CN110247038A - A kind of Bi2S3-MoS2/ graphene composite nano material and preparation method thereof - Google Patents
A kind of Bi2S3-MoS2/ graphene composite nano material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of two-component metal sulfide/graphene composite nano materials and preparation method thereof, which is by Bi2S3Nanoparticle and MoS2Nanometer sheet is compound, and is equably supported on graphene and is constituted, and preparation method is under graphene oxide existence condition, by Bi (NO3)3、Na2MoO4With the hydro-thermal reaction of the mixed solution of L-cysteine under hydrothermal conditions, Bi is prepared2S3‑MoS2/ graphene composite nano material, wherein the molar ratio of Bi and Mo is 1: 9~1: 4.Bi of the invention2S3‑MoS2There is/graphene composite nano material excellent electrochemistry to store lithium performance, have a wide range of applications in high performance lithium ion battery.Bi proposed by the present invention2S3‑MoS2The hydrothermal preparing process of/graphene composite nano material has the characteristics that simple, convenient and is easily enlarged application.
Description
Technical field
The present invention relates to composite material and preparation method more particularly to Bi2S3-MoS2/ graphene composite nano material and
Preparation method belongs to inorganic nano composite material technical field.
Background technique
As lithium ion battery negative material, MoS2Nano material electrochemistry storage lithium capacity with higher (hold by its theory
Amount is 670mAh/g), it is with a wide range of applications in high performance lithium ion battery.But due to its lower conductance
The biggish variation of volume in rate and charge and discharge process causes it to store the rapid decay of lithium capacity in charge and discharge process.Bismuth sulfide
Nano material is also a kind of lithium ion battery negative material with compared with high electrochemical storage lithium capacity, but single bismuth sulfide is received
Rice material similarly haves the shortcomings that capacity attenuation is very fast in charge and discharge process.Recent research indicate that by two different metals
Nano material (such as SnS that sulfide is compounded to form2-MoS2And Ni3S2-MoS2Composite material etc.) it is used as negative electrode of lithium ion battery material
The electrochemical lithium storage performance of material is above single nano metal sulfide material.The reason of its chemical property enhances is two kinds
There is the composite nano materials that different metal sulfides is formed heterogeneous composite construction and more electrochemistry lithiumations-to go lithiumation
Electricity is to reaction.Although the electrochemical lithium storage performance for the composite nano materials that two different metal sulfides are formed makes moderate progress,
Its lower conductivity still affects further enhancing for its electrochemical lithium storage performance.
Graphene has high conductivity and charged mobility, great specific surface area, good flexible and chemical stabilization
Property.By the way that sulfide nano-material is compound with graphene, not only there is prepared composite material high electrochemistry storage lithium to hold
Amount, and with stable charge-discharge performance and significantly increase high power charging-discharging characteristic.Such as: MoS2Graphene composite wood
Material, bismuth sulfide-graphene composite material etc. are shown than individual MoS2Or there is bismuth sulfide higher electrochemistry storage lithium to hold
Amount and superior charge and discharge cycles stability.But what the electrochemistry of these composite materials storage lithium performance also further increased
Space.
The present invention provides a kind of Bi2S3-MoS2/ graphene composite nano material and preparation method thereof.With MoS2Graphite
Alkene and Bi2S3Graphene composite material is compared, MoS of the invention2-Bi2S3/ graphene composite nano material has higher electricity
Chemistry storage lithium reversible specific capacity, more stable charge-discharge performance and the high power charging-discharging characteristic significantly increased.But it arrives
So far, this Bi2S3-MoS2/ graphene composite nano material and preparation method thereof yet there are no open report.
Summary of the invention
The purpose of the present invention is to provide a kind of Bi2S3-MoS2/ graphene composite nano material and preparation method thereof.
Bi of the invention2S3-MoS2/ graphene composite nano material is by Bi2S3Nanoparticle and MoS2Nanometer sheet is compound,
And equably formed on graphene, wherein the molar ratio of Bi and Mo is 1: 9~1: 4, and preparation methods steps are as follows:
(1) by the Bi (NO of metering3)3·5H2O、Na2MoO4·2H2O and L-cysteine are add to deionized water, and
It is sufficiently stirred, obtains uniform mixed solution, Bi (NO in hydro-thermal reaction solution3)3With Na2MoO4The ratio between the amount of substance be 1: 9
~1: 4, the amount of the substance of L-cysteine is Bi (NO3)3With Na2MoO45 times of the sum of the amount of substance;
(2) in deionized water by graphene oxide ultrasonic disperse, uniform suspension is obtained, under constant stirring by oxygen
Graphite alkene hanging drop is added in above-mentioned mixed solution, and continues to stir 2h, is calculated with the amount of the substance of carbon, graphene oxide
Substance amount be equal to Bi (NO3)3With Na2MoO42 times of the sum of the amount of substance;
(3) reaction mixture that step (2) obtains is transferred in the hydrothermal reaction kettle with polytetrafluoroethylliner liner, it is close
It is honored as a queen and is reacted for 24 hours at 200 DEG C, then cooled to room temperature, the precipitated product that hydro-thermal reaction is obtained is centrifugated, and is used in combination
Deionized water and dehydrated alcohol sufficiently wash, and obtain Bi after being finally dried in vacuo 12h at 80 DEG C2S3-MoS2/ graphene is compound
Nano material, the molar ratio of Bi and Mo therein are 1: 9~1: 4.
Compared with the prior art, Bi of the invention2S3-MoS2/ graphene composite nano material and preparation method thereof have with
Significant advantage down: although with single MoS2Or Bi2S3Nano material compares, MoS2/ graphene composite material and Bi2S3/ stone
There is black alkene composite material higher electrochemistry to store lithium capacity, and electrochemistry storage lithium capacity can achieve 900-1000mAh/g, and
With more stable charge-discharge performance and good high power charging-discharging characteristic, but its electrochemistry storage lithium performance also have into
The space that one step is promoted.It is of the invention the result shows that, Bi2S3-MoS2/ graphene composite nano material ratio MoS2/ graphene is compound
Material and Bi2S3/ graphene composite material has higher electrochemistry storage lithium capacity and the high power charging-discharging further enhanced special
Property.The main reason for its chemical property further enhances is: the MoS of hydro-thermal preparation2Microscopic appearance is mainly exemplary two dimensional layer
Shape nanometer sheet, and the Bi of hydro-thermal preparation2S3Mainly show the biggish similar shuttle of particle or olivary microscopic appearance, when
Bi (NO in hydro-thermal reaction solution3)3And Na2MoO4When existing simultaneously, in hydrothermal reaction process, MoS2And Bi2S3Nucleation and life
Length is almost either simultaneously or alternately carrying out, and due to both different sulfide nucleation and grows there are mutual interference and influence, leads
The variation for causing tiny area reaction condition in hydro-thermal reaction system, makes MoS generated2With the less number of plies and more side
Edge, while the Bi generated2S3Partial size also become smaller, and and MoS2It is combined with each other, Bi2S3-MoS2Composite construction and hydro-thermal
Redox graphene has further been compounded to form Bi2S3-MoS2/ graphene composite nano material, due to its Bi2S3, MoS2, stone
The uniform heterojunction structure and Bi formed between black alkene three2S3-MoS2Bimetallic sulfide has more electrochemical lithiums
Change/go lithiated electrode reaction right, the Bi of present aspect of electricity2S3-MoS2/ graphene composite nano material and MoS2/ graphene and
Bi2S3/ graphene composite material is compared, and is filled with higher electrochemistry storage lithium reversible specific capacity and the high magnification further enhanced
Flash-over characteristic.In addition, Bi of the present invention2S3-MoS2One step hydrothermal preparing process of/graphene graphene composite nano material has
Simple process, convenience and the characteristics of be easily enlarged application.
Detailed description of the invention
Fig. 1: the XRD diagram of the different composite material of hydro-thermal method preparation of the present invention: (a) MoS2/ graphene, (b) MoS2-
Bi2S3/ graphene -1 (Bi: Mo=1: 9), (c) MoS2-Bi2S3/ graphene -2 (Bi: Mo=1: 4), (d) MoS2-Bi2S3/ graphite
Alkene -3 (Bi: Mo=1: 1) and (e) Bi2S3/ graphene complex
Fig. 2: the SEM pattern of the composite material of hydro-thermal method preparation of the present invention, (a) MoS2/ graphene, (b) MoS2-Bi2S3/
Graphene -1 (Bi: Mo=1: 9), (c) MoS2-Bi2S3/ graphene -2 (Bi: Mo=1: 4), (d) MoS2-Bi2S3/ graphene -3
(Bi: Mo=1: 1) and (e) Bi2S3/ graphene composite material.
Fig. 3: the TEM/HRTEM photo of the composite material of hydro-thermal hair preparation of the present invention, (a, b) MoS2/ graphene, (c, d)
MoS2-Bi2S3/ graphene -1 (Bi: Mo=1: 9), (e, f) MoS2-Bi2S3/ graphene -2 (Bi: Mo=1: 4), (g, h) MoS2-
Bi2S3/ graphene -3 (Bi: Mo=1: 1), (i, j) Bi2S3/ graphene composite material
Fig. 4: MoS2/ graphene, MoS2-Bi2S3/ graphene -1 (Bi: Mo=1: 9), MoS2-Bi2S3/ graphene -2 (Bi:
Mo=1: 4), and MoS2-Bi2S3/ graphene -3 (Bi: Mo=1: 1) and Bi2S3/ graphene composite material electrode is in 100mA/g electric current
Charge-discharge performance under density
Fig. 5: MoS2/ graphene, MoS2-Bi2S3/ graphene -1 (Bi: Mo=1: 9), MoS2-Bi2S3/ graphene -2 (Bi:
Mo=1: 4), and MoS2-Bi2S3/ graphene -3 (Bi: Mo=1: 1) and Bi2S3/ graphene composite material electrode is close in different electric currents
Charge/discharge rate property under degree
Specific embodiment
The present invention is further illustrated with attached drawing with reference to embodiments.
Bi2S3-MoS2The preparation of/graphene composite nano material: by the Bi of x mmol (x=0.15,0.3,0.75)
(NO3)3·5H2The Na of O and (1.5-x) mmol2MoO4·2H2O and 7.5mmol L-cysteine is added to 50mL deionization
In water, and it is sufficiently stirred and forms uniform mixed solution;By the graphene oxide ultrasonic disperse of freshly prepd 3mmol 20mL's
In deionized water, uniform suspension is obtained, under constant stirring, the hanging drop of graphene oxide is added to the mixing of front
In solution, it is stirred for 2h at room temperature;The mixed reactant finally obtained is transferred to the water that 100mL has polytetrafluoroethylliner liner
In thermal response kettle, sealing is reacted for 24 hours in 200 DEG C of insulating box, after room temperature, by precipitation and centrifugal separation, and
It is sufficiently washed with deionized water and dehydrated alcohol, will obtain finally obtaining after hydro-thermal black product is dried in vacuo 12h at 80 DEG C
Bi2S3-MoS2/ graphene composite nano material, preparation-obtained 3 composite nano materials are denoted as MoS respectively2-Bi2S3/ stone
Black alkene -1, MoS2-Bi2S3/ graphene -2 and MoS2-Bi2S3/ graphene -3, the molar ratio of Bi and Mo therein are respectively 1: 9,1
: 4 and 1: 1.
Comparative example: MoS is prepared for similar hydrothermal method2/ graphene and Bi2S3/ graphene composite material.
MoS2Prepared by the hydro-thermal of/graphene composite material: by 1.5mmol Na2MoO4·2H2Half Guang of O and 7.5mmol L-
Propylhomoserin is added in 50mL deionized water, and is sufficiently stirred and to be formed uniform mixed solution;By the oxidation stone of freshly prepd 3mmol
Black alkene ultrasonic disperse obtains uniform suspension in 20mL deionized water, under constant stirring, by the suspension of graphene oxide
Drop is added in the mixed solution of front, is stirred for 2h at room temperature;The mixed reactant finally obtained is transferred to 100mL to have
In the hydrothermal reaction kettle of polytetrafluoroethylliner liner, sealing is reacted in 200 DEG C of insulating box for 24 hours, after naturally cool to room temperature
Afterwards, it by precipitation and centrifugal separation, and is sufficiently washed with deionized water and dehydrated alcohol, it is true at 80 DEG C that hydro-thermal black product will be obtained
After the dry 12h of sky, MoS is finally obtained2/ graphene composite material.
Bi2S3Prepared by the hydro-thermal of/graphene composite material: by 1.5mmol Bi (NO3)3·5H2Half Guang of O and 7.5mmol L-
Propylhomoserin is added in 50mL deionized water, and is sufficiently stirred and to be formed uniform mixed solution;By the graphene oxide ultrasound of 3mmol
It is dispersed in 20mL deionized water, obtains uniform suspension, under constant stirring, the hanging drop of graphene oxide is added to
In the mixed solution of front, it is stirred for 2h at room temperature;The mixed reactant finally obtained is transferred to 100mL with polytetrafluoroethyl-ne
In the hydrothermal reaction kettle of alkene liner, sealing is reacted for 24 hours in 200 DEG C of insulating box, after room temperature, will be precipitated
Centrifuge separation, and sufficiently washed with deionized water and dehydrated alcohol, hydro-thermal black product will be obtained and be dried in vacuo 12h at 80 DEG C
Afterwards, Bi is finally obtained2S3/ graphene composite material.
With X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope/high-resolution-ration transmission electric-lens (TEM/HRTEM) and
XPS characterizes the sample of above-mentioned preparation.
The test of electrochemical lithium storage performance: by the above-mentioned sample (MoS being prepared2/ graphene, Bi2S3-MoS2/ graphite
Alkene -1 (Bi: Mo=1: 9), Bi2S3-MoS2/ graphene -2 (Bi: Mo=1: 4), Bi2S3-MoS2/ graphene -3 (Bi: Mo=1:
And Bi 1)2S3/ graphene) active material as electrochemical lithium storage, and active material, conductive agent acetylene black and binder are gathered
Vinylidene according to mass ratio 80: 10: 10 fully dispersed (or dissolution) in n-methyl-2-pyrrolidone, after stirring and grinding
Homogeneous paste object is obtained, which is coated on copper foil, is pressed into work electricity after dry 12h in 120 DEG C of vacuum
Pole.Lithium ion is tested battery and is assembled in the glove box full of argon gas, and metallic lithium foil is to electrode and reference electrode poly- third
Alkene film (Celgard-2300) is diaphragm, 1.0M LiPF6EC/DMC solution (volume ratio 1: 1) be electrolyte.At room temperature
The electrochemical lithium storage performance of constant current charge-discharge experiment test and the more above-mentioned composite material being prepared, charging and discharging currents exist
100-1000mA/g, voltage cut-off section are 3.0~0.005V.
The XRD characterization of Fig. 1 is the results show that MoS2/ graphene composite material is in 2 θ=14.4 °, 32.7 °, 33.5 ° and
57.2 ° show 4 diffraction maximums, correspond to 2H-MoS2(002) of (JPCDS no.37-1492), (100), (101), (110)
Face.In addition, occurring 1 new diffraction maximum (* label), interlamellar spacing 0.96nm at 2 θ=9.2 °.Bi2S3/ graphene is compound
The XRD diagram of material meets Bi2S3Standard diffraction card (JPCDS No.17-0320), stronger diffraction maximum illustrates Bi2S3
With good crystallinity.Fig. 1 (b, c, d) is shown for Bi2S3-MoS2/ graphene composite nano material, with Bi content
Increase, Bi2S3XRD peak intensity gradually increase, and MoS2XRD peak intensity gradually die down, this is mainly due in hydrothermal solution
Bi3+Presence and Bi2S3And MoS2Syntrophism results in MoS2Crystallinity reduce, in addition with crystallizing more preferable Bi2S3Contain
The increase of amount, MoS2Content it is relatively low, make to crystallize low MoS in composite material2The peak XRD be barely perceivable.
The SEM morphology characterization of Fig. 2 shows, MoS2/ graphene composite material shows the MoS largely intersected2Nanometer sheet is dispersed in
On graphene.Bi2S3/ graphene composite material shows the Bi of olive shape2S3Particle is evenly dispersed on graphene.From Fig. 2
(b, c, d) is as can be seen that with Bi2S3The increase of content, composite material pattern gradually change, especially Bi2S3-MoS2/
The composite material of graphene -2 (Bi: Mo=1: 4) shows many tiny Bi2S3Nanoparticle and curved MoS2Nanometer sheet
After forming composite construction, it is uniformly dispersed on the surface of graphene.
The TEM/HRTEM characterization result of Fig. 3 shows, MoS2The display of/graphene composite material intersects curved MoS2Nanometer sheet
In dispersion on the surface of graphene.The interlamellar spacing of 0.64nm corresponds to MoS in Fig. 3 (b)2(002) face, the interlamellar spacing of 0.95nm is corresponding
The peak * in XRD diagram.Bi2S3/ graphene composite material shows Bi2S3Particle is grown on graphene, and partial size is about 140-
320nm, interlamellar spacing are that 0.39nm and 0.50nm respectively corresponds (220) and (120) face.Bi2S3Regular lattice fringe illustrates its tool
The crystallinity having had.Fig. 3 (c-h) shows and MoS2/ graphene is compared, Bi2S3-MoS2/ graphene composite nano material shows,
It is dispersed in MoS on graphene2Nanometer sheet has the less number of plies, and more boundaries and disordered structure.Especially MoS2-
Bi2S3The composite nano materials sample of/graphene -2 (Bi: Mo=1: 4), MoS2The number of plies of nanometer sheet significantly reduces, and occurs
Many short sheet-like morphologies, with more tiny Bi2S3Nanocomposites together after, equably load on the surface of graphene.
Fig. 4 is the different composite material electrodes charge-discharge performance under 100mA/g current density at room temperature, with MoS2/
Graphene and Bi2S3/ graphene composite material is compared, Bi2S3-MoS2/ graphene composite nano material shows higher electrification
Learn storage lithium reversible specific capacity and excellent stable circulation performance, especially Bi2S3-MoS2/ graphene -2 (Bi: Mo=1: 4) is compound
Nano material, electrochemical lithium storage reversible capacity reach 1140mAh g-1, its reversible specific capacity still maintains after 100 circles recycle
In 1117mAh g-1, compared to the 1st circle almost without the decaying of capacity, it is shown that excellent charge-discharge performance.Phase therewith
Than MoS2The electrochemical lithium storage reversible specific capacity of/graphene composite material is 952mAh g-1, its reversible ratio after 100 circles recycle
Capacity is 891mAh g-1;Bi2S3The reversible specific capacity of/graphene composite material is 946mAh g-1, but with circulating ring number
Increase, reversible specific capacity is decreased obviously, and reversible specific capacity is 732mAh g after 100 circle circulations-1, for reversible specific volume for the first time
The 77.3% of amount.Therefore, Bi2S3-MoS2/ graphene composite nano material and MoS2/ graphene and Bi2S3/ graphene is compared, no
Higher electrochemical lithium storage reversible specific capacity is only shown, and there is better charge and discharge cycles stability.
Fig. 5 is the multiplying power property test result under different charging and discharging currents density, with MoS2/ graphene and Bi2S3/ stone
Black alkene composite electrode is compared, Bi2S3-MoS2/ graphene composite nano material not only has higher electrochemical lithium storage reversible
Specific capacity, and show the high power charging-discharging characteristic further enhanced.Fig. 5 is shown, is 500 in charging and discharging currents density
When with 1000mA/g, Bi2S3-MoS2The electrochemical lithium storage reversible specific capacity of/graphene -2 (Bi: Mo=1: 4) composite nano materials
Respectively 973 and 870mAh g-1, and show stable cycle performance.It in contrast, is 500 Hes in charging and discharging currents density
When 1000mA/g, MoS2It is respectively 803 and 711mAh g that/graphene composite material electrode electro Chemical, which stores up lithium reversible specific capacity,-1,
Bi2S3/ graphene is 745 and 593mAh g respectively-1.Therefore, with MoS2/ graphene and Bi2S3/ graphene composite material phase
Than Bi2S3-MoS2/ graphene composite nano material shows the high power charging-discharging characteristic further significantly increased.
Claims (2)
1. a kind of Bi2S3-MoS2/ graphene composite nano material, which is characterized in that the composite material is that have Bi2S3Nanoparticle
And MoS2Nanometer sheet is compound, and is equably formed on graphene, and wherein the molar ratio of Bi and Mo is 1: 9~1: 4.
2. Bi described in a kind of claim 12S3-MoS2The preparation method of/graphene composite nano material, which is characterized in that described
Steps are as follows for preparation method:
(1) by the Bi (NO of metering3)3·5H2O、Na2MoO4·2H2O and L-cysteine are add to deionized water, and sufficiently
Stirring, obtains uniform mixed solution, Bi (NO in hydro-thermal reaction solution3)3With Na2MoO4The ratio between the amount of substance be 1: 9~1:
4, the amount of the substance of L-cysteine is Bi (NO3)3With Na2MoO45 times of the sum of the amount of substance;
(2) in deionized water by graphene oxide ultrasonic disperse, uniform suspension is obtained, stone will be aoxidized under constant stirring
Black alkene hanging drop is added in above-mentioned mixed solution, and continues to stir 2h, is calculated with the amount of the substance of carbon, the object of graphene oxide
The amount of matter is equal to Bi (NO3)3With Na2MoO42 times of the sum of the amount of substance;
(3) reaction mixture that step (2) obtains is transferred in the hydrothermal reaction kettle with polytetrafluoroethylliner liner, after sealing
Reacted at 200 DEG C for 24 hours, then cooled to room temperature, the precipitated product that hydro-thermal reaction is obtained is centrifugated, and spend from
Sub- water and dehydrated alcohol sufficiently wash, and obtain Bi after being finally dried in vacuo 12h at 80 DEG C253-Mo52/ graphene composite Nano
Material, the molar ratio of Bi and Mo therein are 1: 9~1: 4.
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CN111710754A (en) * | 2020-05-11 | 2020-09-25 | 桂林理工大学 | Bi preparation by two-phase one-step solvothermal method2S3Method for preparing-graphene-ZnS photoelectric composite material |
CN113437277A (en) * | 2021-07-20 | 2021-09-24 | 广东工业大学 | Bi2S3/NiS2@ C negative electrode material, sodium ion battery and preparation method of sodium ion battery |
CN114094078A (en) * | 2021-11-16 | 2022-02-25 | 中国科学院深圳先进技术研究院 | Nitrogen-doped carbon-coated metal sulfide heterojunction material, preparation method and battery application |
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CN113437277A (en) * | 2021-07-20 | 2021-09-24 | 广东工业大学 | Bi2S3/NiS2@ C negative electrode material, sodium ion battery and preparation method of sodium ion battery |
CN114242964A (en) * | 2021-11-08 | 2022-03-25 | 南京航空航天大学 | Electrode material for lithium ion battery cathode and preparation method thereof |
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