CN106384811A - Blue phosphorus/transition metal disulfide heterojunction anode material and preparation method thereof - Google Patents
Blue phosphorus/transition metal disulfide heterojunction anode material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- 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
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Abstract
The invention relates to a blue phosphorus/transition metal disulfide heterojunction anode material and a preparation method thereof. According to the technical scheme, the method comprises the following steps of: based on computational simulation of a first principle method of a density function theory, screening a blue phosphorus/transition metal disulfide heterojunction, and further designing a method for preparing the heterojunction; preparing transition metal disulfide by adopting a chemical vapor deposition method; and uniformly stirring and mixing the transition metal disulfide, white phosphorus powder and an organic solvent, performing centrifugal treatment, and performing annealing treatment in vacuum or argon atmosphere, thereby obtaining the blue phosphorus/transition metal disulfide heterojunction anode material. The anode material prepared by the invention has high structure stability, conductivity, flexibility, high lithium adsorption capacity and good electrical properties, and the preparation process is simple, high in repeatability, high in yield, low in cost and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to technical field of nano material, a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material is proposed
Material.
Background technology
Two-dimentional transition metal dichalcogenide（transition metal dichalcogenides, TMDs）, typically chemistry
Formula form is MX2, wherein M can be iv, V, VI main group transition metal, and X is chalcogen S, Se, Te, such as MoS2And NbS2,
Cause extensive concern, not only due to its unique electronics and catalytic performance, due also in its relative broad range by strain or
The adjustability to its energy band engineering for the vertical electric field.
Elemental phosphorous have four kinds of allotropes, that is,：White phosphorus, red phosphorus, violet phosphorus and black phosphorus（BP）.From experimentally finding two dimension
Material black phosphorus, Zhu etc. further provides the phosphorus of another kind of form of only two atomic layers thick：Blue phosphorus（Blue
Phosphorus, BlueP）[Zhen Zhu, and David Tománek, Semiconducting Layered Blue
Phosphorus: A Computational Study, Phys. Rev. Lett, 2014, 112(17): 176802].
BlueP has the same heat stability of same BP, and has outstanding process based prediction model.BlueP, MX of stratiform2It is all six
The crystal of square structure, and only have 2% lattice mismatch, this is conducive to building high-quality Van der Waals hetero-junctions.And
BlueP and MX2There are a big specific surface area, therefore, BlueP/MX2Van der Waals hetero-junctions can form a fold
Surface, this be storage lithium ion provide bigger space.Simple " cooking formula " research and development prepared by test are had
Blindness, research cost is high, and efficiency of research and development is low.
Present invention building structure first, carries out material prescription and microcosmic using the first-principles calculations based on Density functional
Structure design, systematically have studied multiple BlueP/MX2The structural stability of Van der Waals hetero-junctions, electronic structure be modified,
Mechanical property, electrochemical properties of lithium absorption etc.；Screening obtains with satisfactory electrical conductivity, mechanical flexibility and has higher further
Lithium memory capacity blue phosphorus/transition metal dichalcogenide hetero-junctions；Finally by the technology of preparing of unique low-dimensional materials, real
Existing high-performance BlueP/MX2Heterojunction material synthetically prepared.
Content of the invention
In order to solve the blindness experimental study exploitation of " the cooking formula " of time-consuming consuming, improve research and development efficiency, reduce
Research and development cost, the first principle based on Density functional for the present invention, systematically have studied BlueP/MX2The structure of hetero-junctions
Stability, electronic structure modification, mechanical property, electrochemical properties etc. of lithium absorption, carry out the recipe calculation of material and microcosmic
Structure design, proposes a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material and preparation method thereof, prepared this material
As lithium ion battery anode material, there is good structural stability and mechanical flexibility, its electrical performance is good simultaneously.
A kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material, it is made up of following raw material：Transiting metal oxidation
Thing, white phosphorus powder, sulfur family non-metal powder and organic solvent.
Wherein according to the molar ratio, transition metal oxide：White phosphorus powder：Sulfur family non-metal powder：Organic solvent=2:1:7:
16.
Described sulfur family non-metal powder is sulphur powder, selenium powder, the one of which of tellurium powder.
Described transition metal oxide is MoO3、WO3、NbO3、TaO3One of which.
Described organic solvent is dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone and isopropanol its
One of or two kinds.
The method preparing described anode material, comprises the following steps that：
（1）Weigh each material according to formula proportion respectively；
（2）With acetone, ethanol, glass substrate is cleaned by ultrasonic successively, then deionized water rinses glass substrate surface 3-
5 times；
（3）Glass substrate and transition metal oxide are placed in the reaction chamber of plasma enhanced chemical vapor deposition, take out true
Empty to 3 × 104~4×104Pa, is passed through argon with 35 ~ 45sccm flow；Sulfur family non-metal powder is heated to by heating furnace
450 ~ 990 DEG C are changed into the nonmetallic steam of sulfur family；The temperature of described reaction chamber is heated to 650 ~ 950 DEG C of holding 2 ~ 3h, then plus
Heat to 750 ~ 1050 DEG C keeps 4 ~ 6h；Using argon, nonmetallic for gained sulfur family steam is blown into reaction chamber simultaneously, and is continually fed into
Terminate to heating；Finally form transition metal dichalcogenide thin film in described substrate surface；
（4）With pocket knife, lower transition metal dichalcogenide thin film is cut from glass substrate, be placed in mortar being slowly ground to powder；
（5）By step（4）Transition metal dichalcogenide powder, white phosphorus powder and the organic solvent obtaining stirs 2 ~ 20h mixing all
Even, stand 8 ~ 10h, then by centrifugation, filtration, then with alcohol washes, obtain the hetero-junctions of blue phosphorus/transition metal dichalcogenide again
Compound；
（6）By step（5）Prepared product, in vacuum or argon gas atmosphere, is made annealing treatment in 700 ~ 900 DEG C, annealing time
For 5 ~ 8h, obtain described blue phosphorus/transition metal dichalcogenide hetero-junctions anode material.
The present invention has advantages below compared with the prior art：
（1）The first-principles method based on Density Functional Theory for the present invention, it is to avoid the experiment repeatedly of blindness " cooking formula ",
Carry out the recipe calculation of material and the structure design of microcosmic, prepared by vapour deposition process and there is good Stability Analysis of Structures
Property, electric conductivity, flexible and larger lithium adsorption capacity Van der Waals hetero-junctions-indigo plant phosphorus/transition metal dichalcogenide different
Matter is tied, and in this, as lithium ion battery anode material；
（2）Present invention further proposes the controlled low-dimensional indigo plant phosphorus/transition metal dichalcogenide hetero-junctions flexible anode material of the number of plies
The preparation method of material.By controlling transition metal dichalcogenide powder, white phosphorus powder and ORGANIC SOLVENT MIXTURES equipped with a high speed
The control to realize the number of plies for the cutting mixing time in the agitator of rotary cutter.Mixing time is longer, and the blue phosphorus preparing/
Transition metal dichalcogenide heterojunction material is thinner, and the corresponding number of plies is fewer.
（3）Preparation process is simple of the present invention, repeatable strong, high yield rate, low cost, it is suitable to industrialization and give birth on a large scale
Produce, there is notable social benefit and economic benefit.
Brief description
Fig. 1 is monolayer indigo plant phosphorus/NbS2, blue phosphorus/TaS2The band structure of hetero-junctions, wherein fermi level are arranged on 0eV.
Fig. 2 is (a) monolayer indigo plant phosphorus/NbS2, (b) indigo plant phosphorus/TaS2Hetero-junctions is respectively along zigzag and armchair shape side
To uniaxial stress-strain curve.
Fig. 3 is blue phosphorus/NbS2, blue phosphorus/TaS2The XRD spectrum of hetero-junction thin-film.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, and the content of protecting of the present invention is not limited to
In following examples.All impartial changes done according to scope of the present invention patent and modification, all should belong to the present invention covers model
Enclose.
Embodiment 1
A kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material, its raw material composition is as follows：According to the molar ratio：NbO3：In vain
Phosphor powder：Sulphur powder：Dimethyl sulfoxide=2:1:7:16.
Concrete preparation process is as follows：
（1）Weigh NbO according to formula proportion respectively3, white phosphorus, sulphur powder, each material of dimethyl sulfoxide；
（2）Using acetone soln, glass substrate is cleaned by ultrasonic, removes organic dirt of glass substrate surface, and adopt wine
Essence carries out to described glass substrate being cleaned by ultrasonic the acetone removing glass substrate surface, deionized water rinsing 3 times；
（3）By glass substrate and NbO3Powder is placed in the reaction chamber of plasma enhanced chemical vapor deposition, it is evacuated down to 3 ×
104Pa, is passed through high pure protective gas Ar, flow-control is in 35sccm；Sulphur powder is heated to 450 DEG C by heating furnace and is changed into sulfur
Steam；Using carrier gas, described sulfur steam is blown into and is equipped with glass substrate and NbO3The reaction chamber of powder；Temperature by described reaction chamber
Degree is heated to the first preset temperature（650℃）And keep the first Preset Time（2h）, now pressed powder appearance evaporation, so that institute
State NbO3Powder generates gaseous NbO with described sulfur steam reaction3-xAnd deposit on described substrate, wherein 0<X≤1, this process
Specifically reaction equation is：NbO3+SNbO3-x+x/2SO2；The temperature of described reaction chamber is heated to the second preset temperature（750
℃）And keep the second Preset Time（4h）, continue to be passed through sulfur steam, so that described sulfur steam continues and NbO3-xReaction, in substrate
Surface forms stratiform NbS2Thin film, the concrete reaction equation of this process is：NbO3-x+(7-x)/2SNbS2+(3-x)/2SO2；
（4）Then by NbS2Powder, white phosphorus powder and dimethyl sulfoxide are placed in the stirring for 300r/min rotary cutter equipped with rotating speed
Mix in bucket, under room temperature, cutting stirring 20h, then stands 8h, then by being centrifuged, filtering and clean, obtain with NbS2For substrate
The blue phosphorus of hexagonal structure, thus be obtained monolayer indigo plant phosphorus/NbS2Heterojunction composite；
（5）Finally by above-mentioned prepared blue phosphorus/NbS2Heterojunction composite, in vacuum atmosphere, is made annealing treatment in 700 DEG C,
Temperature retention time is 5h, obtains the controlled blue phosphorus/NbS of the low-dimensional number of plies2Hetero-junctions flexible anode material.
Embodiment 2
A kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material, its raw material composition is as follows：According to the molar ratio：TaO3：In vain
Phosphorus：Sulphur powder：Organic solvent=2:1:7:16.
Wherein said organic solvent is：In molar ratio, DMF：N-Methyl pyrrolidone=1:3.
（1）Weigh TaO according to formula proportion respectively3, white phosphorus, sulphur powder, N,N-dimethylformamide and N- crassitude
Each material of ketone mixed organic solvents；
（2）Using acetone soln, glass substrate is cleaned by ultrasonic, removes organic dirt of glass substrate surface, and adopt wine
Essence carries out to described glass substrate being cleaned by ultrasonic the acetone removing glass substrate surface, deionized water rinsing 3 times；
（3）By glass substrate and TaO3Powder is placed in the reaction chamber of plasma enhanced chemical vapor deposition, it is evacuated down to 4 ×
104Pa, is passed through high pure protective gas Ar, flow-control is in 45sccm；Sulphur powder is heated to 450 DEG C by heating furnace and is changed into sulfur
Steam；Using carrier gas, described sulfur steam is blown into and is equipped with glass substrate and TaO3The reaction chamber of powder；Temperature by described reaction chamber
Degree is heated to the first preset temperature（750℃）And keep the first Preset Time（3h）, now pressed powder appearance evaporation, so that institute
State TaO3Powder generates gaseous TaO with described sulfur steam reaction3-xAnd deposit on described substrate, wherein 0<X≤1, this process
Specifically reaction equation is：TaO3+STaO3-x+x/2SO2；The temperature of described reaction chamber is heated to the second preset temperature（800
℃）And keep the second Preset Time（5h）, continue to be passed through sulfur steam, so that described sulfur steam continues and TaO3-xReaction, in substrate
Surface forms stratiform TaS2Thin film, the concrete reaction equation of this process is：TaO3-x+(7-x)/2STaS2+(3-x)/2SO2；
（4）Then by TaS2Powder, white phosphorus powder and N,N-dimethylformamide and N-Methyl pyrrolidone mixed organic solvents
It is placed in the agitator equipped with high-speed rotation cutter head, under room temperature, cutting stirring 10h, stands 8h, then pass through centrifugation, filter and clear
Wash, obtain with TaS2For the blue phosphorus of the hexagonal structure of substrate, thus five layer of blue phosphorus/TaS is obtained2Heterojunction composite.
（5）Finally by above-mentioned prepared indigo plant phosphorus/TaS2Heterojunction composite, in vacuum atmosphere, carries out annealing treatment in 750 DEG C
Reason, temperature retention time is 7h, obtains the controlled blue phosphorus/TaS of the number of plies2Hetero-junctions flexible anode material.
Embodiment 3
A kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material, its raw material composition is as follows：According to the molar ratio：MoO3：In vain
Phosphorus：Tellurium powder：Methanol=2:1:7:16.
（1）Weigh MoO according to formula proportion respectively3, white phosphorus, tellurium powder, each material of methanol；
（2）Using acetone soln, glass substrate is cleaned by ultrasonic, removes organic dirt of glass substrate surface, and adopt wine
Essence carries out to described glass substrate being cleaned by ultrasonic the acetone removing glass substrate surface, deionized water rinsing 5 times；
（3）By glass substrate and MoO3Powder is placed in the reaction chamber of plasma enhanced chemical vapor deposition, is evacuated down to 3.5
×104Pa, is passed through high pure protective gas Ar, flow-control is in 45sccm；Tellurium powder is heated to 990 DEG C by heating furnace be changed into
Tellurium steam；Using carrier gas, described tellurium steam is blown into and is equipped with glass substrate and MoO3The reaction chamber of powder；By described reaction chamber
Temperature is heated to the first preset temperature（950℃）And keep the first Preset Time（3h）, now pressed powder appearance evaporation, so that
Described MoO3Powder generates gaseous MoO with described tellurium steam reaction3-xAnd deposit on described substrate, wherein 0<X≤1, this mistake
The concrete reaction equation of journey is：MoO3+TeMoO3-x+x/2TeO2；The temperature of described reaction chamber is heated to the second preset temperature
（1050℃）And keep the second Preset Time（6h）, continue to be passed through tellurium steam, so that described tellurium steam continues and MoO3-xReaction,
Form stratiform MoTe in substrate surface2Thin film, the concrete reaction equation of this process is：MoO3-x+(7-x)/2TeMoTe2+(3-
x)/2TeO2；
（4）Then by MoTe2Powder, white phosphorus powder and isopropanol organic solvent are placed in the agitator equipped with high-speed rotation cutter head
Interior, under room temperature, cutting stirring 4h, stands 8h, then by being centrifuged, filtering and clean, obtains with MoTe2Hexagonal structure for substrate
Blue phosphorus, thus be obtained 3-D solid structure blue phosphorus/MoTe2Complex.
（5）Finally by above-mentioned prepared indigo plant phosphorus/MoTe2Heterojunction composite, in vacuum atmosphere, carries out annealing treatment in 900 DEG C
Reason, temperature retention time is 8h, obtains the blue phosphorus/MoTe of three-dimensional2Hetero-junctions anode material.
The present invention is obtained with satisfactory electrical conductivity using the first-principles calculations based on density functional theory, screening（Energy
Band through fermi level, as shown in Figure 1）, mechanical flexibility（Single shaft limit tensile strain is 17%, as shown in Figure 2）And have higher
Lithium adsorption capacity（528 mAhg−1）Blue phosphorus/NbS2Hetero-junctions, it is better than Graphene（372 mAhg−1, limit tensile strain
For 15%）.And in lithium ion adsorption process, BlueP/NbS2The open-circuit voltage of hetero-junctions is positive, as shown in table 1 all the time.
BlueP/NbS2It is lithium battery flexible anode material that hetero-junctions is expected to application.In XRD spectrum, peak is more sharp, and degree of crystallinity is better.
Therefore as can be seen from Figure 3, BlueP/NbS2Hetero-junctions exists（002）The peak value of maximum is presented on face, and peak width is only 1 °, remaining is brilliant
Face all assumes the peak value of very little or peak, and BlueP/NbS is described2Hetero-junctions has good degree of crystallinity, and it has good
Good structural stability.
Table 1
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with repair
Decorations, all should belong to the covering scope of the present invention.
Claims (6)
1. a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material it is characterised in that：It is made up of following raw material：Cross
Cross metal-oxide, white phosphorus powder, sulfur family non-metal powder and organic solvent.
2. according to claim 1 a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material it is characterised in that：
According to the molar ratio, transition metal oxide：White phosphorus powder：Sulfur family non-metal powder：Organic solvent=2:1:7:16.
3. according to claim 1 a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material it is characterised in that：
Described sulfur family non-metal powder is sulphur powder, selenium powder, the one of which of tellurium powder.
4. according to claim 1 a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material it is characterised in that：
Described transition metal oxide is MoO3、WO3、NbO3、TaO3One of which.
5. according to claim 1 a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material it is characterised in that：
Described organic solvent is dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone and isopropanol one kind therein
Or it is two or more.
6. a kind of prepare as claimed in claim 1 a kind of indigo plant phosphorus/transition metal dichalcogenide hetero-junctions anode material method,
It is characterized in that：Comprise the following steps that：
（1）Weigh each material according to formula proportion respectively；
（2）With acetone, ethanol, glass substrate is cleaned by ultrasonic successively, then deionized water rinses glass substrate surface 3-
5 times；
（3）Glass substrate and transition metal oxide are placed in the reaction chamber of plasma enhanced chemical vapor deposition, take out true
Empty to 3 × 104~4×104Pa, is passed through argon with 35 ~ 45sccm flow；Sulfur family non-metal powder is heated to by heating furnace
450 ~ 990 DEG C are changed into the nonmetallic steam of sulfur family；The temperature of described reaction chamber is heated to 650 ~ 750 DEG C of holding 2 ~ 3h, then plus
Heat to 750 ~ 800 DEG C keeps 4 ~ 6h；Using argon, nonmetallic for gained sulfur family steam is blown into reaction chamber simultaneously, and be continually fed into
Heating terminates；Finally form transition metal dichalcogenide thin film in described substrate surface；
（4）With pocket knife, lower transition metal dichalcogenide thin film is cut from glass substrate, be placed in mortar being slowly ground to powder；
（5）By step（4）Transition metal dichalcogenide powder, white phosphorus powder and the organic solvent obtaining stirs 2 ~ 20h mixing all
Even, stand 8-10h, then by centrifugation, filtration, then with alcohol washes, obtain the hetero-junctions of blue phosphorus/transition metal dichalcogenide again
Compound；
（6）By step（5）Prepared product, in vacuum or argon gas atmosphere, is made annealing treatment in 700 ~ 900 DEG C, annealing time
For 5-8h, obtain described blue phosphorus/transition metal dichalcogenide hetero-junctions anode material.
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| CN107749433B (en) * | 2017-08-30 | 2023-07-04 | 中国科学院上海技术物理研究所 | Two-dimensional van der Waals heterojunction photoelectric detector and preparation method thereof |
| CN107919464A (en) * | 2017-10-27 | 2018-04-17 | 长江大学 | A kind of lithium ion battery telluride molybdenum anode material and preparation method thereof |
| CN107919464B (en) * | 2017-10-27 | 2018-08-17 | 长江大学 | A kind of lithium ion battery telluride molybdenum anode material and preparation method thereof |
| CN108408772A (en) * | 2018-04-27 | 2018-08-17 | 福州大学 | A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material |
| CN108408772B (en) * | 2018-04-27 | 2019-10-15 | 福州大学 | A kind of preparation method of black phosphorus/transition metal trisulfide heterojunction material |
| CN109668942A (en) * | 2019-01-28 | 2019-04-23 | 清华大学 | Two-dimensional metallic/oxide heterojunction, preparation method and sensor |
| CN109999847A (en) * | 2019-04-23 | 2019-07-12 | 福州大学 | A kind of preparation method of III-VI race heterojunction photocatalyst material |
| CN110714224A (en) * | 2019-09-17 | 2020-01-21 | 南京理工大学 | Preparation method of large-area high-stability single-layer blue phospholene based on molecular beam epitaxial growth |
| CN111470538A (en) * | 2020-03-25 | 2020-07-31 | 深圳先进技术研究院 | Method for modifying transition metal chalcogenide by phosphorus in molten system |
| CN111470538B (en) * | 2020-03-25 | 2022-08-05 | 深圳先进技术研究院 | Method for modifying transition metal chalcogenide by phosphorus in molten system |
| CN113053474A (en) * | 2021-04-13 | 2021-06-29 | 南京信息工程大学 | Light chargeable material screening system and operation method thereof |
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