CN111422906A - Preparation method of silylene and molybdenum disulfide lithium battery cathode composite material - Google Patents
Preparation method of silylene and molybdenum disulfide lithium battery cathode composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 30
- QWVMUSBBWGTKML-UHFFFAOYSA-N [Li].[Mo](=S)=S Chemical compound [Li].[Mo](=S)=S QWVMUSBBWGTKML-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 64
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 50
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000002135 nanosheet Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
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- 238000013329 compounding Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 239000011575 calcium Substances 0.000 claims description 14
- 229910004706 CaSi2 Inorganic materials 0.000 claims description 11
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000010410 layer Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 3
- 229910004709 CaSi Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000011630 iodine Substances 0.000 claims description 3
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 2
- -1 argon ions Chemical class 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 abstract description 6
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 239000007773 negative electrode material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
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- 239000002356 single layer Substances 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Abstract
The invention discloses a preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material, which comprises the steps of firstly, generating silylene nanosheets by adopting a molecular beam epitaxy method or a solid-phase reaction method; a hydrothermal method is adopted or a commercial molybdenum disulfide two-dimensional material is stripped and re-stacked, so that a re-stacked molybdenum disulfide nanosheet is prepared; and adding the silylene nanosheets and the molybdenum disulfide nanosheets into a proper amount of deionized water to prepare a suspension, fully dispersing the suspension, filtering the water, drying the water to realize pre-compounding of the two materials, further mixing the pre-compounded materials at a high speed, and finally obtaining the uniformly distributed silylene and molybdenum disulfide lithium battery cathode composite material. The prepared silylene material solves the problem of volume expansion of the traditional silicon material, improves the conductivity of the molybdenum disulfide material by combining the silylene material, and enables the silylene material and the molybdenum disulfide lithium battery cathode composite material to both exert the optimal performance of the two materials, so that an excellent lithium battery cathode material is obtained, and the overall performance of a lithium battery is improved.
Description
Technical Field
The invention relates to the field of lithium battery cathode materials, in particular to a preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material.
Background
With the development of the industry and the competition of the market, the requirements of the lithium battery on the performance, such as high energy density, safety performance, service life and the like, are further improved. The common negative electrode material of the lithium ion battery is graphite, the position where lithium ions can be intercalated is limited due to the small lattice constant, and the capacity value is low. In order to increase the energy density of lithium batteries, it is becoming a hot spot for current lithium ion battery research to find materials with higher capacity and cycle stability, and various types of lithium battery negative electrode materials are proposed and researched, such as silicon, graphene, molybdenum disulfide, and the like.
Compared with the traditional cathode material graphite, silicon has higher gram capacity and abundant reserves, but has the obvious defects that the volume expansion coefficient of silicon after lithium embedding reaches up to 300 percent, and the cycling performance of the battery is seriously influenced.
As a representative two-dimensional material, the transition metal sulfide molybdenum disulfide has very wide application prospects in the fields of materials science, spintronics, micro-nano processing, semiconductor devices and the like. The molybdenum disulfide material is widely researched and used as a lithium ion battery cathode material because atoms in a monolayer layer of the molybdenum disulfide material are combined by covalent bonds, and multiple layers of the molybdenum disulfide material are combined together by Van der Waals force, and the layered structure is favorable for the intercalation and deintercalation of lithium ions and has no serious volume expansion. By re-stacking the molybdenum disulfide material with increased layer spacing, a larger accommodation space can be obtained and the ion mobility of the material can be improved, so that the material has larger capacity and excellent rate capability.
As a negative electrode material of a lithium ion battery, the material can be modified in various ways such as nanocrystallization, doping, coating, compounding with other materials and the like, and the appropriate modification can improve various properties of the material, such as structural stability, gram-volume capacity, rate capability and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material, which solves the problem of volume expansion of the traditional silicon material by preparing a silylene material with two-dimensional characteristics, improves the conductivity of the molybdenum disulfide material by combining the silylene material, enables the silylene and molybdenum disulfide lithium battery cathode composite material to exert the optimal performance of the two materials, obtains an excellent lithium battery cathode material, and improves the overall performance of a lithium battery.
The technical scheme of the invention is as follows:
a preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material specifically comprises the following steps:
(1) generating a silylene nanosheet by adopting a molecular beam epitaxy method or a solid-phase reaction method;
(2) stripping and re-stacking commercial molybdenum disulfide two-dimensional materials by adopting a hydrothermal method to prepare re-stacked molybdenum disulfide nanosheets;
(3) adding the silylene nanosheets and the heavily-stacked molybdenum disulfide nanosheets into a proper amount of deionized water to prepare a suspension, fully dispersing the suspension, filtering water, drying the water to realize pre-compounding of the two materials, further mixing the pre-compounded materials at a high speed, and finally obtaining the uniformly-distributed silylene and molybdenum disulfide lithium battery cathode composite material.
In the step (1), the molecular beam epitaxy method for generating the silylene nanosheet specifically comprises the following steps: the Ag (111) substrate material is sputtered by argon ions in ultrahigh vacuum and annealed at the high temperature of 400-600 ℃ for 3-4 weeks; heating the small silicon wafers placed in the tantalum boat as silicon sources to 1200-1500 ℃, and maintaining the temperature of the Ag (111) substrate material to 210-230 ℃; finally, obtaining high-quality multi-layer silicon on the surface of the Ag (111) substrate through molecular beam epitaxy equipment, introducing a small amount of oxygen into a cavity of the molecular beam epitaxy equipment when the temperature is reduced to 190-210 ℃, chemically passivating the interface of a silicon source and the substrate material, and obtaining the independent silicon-alkene nanosheets through mechanical stripping.
In the step (1), the solid-phase reaction method for producing the silylene nanosheet specifically comprises the following steps: mixing high purity calcium and silicon in a stoichiometric excess of Ca and heating at elevated temperature to obtain polycrystalline CaSi2Then polycrystalline CaSi in the tantalum crucible2Packaging in a quartz tube, sintering at 1000-1200 deg.C for 1-1.5 hr, slowly cooling to 500 deg.C at 10 deg.C/h, and cooling to room temperatureThereby obtaining single crystal CaSi2Preparing the prepared single crystal CaSi2The material and the weak oxidant are subjected to local chemical reaction together to remove Ca metal ions, so that the independent silylene nanosheet is obtained.
In the step (2), the hydrothermal method for preparing the heavily-stacked molybdenum disulfide nanosheet comprises the following specific steps: and (3) putting ammonium molybdate tetrahydrate and thiourea into the ionized water, fully stirring, sealing, heating to the temperature of 160-220 ℃, maintaining for 24 hours, cooling to room temperature, and filtering, washing and drying to obtain the molybdenum disulfide nanosheet with large interlayer spacing.
In the step (2), the specific step of preparing the heavily-stacked molybdenum disulfide nanosheet by stripping and heavily-stacking the commercial molybdenum disulfide two-dimensional material is to soak the commercial molybdenum disulfide material in butyl lithium and keep the commercial molybdenum disulfide material in an argon atmosphere for one week to obtain the lithium-intercalated molybdenum disulfide L iMoS2Then L iMoS2And finally, the molybdenum disulfide layered material is subjected to hydrothermal method at 180 ℃ for about 50 hours to realize the re-stacking of the material, so as to prepare the re-stacked molybdenum disulfide nanosheet.
In the step (3), the mass ratio of the silylene nanosheets to the heavily-stacked molybdenum disulfide nanosheets is 1.9-2.1: 1.
In the step (3), the drying temperature is 75-85 ℃, and the drying time is 3.5-4.5 hours.
In the step (3), the specific steps of high-speed mixing are as follows: mixing is first carried out at low speed 100-.
The molar ratio of the high-purity calcium to the high-purity silicon is 1-1.2: 2.
the single crystal CaSi2The material and weak oxidant iodine are put into methyl cyanide solvent together to carry out local chemical reaction for 4 weeks so as to remove Ca metal ions, thereby obtaining independent silylene nano-sheets.
The invention has the advantages that:
(1) according to the invention, by preparing the two-dimensional silylene nanosheet, the problem that the volume expansion in the traditional silicon negative electrode material affects the material performance is effectively solved.
(2) The main purpose of the heavy-stacking molybdenum disulfide nanosheets is to increase the interlayer spacing of the material, so that the material has larger space capacity and better ion transmission performance.
(3) According to the invention, the problem of conductivity of the molybdenum disulfide material is solved by compounding the silylene nanosheet and the molybdenum disulfide nanosheet, and meanwhile, the composite material enables the two materials to exert the optimal performance, so that the overall performance of the lithium ion battery is improved, and the lithium battery cathode material with excellent performance is obtained.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) representation of a silylene and molybdenum disulfide lithium battery negative electrode composite of the invention.
FIG. 2 is a normal temperature cycle curve diagram of the silylene and molybdenum disulfide lithium battery negative electrode composite material of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material specifically comprises the following steps:
(1) and adopting a solid-state reaction method to generate a silylene nanosheet:
mixing high-purity calcium and silicon with Ca excess stoichiometric composition (molar ratio of Ca to Si is 1.1: 2), introducing argon as protective atmosphere, and heating at high temperature in tantalum crucible to obtain polycrystalline CaSi2Then polycrystalline CaSi in the tantalum crucible2Is packaged in a quartz tube, sintered at 1100 deg.C for 1 hr, and thenSlowly cooling to 500 ℃ at the speed of 10 ℃/h, and then cooling to room temperature, thereby obtaining the single crystal CaSi2Preparing the prepared single crystal CaSi2Putting the material and weak oxidant iodine into a methyl cyanide solvent together for local chemical reaction for 4 weeks to remove Ca metal ions, thereby obtaining independent silylene nanosheets;
(2) stripping and re-stacking a commercial molybdenum disulfide two-dimensional material to prepare a re-stacked molybdenum disulfide nanosheet:
soaking commercial molybdenum disulfide material in butyl lithium, and keeping the butyl lithium in an argon atmosphere for one week to obtain the lithium intercalation molybdenum disulfide L iMoS2L iMoS2Placing the material in water, performing oxidation-reduction reaction to obtain a stripped molybdenum disulfide layered material, and finally performing re-stacking on the molybdenum disulfide layered material at 180 ℃ for about 50 hours by a hydrothermal method to obtain a re-stacked molybdenum disulfide nanosheet;
(3) adding a silylene nanosheet and a heavily-stacked molybdenum disulfide nanosheet into a proper amount of deionized water to prepare a suspension and fully disperse the suspension, wherein the mass ratio of the silylene nanosheet to the heavily-stacked molybdenum disulfide nanosheet is 2:1, then pre-compounding the silylene nanosheet and the heavily-stacked molybdenum disulfide nanosheet by mixing and filtering, and drying in a 80 ℃ oven for 4 hours in vacuum, finally pre-compounding the two materials, and finally mixing the pre-compounded materials at a high speed through a high-speed mixer, firstly mixing at a low speed of 100 plus materials and 300rpm for 5 minutes, then mixing at a high speed of 700 plus materials and 1500rpm for 20 minutes, and finally obtaining the silylene and molybdenum disulfide lithium battery cathode composite.
Fig. 1 is an SEM characterization diagram of the silylene and molybdenum disulfide lithium battery negative electrode composite material, and it can be seen that the prepared silylene and molybdenum disulfide lithium battery negative electrode composite material has a good two-dimensional sheet structure and is well compounded.
FIG. 2 is a normal temperature cycle curve of the negative electrode composite material of the silylene and molybdenum disulfide lithium battery, which shows that the negative electrode composite material of the silylene and molybdenum disulfide lithium battery has excellent cycle performance under high current with high gram capacity of 900mAh/g and 1A/g.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of a silylene and molybdenum disulfide lithium battery cathode composite material is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) generating a silylene nanosheet by adopting a molecular beam epitaxy method or a solid-phase reaction method;
(2) stripping and re-stacking commercial molybdenum disulfide two-dimensional materials by adopting a hydrothermal method to prepare re-stacked molybdenum disulfide nanosheets;
(3) adding the silylene nanosheets and the heavily-stacked molybdenum disulfide nanosheets into a proper amount of deionized water to prepare a suspension, fully dispersing the suspension, filtering water, drying the water to realize pre-compounding of the two materials, further mixing the pre-compounded materials at a high speed, and finally obtaining the uniformly-distributed silylene and molybdenum disulfide lithium battery cathode composite material.
2. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the molecular beam epitaxy method for generating the silylene nanosheet specifically comprises the following steps: the Ag (111) substrate material is sputtered by argon ions in ultrahigh vacuum and annealed at the high temperature of 400-600 ℃ for 3-4 weeks; heating the small silicon wafers placed in the tantalum boat as silicon sources to 1200-1500 ℃, and maintaining the temperature of the Ag (111) substrate material to 210-230 ℃; finally, obtaining high-quality multi-layer silicon on the surface of the Ag (111) substrate through molecular beam epitaxy equipment, introducing a small amount of oxygen into a cavity of the molecular beam epitaxy equipment when the temperature is reduced to 190-210 ℃, chemically passivating the interface of a silicon source and the substrate material, and obtaining the independent silicon-alkene nanosheets through mechanical stripping.
3. The silicon-ene-molybdenum disulfide lithium battery of claim 1The preparation method of the cathode composite material is characterized by comprising the following steps: in the step (1), the solid-phase reaction method for producing the silylene nanosheet specifically comprises the following steps: mixing high purity calcium and silicon in a stoichiometric excess of Ca and heating at elevated temperature to obtain polycrystalline CaSi2Then polycrystalline CaSi in the tantalum crucible2Encapsulating in a quartz tube, sintering at 1000-1200 deg.C for 1-1.5 hr, slowly cooling to 500 deg.C at 10 deg.C/h, and cooling to room temperature to obtain single crystal CaSi2Preparing the prepared single crystal CaSi2The material and the weak oxidant are subjected to local chemical reaction together to remove Ca metal ions, so that the independent silylene nanosheet is obtained.
4. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the hydrothermal method for preparing the heavily-stacked molybdenum disulfide nanosheet comprises the following specific steps: and (3) putting ammonium molybdate tetrahydrate and thiourea into the ionized water, fully stirring, sealing, heating to the temperature of 160-220 ℃, maintaining for 24 hours, cooling to room temperature, and filtering, washing and drying to obtain the molybdenum disulfide nanosheet with large interlayer spacing.
5. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein in the step (2), the step of peeling and re-stacking the commercial molybdenum disulfide two-dimensional material to prepare the re-stacked molybdenum disulfide nanosheet comprises the specific steps of soaking the commercial molybdenum disulfide material in butyl lithium, and keeping the butyl lithium in an argon atmosphere for one week to obtain the lithium intercalated molybdenum disulfide L iMoS2Then L iMoS2And finally, the molybdenum disulfide layered material is subjected to hydrothermal method at 180 ℃ for about 50 hours to realize the re-stacking of the material, so as to prepare the re-stacked molybdenum disulfide nanosheet.
6. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the mass ratio of the silylene nanosheets to the heavily-stacked molybdenum disulfide nanosheets is 1.9-2.1: 1.
7. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the drying temperature is 75-85 ℃, and the drying time is 3.5-4.5 hours.
The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 1, wherein the method comprises the following steps: in the step (3), the specific steps of high-speed mixing are as follows: mixing is first carried out at low speed 100-.
8. The method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 3, wherein the method comprises the following steps: the molar ratio of the high-purity calcium to the high-purity silicon is 1-1.2: 2.
9. the method for preparing the negative electrode composite material of the silylene and molybdenum disulfide lithium battery as claimed in claim 3, wherein the method comprises the following steps: the single crystal CaSi2The material and weak oxidant iodine are put into methyl cyanide solvent together to carry out local chemical reaction for 4 weeks so as to remove Ca metal ions, thereby obtaining independent silylene nano-sheets.
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