lithium/sodium ion, can cause to vulcanize in charge and discharge process
Agglomeration occurs for molybdenum, and electrolyte effectively contacts reduction with active material, causes stability poor, capacity attenuation is fast.MoS2
As negative material, there is also the poor problems of electric conductivity, thus by with the preferable graphene of electric conductivity is compound and elemental selenium
Insertion form multilayered structure negative material, not only alleviate the agglomeration occurred in charge and discharge process, but also increase material
The stability and conductivity of material.It, should 201410843894.0 patent discloses a kind of Sn-Ni-graphene laminar composites
Composite material avoids metallic tin, and there are huge agglomerations after high-temperature heat treatment, it is suppressed that the volume expansion of metallic tin is received
Contracting shows good cycle performance when the composite material is used as negative electrode of lithium ion battery.201010561749.5 patent
A kind of silicon/graphene composite material is disclosed, there is stratiform sandwich structure, silicon nanoparticle is scattered on graphene is per lamella
Son is separated by silicon nano among graphene sheet layer, and overlapping edges are together, constitute layered conductive network structure.System
Standby silicon/graphene composite material has good electric conductivity, power-performance, electro-chemical activity and cyclical stability, especially suitable
For making negative electrode of lithium ion battery.201310444961.7 patent discloses a kind of SiO of layer structurexIt is difunctional compound
Negative material, by self-assembling technique by SiOxIt is supported on the carrier with high conductivity and high tenacity and forms difunctional structure
（SiOxHigh power capacity is provided, carrier provides electric conductivity and is SiOxVolume change provide buffering）Composite material, using carrier come
Improve SiOxElectric conductivity and prevent SiOxReunion in cyclic process, while reducing SiOxBulk effect is to electrode structure
It destroys, to significantly improve SiOxCycle performance.
It to sum up analyzes, novel MoSxSe2-x/ graphene composite negative pole not only has the advantages that layered structure, it may have
Preferable cycle performance and higher specific capacity have larger application prospect as lithium, anode material of lithium-ion battery.
Invention content
The purpose of the present invention is to provide a kind of layering MoSxSe2-x/ graphene composite negative pole, the 0.5≤x
≤ 1.5, the negative material shows multilayered structure, MoSxSe2-xNano particle is embedded between graphene layer（It is further excellent
The structure for being selected as the negative material is MoS1.5Se0.5/ graphene negative material.）.The preparation of the material is using utilization
Graphene oxide solution and ammonium molybdate, thiocarbamide hydro-thermal in certain proportion prepared by Hummers methods, it is dry.Then, it will be formed
Material be uniformly mixed with elemental selenium, 700 in nitrogen atmosphere stove oC is sintered 2 h.Ultimately form layering MoSxSe2-x/ graphene
Composite negative pole material, layered structure are conducive to the insertion of ion, improve the specific capacity of material.
The object of the present invention is achieved like this：A kind of layering MoSxSe2-x/ graphene composite negative pole preparation method,
Its processing step：
Ammonium molybdate and thiocarbamide are added in the water heating kettle for being contained with graphene oxide solution, hydro-thermal reaction 20- at 120-160 DEG C
30h obtains MoS2/ graphene composite material, by the MoS after drying2/ graphene composite material is uniformly mixed with elemental selenium, closed
1-3h is calcined at 600-800 DEG C in nitrogen atmosphere stove afterwards obtains the MoS with layered structurexSe2-x/ graphene composite negative
Material.
The mixing water thermal mass ratio of the graphene oxide, ammonium molybdate and thiocarbamide is 1：6-10：12-18.
The mixing water thermal mass ratio of the graphene oxide, ammonium molybdate and thiocarbamide is 1：8.4：15.5.
The hydrothermal temperature is 140oC, the hydro-thermal reaction time are for 24 hours.
The MoS2/ graphene composite material and the mass ratio of elemental selenium are 1：0.5-3.
Layering MoS provided by the inventionxSe2-x/ graphene composite negative pole has following advantageous effect：
（1）Electrode material prepared by the method has layered structure（Several layers of-tens layers）, as cell negative electrode material, Ke Yirong
It receives more lithiums, sodium ion, improves the specific capacity of material.
（2）Layering MoS prepared by the methodxSe2-xIt is high to be not only provided simultaneously with molybdenum sulfide capacity for/graphene composite negative pole
The good advantage with graphene conductive, and the agglomeration that molybdenum sulfide electrode material occurs during the reaction is alleviated,
The incorporation of elemental selenium simultaneously replaces part sulphur, causes the fault of construction of the inside of material, and more activity are provided for reaction
Site further improves the specific capacity of composite material.
Description of the drawings
Fig. 1 is layering MoS prepared by the embodiment of the present invention 11.5Se0.5The X-ray diffraction of/graphene composite negative pole
(XRD) collection of illustrative plates.
Fig. 2 is layering MoS prepared by the embodiment of the present invention 11.5Se0.5/ graphene composite negative pole is in different times magnifications
Stereoscan photograph (SEM) under several.
A figures are layering MoS prepared by the embodiment of the present invention 1 in Fig. 31.5Se0.5/ graphene composite negative pole as lithium from
Sub- cell negative electrode material 3 times charging and discharging curve；B figures are that embodiment 1 prepares multilayer MoS1.5Se0.5/ graphene composite negative material
Material is used as anode material of lithium-ion battery 3 times charging and discharging curve.
Fig. 4 is layering MoS prepared by the embodiment of the present invention 11.5Se0.5/ graphene composite negative pole is under different multiplying
Cycle performance.
Fig. 5 is layering MoS prepared by the embodiment of the present invention 11.5Se0.5The cyclic voltammetric of/graphene composite negative pole is bent
Line.
Specific implementation mode
With reference to specific example, the present invention is further described.
Embodiment 1：It is layered MoS1.5Se0.5/ graphene composite negative pole I
Take graphene oxide solution (the 2.1 mg mL prepared using Hummers methods-1) 35 mL, 0.618 g ammonium molybdates and
1.142 g thiocarbamides are put into 140 in water heating kettleo24 h of C hydro-thermals.In water-heat process, sodium molybdate and thiocarbamide form MoS2, graphene shape
At multilayered structure, molybdenum sulfide is carried on graphene surface or is inserted into interlayer, improves the stability of material, then, will obtain
Material filter, cleaned with deionized water, ethyl alcohol, be placed in 80oIt is dry in C baking ovens, obtain MoS2/ graphene composite material.It will
This composite material makes both materials be uniformly mixed with elemental selenium grinding（Mass ratio 1:2）, 700 in nitrogen atmosphere stoveoC is forged
2 h are burnt, multilayer MoS is obtained1.5Se0.5/ graphene composite negative pole while calcining, has not only introduced selenium atom, has caused material
Fault of construction inside material, forms novel MoS1.5Se0.5/ graphene combination electrode material, while also improving the crystallization of material
Property and carbonizing degree.Fig. 1 is multilayer MoS1.5Se0.5The XRD spectrum of/graphene composite negative pole.As can be seen from the figure single
The incorporation of matter selenium improves the crystallinity of material, while after selenium adulterates, and part selenium forms MoS instead of sulphur1.5Se0.5Material
Material.Fig. 2 is SEM photograph of the material under different amplification, it can be seen that MoS1.5Se0.5/ graphene composite negative pole
Pattern with stacked in layers, for the number of plies between 10-15, this layered structure has lower impedance, largely carries
Its high electrochemical reaction kinetic characteristics.By the material and binder PVDF and conductive agent acetylene black with 8:1:1 ratio system
At electrode slice, when as lithium ion battery negative material, lithium piece is to electrode, and battery diaphragm uses Celgard 2400（It is beautiful
State）, electrolyte is general 1 M LiPF of lithium-ion battery electrolytes6/DMC: EC=1:1 (volume ratio) prepares 2025 type knobs
Battery is detained, with 0.1 A g-1Current density charge and discharge.3 times charging and discharging curve such as Fig. 3 of the lithium ion battery negative material
(a) shown in, it can be seen that the discharge capacity for the first time of the material is 1056 mAh g-1, reversible charging capacity is 744 mAh for the first time
g-1.When as anode material of lithium-ion battery, sodium piece is to electrode, and battery diaphragm uses Whatman GF/D, and electrolyte is logical
Sodium-ion battery electrolyte 1M NaPF6/(EC+DMC+EMC)=1:1:1 (volume ratio), entire button cell are assembled in
Glove box full of nitrogen（MIKROUNA,<1 ppm H2O,<1 ppm O2）Middle progress.The electrode is as sodium-ion battery cathode
Shown in 3 times charging and discharging curve such as Fig. 3 (b) of material, it can be seen that the discharge capacity for the first time of the material is 810 mAh g-1,
Reversible charging capacity is 444 mAh g for the first time-1.The electrode is as li-ion electrode cathode stable circulation performance such as Fig. 4 (a) institutes
Show, with 0.1 A g-1Specific discharge capacity after current density recycles 30 times is still up to 843 mAh g-1.The electrode as sodium from
Shown in sub-electrode cathode stable circulation performance such as Fig. 4 (b), with 0.3 A g-1Current density recycle 200 times after electric discharge specific volume
Amount is still up to 424 mAh g-1, 1 A g-1Specific discharge capacity after being recycled 200 times under current density is still up to 304 mAh g-1, thus, multilayer MoS1.5Se0.5/ graphene composite material all has preferable as lithium, sodium-ion battery composite material
Cycle performance and higher specific capacity.Fig. 5 is CV curve of the electrode as li-ion electrode negative material, is recycled in first lap
In the process, the discharge platform of 1.05 V is mainly due to lithium ion insertion MoS1.5Se0.5In lattice, 0.67 V corresponds to Li2Se、
Li2The formation of S and metal Mo, while the reduction peak at 0.37 V is since electrode surface forms SEI films, in charging process
The platform of 2.2 V of middle appearance, corresponds to Li2Se and Li2S is oxidized to elemental selenium and elemental sulfur.It is filled in the second circle and third circle
During discharge cycles, there is new 1.92 V of reduction peak and correspond to Se and S to Li2Se and Li2The conversion of S.These results with fill
Discharge curve is consistent, and fully illustrates the mechanism of the electrode during the reaction.
Embodiment 2 is layered MoSSe/ graphene composite negative poles II
Take the graphene oxide solution prepared using Hummers methods（2.1 mg mL-1）35 mL, 0.618 g ammonium molybdates and
1.142 g thiocarbamides are put into 140 in water heating kettleo24 h of C hydro-thermals.Then, obtained material is filtered, it is clear with deionized water, ethyl alcohol
It washes, is placed in 80oIt is dry in C baking ovens, obtain MoS2/ graphene composite material.By this composite material and elemental selenium grinding make this two
Kind material is uniformly mixed（Mass ratio 1:1）, 700 in nitrogen atmosphere stoveoC calcines 2 h, and it is multiple to obtain multilayer MoSSe/ graphenes
Negative material is closed, the electrode material test condition is as described in example 1 above, as lithium ion battery negative material with 0.1 A g-1
Current density carries out charge and discharge, and reversible capacity is 1009 mAh g for the first time-1, the reversible capacity after recycling 30 times is 620 mAh
g-1.As anode material of lithium-ion battery with 0.3 A g-1Current density carries out charge and discharge, and reversible capacity is 405 mAh for the first time
g-1, the reversible capacity after recycling 200 times is 212 mAh g-1。
Embodiment 3 is layered MoS4/3Se2/3/ graphene composite negative pole III
Take the graphene oxide solution prepared using Hummers methods（2.1 mg mL-1）35 mL, 0.618 g ammonium molybdates and
1.142 g thiocarbamides are put into 140 in water heating kettleo24 h of C hydro-thermals.Then, obtained material is filtered, it is clear with deionized water, ethyl alcohol
It washes, is placed in 80oIt is dry in C baking ovens, obtain MoS2/ graphene composite material.By this composite material and elemental selenium grinding make this two
Kind material is uniformly mixed（Mass ratio 2:1）, 700 in nitrogen atmosphere stoveoC calcines 2 h, obtains multilayer MoS4/3Se2/3/ graphite
Alkene composite negative pole material, the electrode material test condition is as described in example 1 above, as lithium ion battery negative material with 0.1
A g-1Current density carries out charge and discharge, and reversible capacity is 980 mAh g for the first time-1, the reversible capacity after recycling 30 times is 523
mAh g-1.As anode material of lithium-ion battery with 0.3 A g-1Current density carries out charge and discharge, and reversible capacity is 390 for the first time
mAh g-1, the reversible capacity after recycling 200 times is 180 mAh g-1。
Claims (8)
1. a kind of layered structure MoSxSe2-x/ graphene negative material, which is characterized in that 0.5≤x≤1.5, it is described
Negative material shows multilayered structure, MoSxSe2-xNano particle is embedded between graphene layer.
2. layered structure MoS described in claim 1xSe2-x/ graphene negative material, which is characterized in that the negative material
Structure be MoS1.5Se0.5/ graphene negative material.
3. layered structure MoS described in claim 1xSe2-xThe preparation method of/graphene negative material, which is characterized in that by molybdenum
Sour ammonium and thiocarbamide are added in the water heating kettle for being contained with graphene oxide solution, and hydro-thermal reaction 20-30h is obtained at 120-160 DEG C
MoS2/ graphene composite material, by the MoS after drying2/ graphene composite material is uniformly mixed with elemental selenium, it is closed after in nitrogen
Calcining obtains the MoS with layered structure in atmosphere furnacexSe2-x/ graphene composite negative pole.
4. the layered structure MoS described in claim 3xSe2-xThe preparation method of/graphene negative material, which is characterized in that oxidation
The mixing water thermal mass ratio of graphene, ammonium molybdate and thiocarbamide is 1：6-10：12-18.
5. the layered structure MoS described in claim 3xSe2-xThe preparation method of/graphene negative material, which is characterized in that oxidation
The mixing water thermal mass ratio of graphene, ammonium molybdate and thiocarbamide is 1：8.4：15.5.
6. the layered structure MoS described in claim 3xSe2-xThe preparation method of/graphene negative material, which is characterized in that hydro-thermal
Reaction temperature is 140oC, the hydro-thermal reaction time are for 24 hours.
7. the layered structure MoS described in claim 3xSe2-xThe preparation method of/graphene negative material, which is characterized in that prepare
Obtained MoS2/ graphene composite material is uniformly mixed with elemental selenium 700 in nitrogen atmosphere stoveo2 h are calcined under C.
8. the layered structure MoS described in claim 3xSe2-xThe preparation method of/graphene negative material, which is characterized in that
MoS2/ graphene composite material and the mass ratio of elemental selenium are 1：0.5-3.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109546098A (en) * | 2018-10-11 | 2019-03-29 | 天津大学 | The preparation method of redox graphene load ReS2 for lithium sulfur battery anode material |
| CN110371934A (en) * | 2019-06-06 | 2019-10-25 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN111916734A (en) * | 2020-07-09 | 2020-11-10 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN112803017A (en) * | 2021-03-01 | 2021-05-14 | 吉林大学 | Hollow spherical bimetal chalcogenide, preparation method thereof and sodium battery cathode |
| CN113764631A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | FeS for sodium ion battery0.5Se0.5/CF composite negative electrode material and preparation method thereof |
| CN114242982A (en) * | 2021-12-20 | 2022-03-25 | 北京理工大学重庆创新中心 | Graphene-coated two-dimensional metal compound electrode material and preparation method and application thereof |
| CN114335408A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Composite electrode and preparation method and application thereof |
| CN114335468A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Positive/negative electrode material of lithium-sulfur battery and preparation method thereof |
| WO2023045125A1 (en) * | 2021-09-24 | 2023-03-30 | 中国科学院深圳先进技术研究院 | Negative electrode material and preparation method therefor, and sodium-ion battery |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109546098A (en) * | 2018-10-11 | 2019-03-29 | 天津大学 | The preparation method of redox graphene load ReS2 for lithium sulfur battery anode material |
| CN111785928B (en) * | 2019-04-04 | 2021-11-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN110371934A (en) * | 2019-06-06 | 2019-10-25 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | A kind of preparation method of carbon-based sulphur selenizing molybdenum composite material |
| CN113764631A (en) * | 2020-06-01 | 2021-12-07 | 南京航空航天大学 | FeS for sodium ion battery0.5Se0.5/CF composite negative electrode material and preparation method thereof |
| CN111916734A (en) * | 2020-07-09 | 2020-11-10 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN111916734B (en) * | 2020-07-09 | 2022-04-12 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN112803017A (en) * | 2021-03-01 | 2021-05-14 | 吉林大学 | Hollow spherical bimetal chalcogenide, preparation method thereof and sodium battery cathode |
| WO2023045125A1 (en) * | 2021-09-24 | 2023-03-30 | 中国科学院深圳先进技术研究院 | Negative electrode material and preparation method therefor, and sodium-ion battery |
| CN114242982A (en) * | 2021-12-20 | 2022-03-25 | 北京理工大学重庆创新中心 | Graphene-coated two-dimensional metal compound electrode material and preparation method and application thereof |
| CN114242982B (en) * | 2021-12-20 | 2023-11-07 | 北京理工大学重庆创新中心 | Graphene-coated two-dimensional metal compound electrode material and preparation method and application thereof |
| CN114335408A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Composite electrode and preparation method and application thereof |
| CN114335468A (en) * | 2021-12-28 | 2022-04-12 | 上海交通大学 | Positive/negative electrode material of lithium-sulfur battery and preparation method thereof |
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