CN109449402A - A kind of nano carbon microsphere supports preparation and its application method of MXene composite material - Google Patents
A kind of nano carbon microsphere supports preparation and its application method of MXene composite material Download PDFInfo
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- CN109449402A CN109449402A CN201811269713.2A CN201811269713A CN109449402A CN 109449402 A CN109449402 A CN 109449402A CN 201811269713 A CN201811269713 A CN 201811269713A CN 109449402 A CN109449402 A CN 109449402A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- C01B32/15—Nano-sized carbon materials
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of preparation of nano carbon microsphere support MXene composite material and its application methods.The present invention obtains two-dimentional carbide MXene using the mixed solution of sodium fluoride and hydrochloric acid etching MAX phase ceramics powder；Nano carbon microsphere is synthesized using hydro-thermal method.Mixed solution is made by electrostatic interaction in MXene, cationic surfactant and nano carbon microsphere, stirs, be centrifuged at room temperature, is dry to get nano carbon microsphere support MXene composite material powder.Preparation method is simple, safe, at low cost.The present invention is using nano carbon microsphere support MXene composite material as magnesium cell anode material, the interlamellar spacing of MXene can not only be expanded, the more surface-active sites of exposure, and increase ion transmission channel, solve the problems, such as that MXene lamella stacks reunion in cyclic process again simultaneously, and then the storage magnesium capacity of MXene is significantly improved, there is good cyclical stability, be a kind of excellent magnesium cell anode material.
Description
Technical field
The invention belongs to new energy field of storage, and in particular to a kind of system of nano carbon microsphere support MXene composite material
The standby and its application method in magnesium cell.
Background technique
New system one of of the Mg secondary cell as the following substitution conventional lithium ion battery most with prospects, have than
The advantages that capacity is high, energy density is big, resourceful, safety is good and pollution-free, but its research is still in the primary stage.With lithium
Ion is compared, and it is reversible in positive electrode that the higher charge density of magnesium divalent ion and stronger solvation limit it
Deintercalation, poor circulation low so as to cause the storage magnesium capacity of material.Therefore, finding suitable positive electrode is Magnesium ion battery
One of research critical issue.
So far, mainly there is Chevrel phase M applied to the positive electrode of Mg secondary cellxMo6T8(M is metal, and T is
Sulphur or selenium), manganous silicate magnesium, transition metal oxide and sulfide etc. it is several.Wherein, most study is Chevrel phase
MxMo6T8(D.Levi,E.Lancry,H.Gizbar,et al.Kinetic and thermodynamic studies of
Mg2+and Li+ion insert into the Mo6S8chevrel phase.Journal of Electrochemical
Society, 2004,151 (7): A1044-1051), Reversible Cycle is had excellent performance, but is prepared and required height, and condition is harsh, is not easy
Operation.Mesoporous manganous silicate magnesium (Mg1.03Mn0.97SiO4) it is used as magnesium cell anode material (Y.N.Nuli, J.Yang, Y.S.Li, et
al.Mesoporous magnesium manganese silicate as cathode materials for
Rechargeable magnesium batteries, Chemical Communications, 2010,46:3794), store up magnesium
Capacity is in 0.2C up to 301.4mAh/g (1C=314mA/g), but its cycle performance is poor (< 20 times).It is with titanium dioxide
The transition metal oxide of representative is safety and environmental protection, easy to operate as magnesium cell anode material, at 0.2C (1C=168mA/g)
Under current density, 90 circulation volumes are maintained at~145mAh/g, but capacity is decayed rapidly under slightly larger current density, exploitation value
It is worth not high.Liu Yong freely waits (Y.C.Liu, L-Z.Fan, L.F.Jiao.Graphene intercalated in graphene-
like MoS2:A promising cathode for rechargeable Mg batteries,Journal of Power
Sources, 2017,340:104-110) by MoS2It is compound as magnesium cell anode material, easy to operate, initial appearance with graphene
Amount is high, safety is good, but cycle life is shorter (< 50 times).Therefore, study it is a kind of it is safe and environment-friendly, capacity is high, cycle performance
Good magnesium cell anode material is extremely important and is highly desirable.
MXene is a kind of New Two Dimensional stratiform transition metal carbide or carbonitride nanometer with class graphene-structured
Material is general to etch away the element A in presoma MAX phase by chemical liquid phase reaction and obtain (M=transition metal element, A=the
IIIA/IVA element, X=carbon or nitrogen).Due to the diversity of MXene type and excellent physics and chemical characteristic, closely
Extensive research is caused over year, has especially shown many application potentials in energy storage and conversion art.It is so far
Only, MXene family includes Ti3C2、Ti2C、Mo2C、(Ti0.5Nb0.5)2C、Ti3CN、Sc2C、Ta4C3、Nb2C、V2C and Nb4C3Deng,
It is widely used in many technical fields such as supercapacitor, lithium ion battery, sodium-ion battery, sensor.Yan Xingbin class
Topic group is utilized respectively cationic surfactant intercalation MXene (M.Xu, S.Lei, J.Qi, et al.Opening Magnesium
Storage Capability of Two-Dimensional MXene by Intercalation of Cationic
Surfactant, ACS nano, 2018,12 (4): 3733-3740) and preparation MoS2/ MXene composite material (M.Xu,
N.Bai,H.X.Li,et al.Synthesis of MXene-supported layered MoS2with enhanced
electrochemical performance for Mg batteries,Chinese Chemical Letters,2018,29
(8): 1313-1316) it is applied in Magnesium ion battery as positive electrode, however there is no quilts for the potential energy storing space of MXene
Full utilization, so that the storage magnesium specific capacity of resulting materials is lower (96mAh/g, 50mA/g), cycle life is shorter (< 50 times).Such as
The interlamellar spacing further expansion of MXene material can be stored up magnesium performance and be expected to be improved significantly by fruit.Prior art research
Work is mainly based upon two-dimensional sheet MXene growth in situ TiO2Nanocomposite [ZL201710324865.7], with APC+
LiCl is the performance in terms of the magnesium cell of electrolyte, and few researchs make nano carbon microsphere support MXene using APC as electrolyte
For the storage magnesium performance of magnesium cell anode material.
Positive electrode using nano carbon microsphere support MXene as magnesium cell, it is not only possible to open MXene to greatest extent
Interlamellar spacing, the more surface-active sites of exposure, and ion transmission channel is increased, realize Mg2+Effective deintercalation, simultaneously
Solve the problems, such as that MXene lamella stacks reunion in cyclic process.As anode of magnesium ion battery material, significantly promoted
The storage magnesium capacity of MXene, shows excellent cyclical stability.
Summary of the invention
The object of the present invention is to provide a kind of preparation of nano carbon microsphere support MXene composite material and its in magnesium cell
Application method.
Based on above-mentioned purpose, this invention takes following technical solutions:
A kind of preparation method of nano carbon microsphere support MXene composite material, includes the following steps:
(1) MAX phase ceramics powder the preparation of MXene powder: is immersed in the mixing of certain density sodium fluoride and hydrochloric acid
Reacted in solution, 90 DEG C~110 DEG C of reaction temperature, the reaction time 48~96 hours, then will precipitating successively with deionized water and
Ethyl alcohol eccentric cleaning to filtrate is neutrality, and obtained solid powder is two-dimentional carbide MXene after drying.The MAX phase powder
Quality and sodium fluoride/hydrochloric acid mixed solution volume ratio be 1g:20mL；The concentration of the sodium fluoride and hydrochloric acid mixed solution is
6mol/L。
(2) preparation of nano carbon microsphere: a certain amount of glucose and deionized water are mixed according to the ratio of 0.9g:10mL,
Dissolution.It is then transferred in reaction kettle, 4~6h is reacted at 160 DEG C~180 DEG C, is centrifuged after being cooled to room temperature, it is dry, i.e.,
Nano carbon microsphere can be obtained.
(3) preparation of nano carbon microsphere support MXene composite material: by two-dimentional carbide MXene, cationic surfactant
Mixed solution is made with the nano carbon microsphere of certain mass.At room temperature, above-mentioned mixed solution is stirred, acquired solution is centrifuged, is dry,
MXene composite material powder is supported up to nano carbon microsphere.
Further, the two-dimentional carbide is Ti3C2、Ti2C or V2C.Nano carbon microsphere content is 5wt%~10wt%.
Further, cationic surfactant is cetyl trimethylammonium bromide, bromination dimethyl benzyl dodecane
Base ammonium, N, the one of which in N dimethyl lauryl amine, octadecyltrimethylammonium chloride, and added cationic surface is living
Property agent content be 0.1wt%.
Using the application method of the support MXene composite material of nano carbon microsphere obtained by above-mentioned preparation method.On it is characterized in that,
It states gained nano carbon microsphere support MXene composite material to apply in magnesium cell as electrode material, when assembling magnesium cell, according to two
Secondary magnesium cell anode material: acetylene black (super-P): N- first is added in the mixing of binder (PVDF, 5wt%)=8:1:1 ratio
Base pyrrolidones (NMP) is solvent, and grinding is slurried, uniform coating (1~2mg/cm2) after electrode is made, be dried in vacuo at 80 DEG C
12h.Using AZ31Mg piece as cathode, the phenyl-magnesium-chloride of 0.4mol/L and the tetrahydrofuran solution of aluminium chloride make electrolyte (i.e. APC
Electrolyte), magnesium cell is assembled in glove box.
The preparation method of nano carbon microsphere support MXene composite material of the present invention, is synthesized by the method for electrostatic self-assembled.It receives
The load capacity of rice carbon ball is adjustable, realizes nano carbon microsphere in the surface two-dimentional carbide MXene and the uniform load of interlayer.
A kind of preparation method of nano carbon microsphere support MXene composite material of the present invention, has an advantage that reaction in room temperature
Under the conditions of carry out, process is simple, it is at low cost, be not necessarily to special process equipment, convenience and high-efficiency；The hetero nano structure of formation,
MXene interlamellar spacing, the more surface-active sites of exposure can not only be expanded to greatest extent, and it is logical to increase ion transmission
Road solves the problems, such as that MXene stacks reunion in cyclic process.As the positive electrode of magnesium cell, the circulation of material is enhanced
Stability improves storage magnesium capacity, is a kind of excellent magnesium cell anode material.
Detailed description of the invention
Fig. 1 is that nano carbon microsphere made from embodiment 1 supports MXene Ti3C2The scanning electron microscopic picture of composite material；
Fig. 2 is that nano carbon microsphere made from embodiment 1 supports MXene Ti3C2Cycle performance of the composite material in magnesium cell
Test result.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but protection model of the invention
It encloses and is not limited thereto.
Embodiment 1:
Nano carbon microsphere supports MXene Ti3C2The preparation of composite material, includes the following steps:
It (1) is the 1g Ti of 500 mesh by partial size3AlC2Powder is immersed in the mixing of the sodium fluoride and hydrochloric acid of 20mL 6mol/L
It in solution, stirs for 24 hours, is cooled to room temperature at 60 DEG C, be subsequently poured into centrifuge tube and be centrifuged repeatedly for several times using deionized water, directly
Solution into centrifuge tube is in neutrality, and upper solution is precipitated, and will be centrifuged the sample that leaves of bottom of the tube and be put in a vacuum drying oven 80
DEG C dry 12h, obtains two dimensional crystal compound MXene Ti3C2, it is clear that from Fig. 1 by sodium fluoride and hydrochloric acid
Mixed solution etching after, present sheet, lamellar structure is obvious, thickness about 50nm.
(2) a certain amount of glucose and deionized water are mixed according to the ratio of 0.9g:10mL, dissolution.It is then transferred to
In reaction kettle, 4~6h is reacted at 160 DEG C~180 DEG C, is centrifuged after being cooled to room temperature, it is dry.Nano carbon microsphere can be obtained,
Gained carbon ball size is uniform, is conducive to being uniformly distributed in MXene interlayer.
(3) the MXene Ti of 1g is weighed3C2The nano carbon microsphere of 20mL surfactant containing 0.1wt% (CTAB) is added in powder
It in solution, stirs, be centrifuged at room temperature, is dry.Gained powder is nano carbon microsphere support MXene Ti3C2Composite material.Fig. 1
For its stereoscan photograph, it can be seen that nano carbon microsphere enters MXene Ti3C2Interlayer further increases its interlamellar spacing, plays
Supporting role, this is conducive to Mg2+Insertion and abjection.
The nano carbon microsphere obtained by embodiment 1 supports MXene Ti3C2Electrode is made in composite material as follows:
Nano carbon microsphere support MXene Ti is weighed respectively with the mass ratio of 8:1:13C2: acetylene black (super-P): binder
(PVDF, 5wt%), with N-Methyl pyrrolidone (NMP) for solvent, grinding is slurried, uniform coating (1~2mg/cm2) after be made
Electrode is dried in vacuo 12h at 80 DEG C.Using AZ31Mg piece as cathode, the phenyl-magnesium-chloride of 0.4mol/L and the tetrahydro furan of aluminium chloride
Solution of muttering makees electrolyte, and magnesium cell is assembled in glove box.
Fig. 2 is that nano carbon microsphere supports MXene Ti3C2Current density be 50mA/g, test voltage range be 0.01~
Cyclic curve when 2.0V.As seen from the figure, after 400 circulations, the storage magnesium specific capacity of sample is maintained at~138mAh/g, library
Logical sequence efficiency is also stabilized in 90% or more.Compared to the MXene Ti handled without nano carbon microsphere3C2Storage magnesium capacity (~3.5mAh/
G), storage magnesium capacity, which has, is significantly promoted.Illustrate that the entrance of nano carbon microsphere expands the interlamellar spacing of MXene, increases its surface
Activated adoption site, and then improve Mg2+Memory capacity.Also indicate that nano carbon microsphere supports MXene Ti simultaneously3C2As
The positive electrode of magnesium cell has excellent cyclicity and structural stability.
Embodiment 2:
Nano carbon microsphere supports MXene Ti2The preparation and its magnesium cell performance of C composite, include the following steps:
It is the 1g Ti of 500 mesh by partial size2AlC powder is immersed in the sodium fluoride of 20mL 6mol/L and the mixed solution of hydrochloric acid
In, 40 DEG C of stirring 48h pour into eccentric cleaning to solution in centrifuge tube and are in neutrality after being cooled to room temperature, upper solution is precipitated, will be from
The sample that heart bottom of the tube leaves puts 80 DEG C of dry 12h in a vacuum drying oven, obtains two dimensional crystal compound Ti2C powder.Nanometer
Preparing for carbon ball is as described in example 1 above.With obtained Ti2Nano carbon microsphere support is made in C powder according to the method for embodiment 1
MXene Ti2C composite, and electrode is made, it is assembled into Magnesium ion battery, is recycled 400 times under the current density of 50mA/g
Discharge capacity afterwards is stablized close to 123mAh/g, coulombic efficiency 90% or more.Compared to the MXene handled without nano carbon microsphere
Ti2C capacity (~5.2mAh/g), nano carbon microsphere support MXene Ti2C composite has excellent cyclical stability.
Embodiment 3:
Nano carbon microsphere supports MXene V2The preparation and its magnesium cell performance of C composite, include the following steps:
It is the 1g V of 500 mesh by partial size2AlC powder is immersed in the sodium fluoride of 20mL 6mol/L and the mixed solution of hydrochloric acid
In, 90 DEG C of stirring 72h pour into eccentric cleaning to solution in centrifuge tube and are in neutrality after being cooled to room temperature, upper solution is precipitated, will be from
The sample that heart bottom of the tube leaves puts 80 DEG C of dry 12h in a vacuum drying oven, obtains two dimensional crystal compound V2C powder.Nanometer
Preparing for carbon ball is as described in example 1 above.With obtained V2Nano carbon microsphere support is made in C powder according to the method for embodiment 1
MXene V2C composite, and electrode is made, it is assembled into Magnesium ion battery, after recycling 200 times under the current density of 50mA/g
Discharge capacity be maintained at~50mAh/g, coulombic efficiency is also stabilized in 96% or more.Compared to pure MXene V2C capacity (~
4mAh/g), nano carbon microsphere supports MXene V2C composite has good cycle performance.
Think finally, it is noted that the explanation of above example is merely used to help understand method and its core of the invention
Think.The substantial technological context being not intended to limit the invention, those skilled in the art can be on this basis to this hairs
It is bright to make various improvement to optimize this programme.Without departing from the principle of the present invention, any modification and modification etc. of progress
It should be included in the range of the claims in the present invention.
Claims (5)
1. a kind of preparation method of nano carbon microsphere support MXene composite material, it is characterised in that preparation step is as follows:
(1) MAX phase ceramics powder the preparation of MXene powder: is immersed in the mixed solution of certain density sodium fluoride and hydrochloric acid
Then precipitating is successively used deionized water and ethyl alcohol by middle reaction, 90 DEG C~110 DEG C of reaction temperature, the reaction time 48~96 hours
Eccentric cleaning, obtained solid powder is two-dimentional carbide MXene after drying；The quality and sodium fluoride/salt of the MAX phase powder
The volume ratio of sour mixed solution is 1g:20mL；The concentration of the mixed solution of the sodium fluoride and hydrochloric acid is 6mol/L；
(2) preparation of nano carbon microsphere: a certain amount of glucose and deionized water are mixed according to the ratio of 0.9g:10mL, dissolution；
It is then transferred in reaction kettle, 4~6h is reacted at 160 DEG C~180 DEG C, is centrifuged after being cooled to room temperature, it is dry, it can be obtained
Nano carbon microsphere；
(3) preparation of nano carbon microsphere support MXene composite material: by two-dimentional carbide MXene, cationic surfactant and one
Mixed solution is made in the nano carbon microsphere for determining quality；It stirs a few hours, is finally centrifuged acquired solution at room temperature, it is dry, it can obtain
Nano carbon microsphere supports MXene composite material.
2. the preparation method of nano carbon microsphere support MXene composite material according to claim 1, which is characterized in that described two
Dimension carbide MXene is Ti3C2、Ti2C or V2C。
3. the preparation method of nano carbon microsphere support MXene composite material according to claim 1, which is characterized in that nano-sized carbon
It is 5wt%~10wt% that ball, which supports the content of nano carbon microsphere in MXene compound,.
4. the preparation method of nano carbon microsphere support MXene composite material according to claim 1, which is characterized in that cation
Surfactant is cetyl trimethylammonium bromide, bromination dimethyl benzyl dodecyl ammonium, N, N dimethyl dodecyl
One of which in amine, octadecyltrimethylammonium chloride, and the content of added cationic surfactant is 0.1wt%.
5. the application method of nano carbon microsphere support MXene composite material according to claim 1, which is characterized in that described to receive
Rice carbon ball support MXene composite material is applied in Magnesium ion battery as electrode material, when assembling magnesium cell, according to secondary magnesium
Cell positive material: acetylene black (super-P): N- methyl is added in binder (PVDF)=8:1:1 ratio mixing of 5wt%
Pyrrolidones is solvent, and grinding is slurried, and electrode is made after uniform coating, and 12h, 1~2mg/ of coating thickness are dried in vacuo at 80 DEG C
cm2；Using AZ31Mg piece as cathode, the phenyl-magnesium-chloride of 0.4mol/L and the tetrahydrofuran solution of aluminium chloride make electrolyte, in hand
Magnesium cell is assembled in casing.
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