CN106571244A - Two-dimensional transition metal carbon (nitrogen) compound and two-dimensional transition metal sulfide nano-composite powder, and preparation and application thereof - Google Patents
Two-dimensional transition metal carbon (nitrogen) compound and two-dimensional transition metal sulfide nano-composite powder, and preparation and application thereof Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- 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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a two-dimensional transition metal carbon (nitrogen) compound and two-dimensional transition metal sulfide nano-composite powder, and a preparation and application thereof. The nano-composite powder is formed by the uniform scattered recombination of a two-dimensional transition metal carbon (nitrogen) compound nanosheet and a two-dimensional transition metal sulfide nanosheet, wherein the percentage of the mass of the two-dimensional transition metal sulfide to the total mass of the nano-composite powder is 10%-99%. The method comprises the steps: enabling the steady suspension liquid of the two-dimensional transition metal carbon (nitrogen) compound nanosheet and the suspension liquid of the two-dimensional transition metal sulfide nanosheet are mixed according to a proportion; carrying out cooling and drying after supersonic mixing, and then obtaining the nano-composite powder. The nano-composite powder is simple in preparation, is safe and high in efficiency, is low in cost, remarkably irons out the defects of conductivity of the two-dimensional transition metal sulfide, and can regulate the conductivity through proportion change. The nano-composite powder serves as a negative electrode of a lithium ion battery and the electrode material of a supercapacitor, is good in application prospect in the field of energy storage devices, and is better in electrochemical performance than the two-dimensional transition metal sulfide.
Description
Technical field
The invention belongs to nano composite material technical field, and in particular to a kind of two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound with
Two-dimentional transition-metal sulphides composite nano-powder and its preparation and application.
Background technology
Lithium ion battery has the advantages that energy density is high and has extended cycle life, and obtains as the power supply of portable electric appts
To being widely applied.Current commercial Li-ion batteries are mainly using graphite as negative pole, but the theoretical capacity of graphite is relatively low
(372mAh/g), this causes lithium ion battery to be difficult to meet especially new in fields such as some high-energy-densities, high power densities
The application requirement of energy electric vehicle.Electrode material is a key factor for affecting performance of lithium ion battery.Two-dimentional material with carbon element
Since Graphene finds, its high electrical conductivity and nuclear power mobility, big surface area, good pliability have attracted research people
Application of the member to which in lithium ion battery has carried out widely studied.Graphene and its composite are used as lithium ion battery negative
Show the electrochemical lithium storage cyclical stability for significantly increasing and the rate charge-discharge characteristic [Rinaldo of improvement
Raccichini,Alberto Varzi,Stefano Passerini,Bruno Scrosati,The role of
graphene for electrochemical energy storage.Nature Materials,2015,14:271-
279]。
Magnesium-yttrium-transition metal disulphide (transition metal dichalcogenides, abbreviation TMDs) with stone
The similar layer structure of ink, can make the embedded abjection molecule lamellar spacing of Li ions, be the new lithium ion battery negative material of a class,
Transition-metal sulphides after stripping are the two dimensional crystals with class graphene-structured, compared with TMDs bodies material more suitable for making
Negative pole [Huang X, Zeng Z-Y, Zhang H.Metal dichalcogenide nanosheets for lithium ion battery:
preparation,properties and applications.Chem Soc Rev,2013,42:1934-1946].Two sulfur
Change molybdenum MoS2It is the Typical Representative of transition-metal sulphides, research shows, two-dimentional MoS2Nanometer sheet is used as lithium ion battery negative
Material shows higher electrochemical lithium storage content (850～1000mAh/g) and the cycle performance for improving.But due to discharge and recharge
There is the accumulation of nanometer sheet and unstable, the single MoS of the Li ions structure that deintercalation causes repeatedly in journey2The cyclicity of negative pole
Can poor [Xiao J, Choi D W, Cosimbescu L, etal.Exfoliated MoS2nano compsite as an
anode material for lithium ion batteries.Chem Mater,2010,22(16):4522-4524.] this
Outward, the electric conductivity of two-dimentional transition-metal sulphides is generally poor, this be also restrict one of its chemical property and application it is heavy
Want factor.Due to two-dimentional MoS2Nanometer sheet has similar microstructure and pattern with graphene nanometer sheet, and both are compound to have
The good compatibility, recently, the MoS that research worker will be peeled off2Composite is prepared for lithium ion battery negative with Graphene.
As a result show, during the compound electric conductivity for significantly enhancing combination electrode material of Graphene and electrochemistry storage lithium, electronics is passed
Pass ability.Combination electrode material show excellent electrochemical lithium storage content (1022mAh/g), more preferable stable circulation performance and
Significantly increase charge-discharge magnification performance [horse beautiful jade, normal Kun, Chen Weixiang. slightly peel off molybdenum bisuphide/graphene composite material system
Standby and its electrochemical lithium storage performance. Chinese science and technology paper, 2013,8 (12)：1247-1251].
Two-dimensional material adds a new family again recently：Two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound, abbreviation MXene, its
Chemical general formula is Mn+1XnTx(M is early stage transiting group metal elements, and X is carbon or/and nitrogen, and n=1,2 or 3, T represent-F ,-O
And the surface functional group such as-OH, monolayer Mn+1XnNanometer sheet replaces stacking by n-layer X atom and n+1 layer M atoms and forms, M atomic layers position
In outermost layer).It is that (chemical formula is M from ternary layered compound MAX phasesn+1AXn, the wherein implication and M of M, X, nn+1XnTxIn
As, A be III, IV major element) in selective corrosion go out the new class Graphene two dimensional crystal of a class obtained by A layer atoms.
The MXene for having prepared at present has Ti3C2Tx、Ti2CTx、(Ti0.5,Nb0.5)2CTx、(V0.5,Cr0.5)3C2Tx、Ti3CNTx、
Ta4C3Tx、V2CTx、Nb2CTx、Nb4C3Tx、(Nb0.8,Ti0.2)4C3Tx、(Nb0.8,Zr0.2)4C3Tx、Mo2TiC2Tx、Mo2Ti2C3Tx、
Mo2CTx、Cr2TiC2Tx、Zr3C2Tx、Ti4N3Tx[Anasori B,Xie Y,Beidaghi M,et al.Two-
Dimensional,Ordered,Double Transition Metals Carbides(MXenes),ACS Nano,2015,9
(10):9507-9516.Zhou J,Zha X-H,Chen F-Y,et al.A Two-Dimensional Zirconium
Carbide by Selective Etching of Al3C3from Nanolami-nated Zr3Al3C5,Angew Chem
Int Edit,2016,55(16):5008-5013.]。Ti3C2TxIt is the MXene of current most study.MXene has unique
Two-dimensional slice structure and good conductive and mechanical performance, therefore in energy storage, catalysis, composite, environmental improvement etc.
Field has broad application prospects [Naguib M, Mochalin V N, Barsoum M W, et al.25th
Anniversary Article:MXenes:A New Family of Two-Dimensional Materials,Advanced
Materials,2014,26(7):992-1005.], especially as electrochemical energy storage part such as ultracapacitor and lithium
The electrode material of ion battery has shown outstanding performance [Naguib M, Halim J, Lu J, et al.New Two-
Dimensional Niobium and Vanadium Carbides as Promising Materials for Li-Ion
Batteries,Journal of the Ameri-can Chemical Society,2013,135(43):15966–
15969.Lukatskaya M R,Mashtalir O,Ren C E,et al.Cation Intercalation and High
Volumetric Capacitance of Two-dimensional Titanium Carbide,Science,2013,341
(6153):1502-1505.]。
Based on two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene and two-dimentional transition-metal sulphides in crystal structure and micro-
The complementarity in the matching and electric property on pattern is seen, by both the compound mutual supplement with each other's advantages and collaboration for being capable of achieving both performances
Effect, has a good application prospect in electrochemical energy field of storage.
The content of the invention
It is an object of the invention to provide a kind of two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound and two-dimentional magnesium-yttrium-transition metal sulfuration
Thing composite nano-powder, it is a further object of the present invention to provide the preparation method of above-mentioned composite nano-powder, the present invention also has individual
Purpose is to provide the application of above-mentioned composite nano-powder.
The technical scheme is that：Two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound and two-dimentional transition-metal sulphides nanometer
Composite granule, it is characterised in that：The composite nano-powder is by two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound nanometer sheet and two-dimentional transition
Race's nano metal sulfide piece is dispersed to be composited, wherein the quality of two-dimentional transition-metal sulphides to account for composite granule total
The percentage composition of quality is 10～99%.
It is preferred that above-mentioned two-dimentional magnesium-yttrium-transition metal (nitrogen) compound is Ti3C2Tx、Ti3CNTx、Ti2CTx、(Ti0.5,Nb0.5)2CTx、(V0.5,Cr0.5)3C2Tx、Ta4C3Tx、V2CTx、Nb2CTx、Nb4C3Tx、(Nb0.8,Ti0.2)4C3Tx、(Nb0.8,Zr0.2)4C3Tx、
Mo2TiC2Tx、Mo2Ti2C3Tx、Mo2CTx、Cr2TiC2Tx、Zr3C2TxOr Ti4N3TxDeng；Described two-dimentional transition-metal sulphides
For MoS2、WS2Or CoS2Deng.
Present invention also offers above-mentioned two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound is received with two-dimentional transition-metal sulphides
The method of rice composite granule, it is characterised in that comprise the following steps that：
Two-dimentional transition-metal sulphides nanometer sheet suspension is added to into two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene
In nanometer sheet suspension, ultrasound makes two kinds of suspension mix homogeneously, then freeze-dried to obtain two-dimentional magnesium-yttrium-transition metal carbon
(nitrogen) compound nanometer sheet and two-dimentional transition-metal sulphides composite nano-powder.
It is preferred that above-mentioned two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer sheet suspension is prepared into by following methods
Arrive, concretely comprise the following steps：LiF is dissolved in hydrochloric acid, the leaching of ternary layered compound MAX powder is slowly added to into above-mentioned solution then
In, the magnetic agitation reaction at 30～40 DEG C, product adopt washing with alcohol to be centrifuged to supernatant pH value as 6.2～6.5,
Dried solid sample is added in deionized water, under flowing argon protection, ultrasound is peeled off, be then centrifuged for obtaining few layer or
The stable suspension of monolayer magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer sheet.
It is preferred that preparing the rotating speed of magnetic agitation during two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer sheet suspension
For 250-550rpm, the time of magnetic agitation is 6～24h；Supersonic frequency when described ultrasound is peeled off is 40-100kHz, is surpassed
The time that sound is peeled off is 0.5～2h；After ultrasound is peeled off, centrifugal rotational speed is 3000-4000rpm, and centrifugation time is 0.5～1.5h.
It is preferred that above-mentioned two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound suspension concentration is 0.2-1.5mg/ml；Described two dimension
Transition-metal sulphides nanometer sheet suspension concentration is 0.5-2mg/ml.
Described two-dimentional transition-metal sulphides nanometer sheet is prepared using lithium graft process, is not limited to using lithium graft process system
It is standby.
It is preferred that above-mentioned ultrasonic mixing refers to that ultrasound 0.2-1h is mixed under power of the ultrasonic power for 30-150W.
It is preferred that above-mentioned lyophilization refers to that Jing temperature be at -30 DEG C～-75 DEG C after precooling 3-12h, then in temperature
To be dried 8-24h under -55 DEG C～-75 DEG C vacuum.
Present invention also offers above-mentioned two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound is received with two-dimentional transition-metal sulphides
Rice application of the composite granule as lithium ion battery negative, electrode material for super capacitor in energy storage device.
Beneficial effect：
(1) two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound is combined by the present invention with two-dimentional transition-metal sulphides, utilizes two
The excellent electric conductivity of dimension magnesium-yttrium-transition metal carbon (nitrogen) compound can improve the deficiency of two-dimentional transition-metal sulphides electric conductivity, real
The regulation and control of existing electric conductivity.
(2) present invention two dimension magnesium-yttrium-transition metal carbon (nitrogen) compound nanometer sheet and two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound with
The preparation process is simple of two-dimentional transition-metal sulphides composite nano-powder, safe and efficient, with low cost, two-dimentional transition group gold
Category carbon (nitrogen) compound nanometer sheet is compound uniform with two-dimentional transition-metal sulphides nanometer sheet dispersion.
(3) present invention two dimension magnesium-yttrium-transition metal carbon (nitrogen) compound can with two-dimentional transition-metal sulphides composite nano-powder
Energy storage device field is applied to as lithium ion battery negative, electrode material for super capacitor etc., excellent electricity is shown
Chemical property.Relative to two-dimentional transition-metal sulphides, its electric conductivity is substantially improved, and can promote electricity during electrochemical lithium storage
The transmission of son, effectively improves the circulation specific capacity of lithium ion battery, and flexible preferably two dimension magnesium-yttrium-transition metal carbon (nitrogen) is changed
The two-dimentional transition-metal sulphides nanometer sheet of thing nanometer sheet parcel, can reduce the lithium ion two-dimentional transition group gold that deintercalation causes repeatedly
The change in volume of category sulfide nanometer sheet, significantly improves cyclical stability.
Description of the drawings
Fig. 1 is two-dimentional transition metal carbides Ti prepared by the embodiment of the present invention 13C2The afm image of MXene nanometer sheet；
Fig. 2 is Ti prepared by the embodiment of the present invention 1,2,33C2Content is 20%, 50%, 90% two-dimentional Ti3C2With two dimension
MoS2The XRD figure of composite nano-powder；
Fig. 3 is the SEM figures of the composite nano-powder prepared by embodiment 1,4；Wherein a is that nanometer prepared by embodiment 1 is multiple
Close the SEM figures of powder body；B is the SEM figures of composite nano-powder prepared by embodiment 4.
Specific embodiment
The present invention is further described below by way of specific embodiment, it should be noted that described below is only the present invention's
Preferred embodiment, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes
And change.All any modification, equivalent substitution and improvements retouchings within the spirit and principles in the present invention, done etc., all should include
Within protection scope of the present invention.
Embodiment 1
(1) two-dimentional transition metal carbides Ti3C2The preparation of nanometer sheet suspension：By 10mL concentration for 6M dilute HCl and
The LiF of 0.662g is added in plastic bottle, is slowly added to the ternary layered carbide that 1g crosses 400 mesh sieves under magnetic stirring
Ti3AlC2Powder, and magnetic agitation 22h under 250r.p.m rotating speeds at 35 DEG C, reaction terminate after by product ethanol wash be centrifuged to
Supernatant pH value is 6.2, takes 0.1g and be added in 50mL deionized waters under precipitation room temperature after being dried, in flowing argon protection
Under, under the supersonic frequency of 40kHz, ultrasound peels off 1h, 1h is centrifuged under the rotating speed of 3500r.p.m subsequently and obtains few layer or monolayer two
Dimension transition metal carbides Ti3C2The stable suspension of nanometer sheet, suspension concentration are 0.6mg/ml.Fig. 1 is shown two dimension
Transition metal carbides Ti3C2The afm image of nanometer sheet, there it can be seen that its lamellar spacing is 1nm or so, it is typical
Two-dimension nano materials.
(2) two dimension Ti3C2With two-dimentional MoS2The preparation of composite nano-powder：By two-dimentional Ti3C2Nanometer sheet suspension is with 20%
Mass percent be added to two-dimentional MoS2In nanometer sheet suspension (0.5mg/ml, 20-500nm), ultrasonator is placed in (super
Acoustical power 100W) in ultrasound 30min.The suspension of mix homogeneously is placed in into precooling 10h under -50 DEG C of environment, after be transferred to it is cold
In lyophilizer, 15h is dried under -55 DEG C of temperature, vacuum compound uniform Ti is obtained3C2Content is 20% two-dimentional Ti3C2With
Two-dimentional MoS2Composite nano-powder.Two-dimentional Ti is found out from Fig. 2 XRD spectrums3C2With two-dimentional MoS2Include in composite nano-powder
MoS2And Ti3C2It is biphase.Two dimension MoS in composite granule is can be seen that from Fig. 3 (a) SEM images2Nanometer sheet and the two dimension of bending
Ti3C2Nanometer sheet is evenly distributed, wherein most two dimension MoS2The two-dimentional Ti that nanometer sheet is bent3C2Nanometer sheet is wrapped up.
(3) electrochemical property test：With NMP (N-Methyl pyrrolidone) as dispersant, by two-dimentional Ti3C2With two-dimentional MoS2
Composite nano-powder, acetylene black and PVDF (Kynoar) are 8 in mass ratio:1:1 ratio is uniformly mixed makes slurry
Material, is coated uniformly on Cu paper tinsels with film applicator, and cut-parts after being vacuum dried 12h at 55 DEG C are obtained 13mm electrode slices.With the gold of 0.5mm
Category lithium piece is that to electrode, Celgard3501 polypropylene porous films are barrier film, the LiPF of 1mol/L6(wherein solvent is carbonic acid to solution
Vinyl acetate (EC) and diethyl carbonate (DEC) by volume 1:1 composition) for electrolyte, button cell is assembled into, after standing 10h
Carry out electro-chemical test.Under the electric current density of 100mA/g, first discharge specific capacity is 1337mAh/g, after circulating at second
Specific discharge capacity is 936mAh/g.
Embodiment 2：
(1) two-dimentional transition metal carbides Ti3C2The preparation of nanometer sheet suspension：By 10mL concentration for 6M dilute HCl and
The LiF of 0.662g is added in plastic bottle, is slowly added to the ternary layered carbide that 1g crosses 400 mesh sieves under magnetic stirring
Ti3AlC2Powder, and magnetic agitation 12h under 300r.p.m rotating speeds at 33 DEG C, reaction terminate after by product ethanol wash be centrifuged to
Supernatant pH value is 6.3, takes 0.1g and be added in 50mL deionized waters under precipitation room temperature after being dried, in flowing argon protection
Under, under the supersonic frequency of 50kHz, ultrasound peels off 1.5h, 1.2h is centrifuged under the rotating speed of 3800r.p.m subsequently and obtains few layer or list
The two-dimentional transition metal carbides Ti of layer3C2The stable suspension of nanometer sheet, suspension concentration are 0.3mg/ml.
(2) two dimension Ti3C2With two-dimentional MoS2The preparation of composite nano-powder：By two-dimentional Ti3C2Nanometer sheet suspension is with 50%
Mass percent be added to two-dimentional MoS2In nanometer sheet suspension (0.8mg/ml, 20-500nm), ultrasonator is placed in (super
Acoustical power 90W) in ultrasound 45min.The suspension of mix homogeneously is placed in into precooling 12h under -45 DEG C of environment, after be transferred to freezing
In drying machine, the Ti that 22h is obtained mix homogeneously is dried under -50 DEG C of temperature, vacuum3C2Content is 50% two-dimentional Ti3C2With two
Dimension MoS2Composite nano-powder.
(3) electrochemical property test：Half-cell is assembled into by the method in embodiment 1 carries out electrochemical property test.
Under the electric current density of 100mA/g, first discharge specific capacity is 1175mAh/g, and after circulating at second, specific discharge capacity is
810mAh/g。
Embodiment 3：
(1) two-dimentional transition metal carbides Ti3C2The preparation of nanometer sheet suspension：By 10mL concentration for 6M dilute HCl and
The LiF of 0.662g is added in plastic bottle, is slowly added to the ternary layered carbide that 1g crosses 400 mesh sieves under magnetic stirring
Ti3AlC2Powder, and magnetic agitation 23h under 500r.p.m rotating speeds at 36 DEG C, reaction terminate after by product ethanol wash be centrifuged to
Supernatant pH value is 6.5, takes 0.1g and be added in 50mL deionized waters under precipitation room temperature after being dried, in flowing argon protection
Under, under the supersonic frequency of 80kHz, ultrasound peels off 0.8h, 0.8h is centrifuged under the rotating speed of 3200r.p.m subsequently and obtains few layer or list
The two-dimentional transition metal carbides Ti of layer3C2The stable suspension of nanometer sheet, suspension concentration are 0.9mg/ml.
(2) two dimension Ti3C2With two-dimentional MoS2The preparation of composite nano-powder：By two-dimentional Ti3C2Nanometer sheet suspension is with 90%
Mass percent be added to two-dimentional MoS2In nanometer sheet suspension (1mg/ml, 20-500nm), ultrasonator (ultrasound is placed in
Power 70W) in ultrasound 50min.The suspension of mix homogeneously is placed in into precooling 8h under -55 DEG C of environment, after to be transferred to freezing dry
In dry machine, the Ti that 10h is obtained mix homogeneously is dried under -60 DEG C of temperature, vacuum3C2Content is 90% two-dimentional Ti3C2With two dimension
MoS2Composite nano-powder.
(3) electrochemical property test：Half-cell is assembled into by the method in embodiment 1 carries out electrochemical property test.
Under the electric current density of 100mA/g, first discharge specific capacity is 601mAh/g, and after circulating at second, specific discharge capacity is 305mAh/
g。
Embodiment 4：
(1) two-dimentional transition metal carbides Ti3The preparation of CN nanometer sheet suspensions：By dilute HCl that 10mL concentration is 6M
It is added in plastic bottle with the LiF of 0.66g, is slowly added to the ternary layered carbide that 1g crosses 400 mesh sieves under magnetic stirring
Ti3AlCN powder, and magnetic agitation 6h under 400r.p.m rotating speeds at 30 DEG C, reaction terminate after by product ethanol wash be centrifuged to
Supernatant pH value is 6.5, takes 0.1g and be added in 50mL deionized waters under precipitation room temperature after being dried, in flowing argon protection
Under, under the supersonic frequency of 60kHz, ultrasound peels off 1.3h, 0.5h is centrifuged under the rotating speed of 3000r.p.m subsequently and obtains few layer or list
The two-dimentional transition metal carbides Ti of layer3The stable suspension of CN nanometer sheet, suspension concentration are 1.2mg/ml.
(2) two dimension Ti3CN and two dimension WS2The preparation of composite nano-powder：By two-dimentional Ti3CN nanometer sheet suspension is with 20%
Mass percent be added to two-dimentional WS2In nanometer sheet suspension (1.5mg/ml, 20-500nm), ultrasonator is placed in (super
Acoustical power 50W) in ultrasound 60min.The suspension of mix homogeneously is placed in into precooling 3h under -65 DEG C of environment, after be transferred to freezing
In drying machine, the Ti that 11h is obtained mix homogeneously is dried under -60 DEG C of temperature, vacuum3CN contents are 20% two-dimentional Ti3CN and two
Dimension WS2Composite nano-powder.Two dimension WS in composite granule is can be seen that from Fig. 3 (b) SEM images2Nanometer sheet and the two of bending
Dimension Ti3CN nanometer sheet is evenly distributed, wherein most two dimension WS2The two-dimentional Ti that nanometer sheet is bent3CN nanometer sheet is wrapped up.
(3) electrochemical property test：(3) electrochemical property test：Half-cell is assembled into by the method in embodiment 1 is carried out
Electrochemical property test.Under the electric current density of 100mA/g, first discharge specific capacity is 690mAh/g, is put after circulating at second
Electric specific capacity is 316mAh/g.
Claims (9)
1. two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound and two-dimentional transition-metal sulphides composite nano-powder, it is characterised in that：
The composite nano-powder is equal with two-dimentional transition-metal sulphides nanometer sheet by two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound nanometer sheet
Even dispersion is composited, wherein the quality of two-dimentional transition-metal sulphides account for the percentage composition of composite granule gross mass be 10～
99%.
2. two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound according to claim 1 is multiple with two-dimentional transition-metal sulphides nanometer
Close powder body, it is characterised in that：Described two-dimentional magnesium-yttrium-transition metal (nitrogen) compound is Ti3C2Tx、Ti3CNTx、Ti2CTx、(Ti0.5,
Nb0.5)2CTx、(V0.5,Cr0.5)3C2Tx、Ta4C3Tx、V2CTx、Nb2CTx、Nb4C3Tx、(Nb0.8,Ti0.2)4C3Tx、(Nb0.8,
Zr0.2)4C3Tx、Mo2TiC2Tx、Mo2Ti2C3Tx、Mo2CTx、Cr2TiC2Tx、Zr3C2TxOr Ti4N3Tx；Described two-dimentional transition group gold
Category sulfide is MoS2、WS2Or CoS2。
3. one kind prepares two dimension magnesium-yttrium-transition metal carbon (nitrogen) compound as claimed in claim 1 with two-dimentional transition-metal sulphides
The method of composite nano-powder, it is characterised in that comprise the following steps that：
Two-dimentional transition-metal sulphides nanometer sheet suspension is added to into two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer
In piece suspension, ultrasound makes two kinds of suspension mix homogeneously, then freeze-dried to obtain two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) change
Thing nanometer sheet and two-dimentional transition-metal sulphides composite nano-powder.
4. method as claimed in claim 3, it is characterised in that described two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer
Piece suspension is prepared by following methods, is concretely comprised the following steps：LiF is dissolved in hydrochloric acid, then by ternary layered compound
MAX powder leaching be slowly added in above-mentioned solution, at 30～40 DEG C magnetic agitation reaction, product using washing with alcohol be centrifuged to
Supernatant pH value is 6.2～6.5, and dried solid sample is added in deionized water, the ultrasound under flowing argon protection
Peel off, be then centrifuged for the stable suspension for obtaining few layer or monolayer magnesium-yttrium-transition metal carbon (nitrogen) compound MXene nanometer sheet.
5. method as claimed in claim 4, it is characterised in that the rotating speed of magnetic agitation is 250-550rpm, magnetic agitation when
Between be 6～24h；Supersonic frequency when described ultrasound is peeled off is 40-100kHz, and the time that ultrasound is peeled off is 0.5～2h；Ultrasound
After stripping, centrifugal rotational speed is 3000-4000rpm, and centrifugation time is 0.5～1.5h.
6. method as claimed in claim 3, it is characterised in that：Described two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound suspension is dense
Spend for 0.2-1.5mg/ml；Described two-dimentional transition-metal sulphides nanometer sheet suspension concentration is 0.5-2mg/ml.
7. method as claimed in claim 3, it is characterised in that：Described ultrasonic mixing refers to that in ultrasonic power be 30-150W
Power under ultrasound 0.2-1h mixed.
8. method as claimed in claim 3, it is characterised in that：Described lyophilization refers to that Jing temperature is -30 DEG C～-75 DEG C
After lower precooling 3-12h, then 8-24h is dried in the case where temperature is for -55 DEG C～-75 DEG C vacuum.
9. a kind of two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound as claimed in claim 1 and two-dimentional transition-metal sulphides nanometer
Application of the composite granule as lithium ion battery negative material in energy storage device.
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