CN114975993A - MXene self-supporting film electrode with high mechanical property and excellent electrochemical property prepared by utilizing nano cellulose containing lignin - Google Patents

MXene self-supporting film electrode with high mechanical property and excellent electrochemical property prepared by utilizing nano cellulose containing lignin Download PDF

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CN114975993A
CN114975993A CN202210627071.9A CN202210627071A CN114975993A CN 114975993 A CN114975993 A CN 114975993A CN 202210627071 A CN202210627071 A CN 202210627071A CN 114975993 A CN114975993 A CN 114975993A
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mxene
film electrode
lcnf
thin film
mechanical property
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陈卫民
李昭
周晓燕
刘朝政
杨凯
张道通
杨培
陈敏智
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Nanjing Forestry University
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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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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

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Abstract

The invention provides a method for preparing an MXene self-supporting film electrode with high mechanical property and excellent electrochemical property by utilizing nano cellulose containing lignin, belonging to the field of MXene film material modification. The method takes MXene as a raw material, takes lignin-containing nanocellulose (LCNF) obtained by treating waste biomass by a microwave heating method as a modifier, mixes the suspension of the MXene and the LCNF in a certain proportion, ultrasonically disperses the mixture, and then prepares the LCNF modified MXene film electrode by vacuum filtration. The method remarkably improves the mechanical property of the MXene thin film electrode, simultaneously considers the electrochemical property of the MXene thin film electrode, effectively solves the problem of low electrolyte ion transmission efficiency caused by self-stacking of the MXene nano sheets, does not cause remarkable reduction of the conductivity of the thin film electrode, and has the characteristics of simple preparation process, green and environment-friendly preparation process and the like. The LCNF modified MXene film electrode has good mechanical property, high conductivity and excellent electrochemical property, and can be efficiently applied to energy storage devices such as flexible batteries, super capacitors and the like.

Description

MXene self-supporting film electrode with high mechanical property and excellent electrochemical property prepared by utilizing nano cellulose containing lignin
Technical Field
The invention relates to a method for preparing an MXene thin film electrode with high mechanical property and excellent electrochemical property by utilizing nano cellulose containing lignin, belonging to the field of MXene thin film material modification.
Background
MXene is a two-dimensional transition metal carbon/nitride with ultrahigh conductivity, good hydrophilicity, high electrochemical activity and rich surface functional groups, and the general formula of MXene is M n+1 X n T x (N ═ 1, 2, 3) where M is a transition metal (Ti, Nb, Mo, etc.), X is a C or N element, and T is a surface terminal group (-F, -O, -Cl, etc.). The MXene film can be prepared by utilizing rich functional groups on the surface of MXene through a simple vacuum-assisted suction filtration mode, and can be used as a self-supporting film electrode to be applied to the field of electrochemical energy storage. Compared with the traditional electrode, the MXene thin film electrode does not need to be compounded with a conductive agent, a binder and a current collector, and has the characteristics of high active substance occupation ratio, light weight, good flexibility and the like. However, the bonding between MXene nanosheets dominated by hydrogen bonding and van der Waals forces is weak, resulting in poor mechanical properties of the prepared thin film electrode. In addition, hydrogen bonds and van der waals forces between adjacent MXene nanosheets inevitably cause a self-stacking phenomenon, which not only results in a substantial reduction of MXene thin film electrode electrochemically active sites, but also severely hinders rapid diffusion of electrolyte ions in the thin film electrode. Therefore, the mechanical property and the electrochemical property of the thin film electrode still have a larger promotion space.
Currently, Cellulose Nanofibers (CNF) are widely used as a renewable reinforcement material for thin film electrodes. The MXene suspension and the CNF suspension are uniformly mixed and subjected to vacuum filtration to prepare the CNF modified MXene thin film electrode. On one hand, the nature of the high degree of polymerization and high crystallinity of CNF makes it have the characteristics of high strength and high modulus, and can be used as an excellent support material. On the other hand, rich oxygen-containing functional groups on the surface of the CNF can be used as active sites to form firm combination with the MXene nanosheets through hydrogen bonds, so that the mechanical properties of the MXene thin film electrode are remarkably improved. In addition, CNF has a fine nanostructure and a large aspect ratio (transverse dimension between tens of nanometers and length up to several micrometers), and can be used as an intercalator to be embedded between MXene nanosheets, thereby widening electrolyte ion diffusion channels by increasing interlayer spacing and providing more ion accessible active sites. Moreover, due to the one-dimensional structure of the CNF, the CNF and the MXene nanosheet are in a line-to-plane contact mode, and the effect of electrode conductivity reduction caused by the insulation property of the CNF can be effectively weakened. However, the addition of CNF decreases the proportion of the active material MXene in the electrode, and thus inevitably sacrifices the electrochemical performance of the thin film electrode. In addition, the conventional CNF preparation methods (such as TEMPO oxidation) are generally complicated and costly, which limits their large-scale application. Therefore, the development of the modified reinforcing material which is low in cost, improves the mechanical property of the thin film electrode and simultaneously gives consideration to the electrochemical property of the thin film electrode has practical significance for obtaining the MXene thin film electrode with good mechanical property and excellent electrochemical property, and is beneficial to widening the application of the electrode in flexible electronic devices.
The method takes MXene as a raw material, takes nano cellulose (LCNF) containing lignin as a modifier, mixes the suspension of the MXene and the nano cellulose (LCNF) according to a certain proportion, and prepares the LCNF modified MXene film electrode by ultrasonic dispersion and vacuum filtration. The addition of LCNF can greatly improve the mechanical property of the thin film electrode, and simultaneously effectively increase the interlayer spacing between MXene nano sheets through the intercalation effect without causing the obvious reduction of the conductivity of the thin film electrode. Compared with CNF adopted by the traditional method, the existence of lignin in LCNF can effectively counteract the hydrogen bond effect between cellulose and inhibit the entanglement of cellulose chains, thereby increasing the accessibility of hydroxyl, constructing a richer pore structure for the film electrode, increasing the diffusion channel of electrolyte ions and greatly shortening the longitudinal diffusion distance of the electrolyte ions in the film electrode. In addition, lignin in the LCNF is beneficial to storing and exchanging electrons and protons in the oxidation-reduction process, and the high specific capacitance and excellent rate characteristic of the film electrode are ensured. Moreover, compared with the preparation method of CNF (such as TEMPO oxidation method and the like), LCNF does not need a fine lignin removal step, can be quickly prepared by treating waste biomass raw materials (sawdust, bagasse and the like) through microwave heating, is simpler in preparation process, is green and environment-friendly, and is suitable for large-scale production. Therefore, by adopting the low-cost modified reinforced material, the mechanical property of the MXene thin film electrode can be greatly improved on the premise of not sacrificing the electrochemical property, and reliable technical support is provided for developing the MXene thin film electrode with good mechanical property and excellent electrochemical property.
Disclosure of Invention
The invention aims to use MXene as a raw material and LCNF as a modifier. The LCNF modified MXene membrane electrode is prepared by vacuum filtration, so that the excellent electrochemical performance of the membrane electrode is ensured, and the mechanical performance of the membrane electrode is improved. The introduction of LCNF can construct a large number of electrolyte ion diffusion channels in the MXene thin film electrode, greatly improve the transmission efficiency of electrolyte ions in the thin film electrode, improve the multiplying power characteristic under the condition of not reducing the specific capacitance of the MXene thin film electrode, and finally obtain the LCNF modified MXene thin film electrode with high mechanical property and excellent electrochemical property.
The technical solution of the invention is as follows: the preparation of MXene self-supporting thin film electrode with high mechanical property and excellent electrochemical property by using LCNF is completed according to the following steps:
preparation of LCNF
The method comprises the steps of treating waste biomass raw materials by using a choline chloride and lactic acid system eutectic solvent (DES) through microwaves, and then obtaining LCNF suspension through ultrasonic dispersion.
The preparation method of the LCNF comprises the following specific steps: the waste biomass raw material is first pretreated, soaked in hot water at 70 ℃ for 2 hours to remove impurities, and then dried at 60 ℃ for 24 hours. Choline chloride and lactic acid were mixed at 80 ℃ in a ratio of 1: 10, and stirred for 2 hours to obtain DES. 1g of the dried material and 10g of DES were mixed and placed in a microwave reaction vessel and subjected to microwave treatment at 130 ℃ for 30 minutes. Subsequently, the obtained sample was washed in 200mL of ethanol with constant stirring for 2 hours, and the LCNF suspension was obtained by vacuum filtration, low-temperature drying (60 ℃, 24h) and ultrasonic dispersion (960W, 30min) in this order.
Preparation of LCNF modified MXene film electrode
Mixing MXene suspension obtained by wet etching and LCNF suspension according to a certain proportion, carrying out ultrasonic treatment for 10min to ensure that the MXene suspension and the LCNF suspension are uniformly dispersed, carrying out vacuum filtration, and drying in a vacuum oven for 12 hours to obtain the LCNF modified MXene film electrode.
Compared with the common CNF modification MXene thin film electrode method, the method has the advantages that: (1) the preparation process of LCNF is simple and efficient: the LCNF used by the invention is prepared by microwave treatment of waste biomass raw materials for 30 minutes, has short preparation time and simple method, and does not need complicated steps of removing lignin. (2) The mechanical strength of the film electrode is improved, and the excellent electrochemical performance of the film electrode is ensured by utilizing the advantages of lignin.
Detailed Description
Example 1
(1) Preparation of LCNF: bagasse was first pretreated, soaked in hot water at 70 ℃ for 2 hours to remove impurities, and then dried at 60 ℃ for 24 hours. Choline chloride and lactic acid were mixed at 80 ℃ in a ratio of 1: 10, and stirred for 2 hours to obtain DES. 1g of the dried material and 10g of DES were mixed and placed in a microwave reaction vessel and subjected to microwave treatment at 130 ℃ for 30 minutes. Subsequently, the obtained sample was washed in 200mL of ethanol for 2 hours with constant stirring, and LCNF suspension was obtained by vacuum filtration, low-temperature drying (60 ℃, 24 hours) and ultrasonic dispersion (960W, 30min) in this order.
(2) Preparing an LCNF modified MXene film electrode: taking 15mL of Ti obtained by wet etching 3 C 2 T x (an MXene) suspension according to m (Ti) 3 C 2 T x ) Adding certain amount of LCNF suspension in the ratio of m to 1, ultrasonic treating for 10min to disperse homogeneously, vacuum filtering, and drying in vacuum oven for 12 hr to obtain LCNF modified Ti 3 C 2 T x And a thin film electrode. LCNF modified Ti 3 C 2 T x The tensile strength, specific capacitance and rate characteristics of the film electrode are shown in table 1.
Example 2
(1) The same procedure (1) as in example 1 was followed to prepare an LCNF suspension starting from sawdust.
(2) Taking 15mL of Ti obtained by wet etching 3 C 2 T x The suspension being in accordance with m (Ti) 3 C 2 T x ) Adding certain amount of LCNF suspension in the ratio of m to 3 to 10, ultrasonic treating for 10min to disperse homogeneously, vacuum filtering, and drying in vacuum oven for 12 hr to obtain LCNF modified Ti 3 C 2 T x And a thin film electrode. LCNF modified Ti 3 C 2 T x The tensile strength, specific capacitance and rate characteristics of the film electrode are shown in table 1.
Example 3
(1) LCNF suspension was prepared by the same procedure (1) as in example 1 using corn stover as a starting material.
(2) Taking 15mL of Ti obtained by wet etching 3 C 2 T x The suspension being in accordance with m (Ti) 3 C 2 T x ) Adding certain amount of LCNF suspension in the ratio of m to 5 to 10, ultrasonic treating for 10min to disperse homogeneously, vacuum filtering, and drying in vacuum oven for 12 hr to obtain LCNF modified Ti 3 C 2 T x And a thin film electrode. LCNF modified Ti 3 C 2 T x The tensile strength, specific capacitance and rate characteristics of the film electrode are shown in table 1.
Comparative example 1:
taking 15mL of Ti obtained by wet etching 3 C 2 T x Vacuum filtering the suspension, and drying in a vacuum oven for 12 hours to obtain Ti 3 C 2 T x And a thin film electrode. Ti 3 C 2 T x The tensile strength, specific capacitance and rate characteristics of the film electrode are shown in table 1.
Comparative example 2:
taking 15mL of Ti obtained by wet etching 3 C 2 T x Suspension according to m (Ti) 3 C 2 T x ) Adding certain amount of the suspension of CNF prepared by TEMPO method into the mixture in the ratio of m to CNF of 10 to 1, performing ultrasonic treatment for 10min to disperse the mixture uniformly, performing vacuum filtration, and drying in a vacuum oven for 12 hours to obtain CNFModified Ti 3 C 2 T x And a thin film electrode. CNF modified Ti 3 C 2 T x The tensile strength, specific capacitance and rate characteristics of the film electrode are shown in table 1.
TABLE 1 comparison of the properties of the various thin-film electrodes
Figure BSA0000274428350000041
Note:
firstly, a tensile strength result is obtained by testing a universal mechanical testing machine;
② the mass specific capacitance result is obtained by the constant current charge-discharge test method of the electrochemical workstation (CHI660D), the tested current density is 0.5A/g, and the voltage window is-0.6 eV to 0.2 eV. The mass specific capacitance refers to the capacitance per unit mass of electroactive substance at a current density of 0.5A/g;
③ the multiplying power characteristic result is obtained by a constant current charging and discharging test method of an electrochemical workstation (CHI660D), the current density of all the tests is 0.5A/g, 1A/g, 1.5A/g, 2A/g, 5A/g and 10A/g, and the voltage window is-0.6 eV to 0.2 eV. The rate characteristic is the capacity retention rate of the thin film electrode when the current density is from 0.5Aag to 10A/g.

Claims (4)

1. The invention relates to a method for preparing an MXene self-supporting film electrode with high mechanical property and excellent electrochemical property by utilizing nano cellulose containing lignin, which is characterized by comprising the following steps of: the MXene thin film electrode with high mechanical property and excellent electrochemical property is prepared by the following steps:
the method comprises the following steps: preparation of lignin-containing nanocellulose (LCNF): the waste biomass raw material is first pretreated, soaked in hot water at 70 ℃ for 2 hours to remove impurities, and then dried at 60 ℃ for 24 hours. Choline chloride and lactic acid were mixed at 80 ℃ in a ratio of 1: 10, and stirred for 2 hours to obtain a eutectic solvent (DES). 1g of the dried material and 10g of DES were mixed and placed in a microwave reaction vessel and subjected to microwave treatment at 130 ℃ for 30 minutes. Subsequently, the obtained sample was washed in 200mL of ethanol for 2 hours with constant stirring, and LCNF suspension was obtained by vacuum filtration, low-temperature drying (60 ℃, 24 hours) and ultrasonic dispersion (960W, 30min) in this order.
Step two: preparing an LCNF modified MXene film electrode: taking 15mL of MXene suspension obtained by wet etching according to m (Ti) 3 C 2 T x ) Adding certain amount of LCNF suspension in the ratio of m to 1, ultrasonic treating for 10min to disperse homogeneously, vacuum filtering, and drying in a vacuum oven for 12 hr to obtain LCNF modified MXene composite film electrode.
2. The method for preparing the MXene self-supporting thin film electrode with high mechanical property and excellent electrochemical property by using the lignocellulose containing the lignin according to claim 1, wherein the method comprises the following steps: the waste biomass raw material in the step one comprises all biomass raw materials containing lignin and cellulose, such as bagasse, sawdust and the like.
3. The method for preparing the MXene self-supporting thin film electrode with high mechanical property and excellent electrochemical property by using the lignocellulose containing the lignin according to claim 1, wherein the method comprises the following steps: MXene in the second step comprises Ti 3 C 2 T x 、Nb 2 C、V 2 C、Mo 2 C and all other mxenes that enable the preparation of self-supporting thin film electrodes by vacuum filtration.
4. The method for preparing the MXene self-supporting thin film electrode with high mechanical property and excellent electrochemical property by using the lignocellulose containing the lignin according to claim 1, wherein the method comprises the following steps: and the addition amount of the LCNF in the step two is 10-60% of the weight of MXene.
CN202210627071.9A 2022-06-02 2022-06-02 MXene self-supporting film electrode with high mechanical property and excellent electrochemical property prepared by utilizing nano cellulose containing lignin Pending CN114975993A (en)

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CN115497753A (en) * 2022-09-14 2022-12-20 江苏科技大学 Preparation method of polyaniline/bamboo fiber/MXene composite material, product and application thereof
CN117976853A (en) * 2023-12-29 2024-05-03 云南中晟新材料有限责任公司 Lithium ion battery negative electrode material, and preparation method and application thereof

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CN115497753B (en) * 2022-09-14 2023-11-21 江苏科技大学 Preparation method of polyaniline/bamboo fiber/MXene composite material, and product and application thereof
CN117976853A (en) * 2023-12-29 2024-05-03 云南中晟新材料有限责任公司 Lithium ion battery negative electrode material, and preparation method and application thereof
CN117976853B (en) * 2023-12-29 2024-08-16 云南中晟新材料有限责任公司 Lithium ion battery negative electrode material, and preparation method and application thereof

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Application publication date: 20220830