CN106328890A - Carbon-pillared MXene composite material and application thereof - Google Patents

Carbon-pillared MXene composite material and application thereof Download PDF

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CN106328890A
CN106328890A CN201610733990.9A CN201610733990A CN106328890A CN 106328890 A CN106328890 A CN 106328890A CN 201610733990 A CN201610733990 A CN 201610733990A CN 106328890 A CN106328890 A CN 106328890A
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carbon
mxene
pillared
solution
mxene composite
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CN106328890B (en
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罗剑敏
袁华栋
陶新永
夏阳
梁初
黄辉
张俊
甘永平
张文魁
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Zhejiang University of Technology ZJUT
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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
    • H01M4/366—Composites as layered products
    • 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
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • 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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • 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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • Y02E60/10—Energy storage using batteries
    • 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 provides a carbon-pillared MXene composite material and an application thereof. The carbon-pillared MXene composite material comprises a two-dimensional layered MXene carrier and a carbon nanosheet loaded between MXene layers; and a preparation method comprises the following steps of (1) processing a taken MAX raw material in an HF solution to obtain an MXene material; (2) soaking the MXene material obtained in the step (1) into a solution of which the cationic carbon precursor content is 0.005-20g/mL, stirring at 30-100 DEG C for 0.5-72 hours and centrifuging, washing and drying a product to obtain a pre-pillared MXene material; and (3) heating the pre-pillared MXene material in a protective atmosphere to 300-800 DEG C at the rate of 2-10 DEG C/min and carrying out insulating calcination treatment for 0.5-4 hours to obtain the carbon-pillared MXene material. The invention provides an application of the carbon-pillared MXene composite material as an electrode material of a lithium-ion battery or a super capacitor. The capacity of the electrode material can be greatly improved and the cycle performance is good, so that the operating requirements in the field of high energy and high power are met.

Description

A kind of carbon pillared MXene composite and application thereof
(1) technical field
The present invention relates to a kind of carbon pillared MXene composite and as lithium ion battery or electrode of super capacitor material The application of material.
(2) background technology
MXene material is a class New Two Dimensional stratiform transition metal C/N compound-material.This two dimension MXene material has The features such as excellent electric conductivity, chemical stability.Up to the present prepare MXene material to be mainly by HF solution etches MAX Raw material and obtain.Up to now, MXene has been applied to multiple field, such as: lithium ion battery, ultracapacitor, light The fields such as catalysis, hydrogen storage.Although MXene material has the electric conductivity of excellence, excellent chemical stability, but it is at lithium ion Battery is applied capacity relatively low (50-200mAh/g), hence it is evident that less than the capacity (372mAh/g) of commercialization graphite material.This is very MXene application prospect in lithium ion battery is limited in big degree.Although it addition, MXene material is led at ultracapacitor Territory application has high capacity (～360F/cm3), but its potential interlayer energy storing space is not fully used.If The interlayer energy storing space of MXene material is exploited further, and it is as lithium ion battery material, the capacity of ultracapacitor It is expected to promote further.
(3) summary of the invention
The goal of the invention of the present invention is to provide a kind of carbon pillared MXene composite and as lithium ion battery or super The application of electrode material in capacitor.
Technical scheme is specifically described below.
The invention provides a kind of carbon pillared MXene composite, including two-dimensional layer MXene carrier and be supported on The carbon nanosheet of MXene interlayer；Its preparation method comprises the steps:
(1) take MAX raw material, process in HF solution and obtain MXene material；
(2) the MXene material that step (1) obtains being immersed in cationic carbon matrix precursor content is 0.005-20g/mL's In solution, at 30-100 DEG C, stir 0.5～72h, be then centrifuged for, wash, be dried to obtain pre-pillared MXene material；
(3) by pre-pillared MXene material under protective atmosphere with the ramp of 2～10 DEG C/min to 300-800 DEG C, protect Temperature calcination processing 0.5～4h, obtains carbon pillared MXene material.
In step of the present invention (1), described MXene material is Ti3C2、Ti2C、Ti2N、Nb2C、Nb4C3、Ta2C、Ta4C3、 V2C、V3C2、Cr2C、Cr3C2、(Ti0.5Nb0.5)2C or Ti3(C0.5N0.5)2.Those skilled in the art can be according to required preparation MXene material, selects suitable MAX raw material, and the method reported by document prepares MXene material.Preferably, step (1) concrete operations are: weigh MAX raw material, add in the HF solution that mass fraction is 10%～50%, wherein HF solution Inventory is calculated as 3～50mL/g with the raw-material quality of MAX, under room temperature soak 2～56h, be then centrifuged for, be washed to pH=6～ 7, MXene powder it is dried to obtain.
In step of the present invention (2), described cationic carbon matrix precursor can be cationic natural polymer, as bright Glue, chitosan, chitin etc.；Can also be cationic polyelectrolyte, such as diallyl dimethyl ammoniumchloride, polydiene diformazan Ammonium chloride, polymine, polyvinylamine etc.；Preferably its purity is more than 90%.The solvent of described solution can be water, second The common solvents, preferably its purity such as alcohol, methanol, acetone are more than 90%.Anions in solution type carbon matrix precursor content is preferably 0.05-15g/mL, more preferably 0.05～10g/mL.The inventory of the solution containing cationic carbon matrix precursor is with MXene material The quality of material is calculated as 5～1000mL/g.
In step of the present invention (2), stirring, preferably at 30-80 DEG C, is carried out at more preferably 40-80 DEG C, and mixing time is preferably 1-48h, more preferably 3～36h.
In step of the present invention (3), the group of one or both arbitrary proportions during protective atmosphere is argon, nitrogen during calcining Closing, preferably its purity is more than 90%.Calcining heat is preferably 400～700 DEG C, and calcination time is preferably 1～4 hour.
The present invention provides a kind of carbon pillared MXene composite as lithium ion battery or electrode material for super capacitor Application.
Compared with prior art, the beneficial effects are mainly as follows: preparation method of the present invention is simple, utilize The electronegative characteristic of MXene material surfaces externally and internally after acid etch, allows the cationic carbon matrix precursor of positively charged pass through electrostatic Adsorption inserts MXene material interlayer, effectively struts MXene material interlayer；Afterwards through a step carbonization, obtain carbon pillared MXene material.This material is as lithium ion battery, super capacitor material, and in charge and discharge process, carbon nanosheet itself provides Capacity, and it can effectively strut MXene interlayer, gives the energy storing space that material is bigger, it is provided that more capacity, significantly MXene is as lithium ion battery, the capacity of ultracapacitor in lifting, and stable cycle performance, thus meet and use requirement.
(4) accompanying drawing explanation
Fig. 1 is the embodiment 1 pillared Ti of carbon3C2XRD comparison diagram before and after MXene.According to Bragg equation, the angle in XRD peak θ is the least for degree, and just explanation interlamellar spacing d is the biggest, so from comparison diagram, after carbon is pillared, interlamellar spacing becomes big, just illustrates that carbon is received Rice sheet enters into Ti3C2MXene interlayer.
Fig. 2 is the embodiment 1 pillared Ti of carbon3C2The SEM figure of MXene.
Fig. 3 is the pillared Ti of the carbon prepared by embodiment 13C2The cycle performance of lithium ion battery figure of MXene.
Fig. 4 is the pillared Ti of the carbon prepared by embodiment 13C2The ultracapacitor cycle performance figure of MXene.
(5) detailed description of the invention
With specific embodiment, technical scheme is described further below, but protection scope of the present invention does not limits In this.
Embodiment 1
Take 3g Ti3AlC2Powder (MAX), in beaker, adds the HF solution that 10ml mass fraction is 40%, stirring, room temperature Lower etching 16h.Then by the Ti after etching3C2MXene powder is centrifuged out, and spends Ion Cleaning to PH=6～7, at 80 DEG C Convection oven in dry 12h.0.1g Ti after drying3C2MXene powder, at 40mL, containing 0.05g/mL gelatin, (Aladdin tries Agent, chemical pure) aqueous solution in 50 DEG C of stirring 5h, centrifugal, spend Ion Cleaning, dry, after in nitrogen atmosphere with 10 DEG C/ It is incubated 2h at the heating rate of min 500 DEG C and obtains the pillared Ti of carbon3C2MXene material.
With the pillared Ti of carbon obtained by embodiment 13C2MXene material powder makes electrode as follows.
The pillared Ti of carbon is weighed respectively with the mass ratio of 80:10:103C2MXene material: super-P:PVDF, after grinding uniformly Making electrode, metal lithium sheet is to electrode, and electrolyte is 1mol/L LiPF6/ EC:DMC (1:1), polypropylene microporous film be every Film, is assembled into simulation lithium ion battery.Fig. 3 be respective battery under 100mA/g electric current density, the voltage range of 0.01 3.0V Interior cycle performance curve, shows that surveyed battery has higher capacity, good cycle performance under 100mA/g electric current density With high coulombic efficiency, it can be seen that the pillared Ti of carbon prepared by embodiment 13C2MXene material is under 100mA/g electric current density Circulate the discharge capacity after 50 times close to 520mAh/g (Fig. 3), compared to the Ti of the most pillared process3C2The capacity of MXene (～ 120mAh/g), capacity has had and has significantly promoted, and cycle performance is excellent.
The pillared Ti of carbon is weighed respectively with the mass ratio of 85:10:53C2MXene material: super-P:PTFE, drips the most different Propanol, after grinding uniformly, rolls film, tabletting, engraved film, makes circular membrane, and the electrode material membrane made is dry in vacuum drying oven Dry a whole night, weigh film quality, use the pressure of 14Mpa to be pressed in by thin film on the stainless (steel) wire made in advance afterwards and be used for surveying The chemical property of examination material.In three-electrode system, with 1mol/L H2SO4Solution is electrolyte solution, with the electrode made Material is working electrode, and saturated calomel electrode is reference electrode, and platinized platinum is auxiliary electrode, and electrochemical workstation is circulated volt-ampere Curve, constant current charge-discharge are tested.Test voltage scope is-0.8-0.1V.Fig. 4 be respective battery under 5A/g electric current density ,- Cycle performance curve in the voltage range of 0.8-0.1V, the ultracapacitor that surface is surveyed circulates the discharge capacity after 5000 times Close to 285F/g (Fig. 4), compared to the Ti of the most pillared process3C2The capacity (～100F/g) of MXene, capacity has had and has significantly carried Rising, cycle performance is excellent.
Embodiment 2
Take 2.5g Ti2AlC powder, in beaker, adds the HF solution that 30ml mass fraction is 40%, and stirring, under room temperature Etching 8h.Then etching powder is centrifuged out Ti2C MXene powder, spends Ion Cleaning to PH=6～7, the air blast of 80 DEG C Baking oven dries 12h.Ti after 0.2g is dried2C MXene powder, in 50mL diallyl dimethyl chlorination Han 0.5g/mL In the aqueous solution (Aladdin reagent, Mw 100000-200000,20wt.% aqueous solution, CP) of ammonium, 60 DEG C of stirring 4h, centrifugal, uses Deionization clean, dry, after in argon gas atmosphere with at the heating rate 500 DEG C of 5 DEG C/min be incubated 2h obtain the pillared Ti of carbon2C MXene material.With the obtained pillared Ti of carbon2Electrode made as described in Example 1 by C MXene material, be assembled into mould lithium from Sub-battery, circulates the discharge capacity after 50 times close to 485mAh/g, compared to the most pillared process under 100mA/g electric current density Ti2The capacity (～135mAh/g) of CMXene, capacity has had and has significantly promoted, and cycle performance is good.
Embodiment 3
Take 2.8g Nb2AlC powder, in beaker, adds the HF solution that 20ml mass fraction is 35%, and stirring, under room temperature Etching 18h.Then etching powder is centrifuged out Nb2C MXene powder, spends Ion Cleaning to PH=6～7, at the drum of 80 DEG C Wind baking oven dries 8h.Nb after 0.15g is dried2C MXene powder, 60mL contain 2g/mL chitosan (Aladdin reagent, Middle viscosity, 200-400mPa.s) solution in 60 DEG C of stirring 8h, centrifugal, spend Ion Cleaning, dry, after in argon gas atmosphere The pillared Nb of carbon is obtained with insulation 2h at the heating rate 600 DEG C of 3 DEG C/min2C MXene material.With the obtained pillared Nb of carbon2C Electrode made as described in Example 1 by MXene material, is assembled into simulation ultracapacitor, circulates under 10A/g electric current density Discharge capacity after 3000 times is close to 275F/g, compared to the Nb of the most pillared process2The capacity (～95F/g) of C MXene, capacity Having had and significantly promoted, cycle performance is good.
Embodiment 4
Take 4g V2AlC powder, in plastic beaker, adds the HF solution that 40ml mass fraction is 20%, soaks under room temperature 16h.Then the powder after soaking is centrifuged out, and is washed with deionized water to PH=6～7, dries in the convection oven of 80 DEG C 20h.V after 0.25g is dried2C MXene powder, 50mL containing 1g/mL polymine (Aladdin reagent, Mw 10000, 99%) in ethanol solution, 40 DEG C of stirring 6h, centrifugal, spends Ion Cleaning, dries, after in argon gas atmosphere with 6 DEG C/min's It is incubated 4h at heating rate 700 DEG C and obtains the pillared V of carbon2C MXene material.With the obtained pillared V of carbon2C MXene material is by real The method executing example 1 makes electrode, is assembled into mould lithium ion battery, circulates the electric discharge after 50 times and hold under 100mA/g electric current density Amount is close to 520mAh/g, compared to the V of the most pillared process2Capacity (～105mAh/g) cycle performance of CMXene is good.

Claims (10)

1. a carbon pillared MXene composite, its preparation method comprises the steps:
(1) take MAX raw material, process in HF solution and obtain MXene material；
(2) the MXene material that step (1) obtains being immersed in cationic carbon matrix precursor content is the solution of 0.005-20g/mL In, at 30-100 DEG C, stir 0.5～72h, be then centrifuged for, wash, be dried to obtain pre-pillared MXene material；
(3) by pre-pillared MXene material under protective atmosphere with the ramp of 2～10 DEG C/min to 300-800 DEG C, insulation is forged Burning processes 0.5～4h, obtains carbon pillared MXene material.
2. carbon pillared MXene composite as claimed in claim 1, it is characterised in that: in step (1), MXene material is Ti3C2、Ti2C、Ti2N、Nb2C、Nb4C3、Ta2C、Ta4C3、V2C、V3C2、Cr2C、Cr3C2、(Ti0.5Nb0.5)2C or Ti3 (C0.5N0.5)2。
3. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: in step (2), cationic carbon Presoma is cationic natural polymer or cationic polyelectrolyte.
4. carbon pillared MXene composite as claimed in claim 3, it is characterised in that: described cationic carbon matrix precursor Selected from one of following: gelatin, chitosan, chitin, diallyl dimethyl ammoniumchloride, polydiallyldimethyl ammonium chloride, poly- Aziridine, polyvinylamine.
5. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: in step (2), described solution Solvent is water, ethanol, methanol or acetone.
6. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: in step (2), solution middle-jiao yang, function of the spleen and stomach from Subtype carbon matrix precursor content is 0.05-15g/mL, and the inventory of the solution containing cationic carbon matrix precursor is with MXene material Quality is calculated as 5～1000mL/g.
7. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: in step (3), protect during calcining Atmosphere is the combination of one or both arbitrary proportions in argon, nitrogen.
8. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: in step (3), calcining heat is 400-700 DEG C, calcination time is 1～4 hour.
9. carbon pillared MXene composite as claimed in claim 1 or 2, it is characterised in that: described preparation method is by step (1)～(3) composition.
10. carbon pillared MXene composite as claimed in claim 1 or 2 is as lithium ion battery or electrode of super capacitor The application of material.
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CN107777688A (en) * 2017-10-13 2018-03-09 合肥工业大学 A kind of preparation method of laminar Mxene sheet materials
CN108470633A (en) * 2018-04-10 2018-08-31 中国科学院合肥物质科学研究院 A kind of electrode material for super capacitor of the excellent cyclical stability of height ratio capacity
CN108975462A (en) * 2018-08-23 2018-12-11 中南大学 A kind of ferrite modification MXene laminar gas diffusion electrode and the preparation method and application thereof
CN109279592A (en) * 2018-09-13 2019-01-29 郑州轻工业学院 It is a kind of to accumulate porous nitrogen-doped carbon nanometer sheet electrode material and preparation method thereof
CN109449402A (en) * 2018-10-29 2019-03-08 北京科技大学 A kind of nano carbon microsphere supports preparation and its application method of MXene composite material
CN109535476A (en) * 2018-11-27 2019-03-29 北京化工大学 A kind of Mxene@chitosan@polyurethane foam three-dimensional composite material and its preparation method and application
CN109851313A (en) * 2019-01-22 2019-06-07 华南理工大学 A kind of highly sensitive, the wide line sensing scope compressible compound carbon aerogels and its preparation and application
CN110311112A (en) * 2019-07-02 2019-10-08 东南大学 A kind of HPCSs@d-Ti for lithium-sulphur cell positive electrode3C2Composite material and its application
CN113140410A (en) * 2020-01-17 2021-07-20 西交利物浦大学 Nitrogen-doped carbon nanosheet/MXene composite nanomaterial, and preparation method and application thereof
CN113817195A (en) * 2021-11-02 2021-12-21 浙江优可丽新材料有限公司 Chitin @ MXene @ Ni chain thin film material and preparation method and application thereof
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CN107777688B (en) * 2017-10-13 2020-01-07 合肥工业大学 Preparation method of sheet-like Mxene sheet material
CN107777688A (en) * 2017-10-13 2018-03-09 合肥工业大学 A kind of preparation method of laminar Mxene sheet materials
CN108470633A (en) * 2018-04-10 2018-08-31 中国科学院合肥物质科学研究院 A kind of electrode material for super capacitor of the excellent cyclical stability of height ratio capacity
CN108975462A (en) * 2018-08-23 2018-12-11 中南大学 A kind of ferrite modification MXene laminar gas diffusion electrode and the preparation method and application thereof
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