CN111554889A - polyimide/MXene composite material and preparation and application thereof - Google Patents

polyimide/MXene composite material and preparation and application thereof Download PDF

Info

Publication number
CN111554889A
CN111554889A CN202010283992.9A CN202010283992A CN111554889A CN 111554889 A CN111554889 A CN 111554889A CN 202010283992 A CN202010283992 A CN 202010283992A CN 111554889 A CN111554889 A CN 111554889A
Authority
CN
China
Prior art keywords
mxene
polyimide
composite material
mxene composite
material according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010283992.9A
Other languages
Chinese (zh)
Inventor
黄燕山
马健
孔玥
杨圆圆
李原婷
常宾
高丽
韩生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Institute of Technology
Original Assignee
Shanghai Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Institute of Technology filed Critical Shanghai Institute of Technology
Priority to CN202010283992.9A priority Critical patent/CN111554889A/en
Publication of CN111554889A publication Critical patent/CN111554889A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • H01M4/602—Polymers
    • 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

Abstract

The invention relates to a polyimide/MXene composite material, and preparation and application thereof, wherein MXene (Ti) with a two-dimensional structure is adopted2C3) As substrate materials, pyromellitic dianhydride (PMDA) and melamine polymerize Polyimide (PI) in situ on an MXene substrate by a solvothermal method to obtain a novel polyimide MXene composite material, and the PI obtained by the method is uniformly loaded on the MXene substrate. Compared with the prior art, the polyimide composite material prepared from the carbide with the two-dimensional structure and the PMDA shows excellent electrochemical performance as a negative electrode of a sodium-ion battery, and the electrochemical performance is 100 mA.g‑1The capacity of the battery can reach 400 mAh.g under charging and discharging current‑1At 4A · g‑1The lower capacity is 200mAh g‑1The excellent rate capability of the composite material and provides good experimental data and theoretical support for the research and application of MXene and organic materials in the electrochemical field.

Description

polyimide/MXene composite material and preparation and application thereof
Technical Field
The invention belongs to the technical field of lithium ion battery electrode materials, and relates to a polyimide/MXene composite material, and preparation and application thereof.
Background
In recent decades, Lithium Ion Batteries (LIBs) have played a crucial role in the energy storage of portable electronic devices. However, the increasing demand for energy storage, particularly grid-scale storage of electric vehicles and renewable electricity, has not only raised a great deal of attention to energy density and power density.
In view of the complicated preparation process, limited resources, and the diversity of designed molecular structures, organic materials are interesting sustainable battery replacements, because of potential low cost, high safety, and diversity of designed molecular structures, and because of high theoretical capacity due to low molecular weight and multiple electron transfer capacity, but organic materials still have the disadvantage of poor conductivity, their electrochemical properties are not good, and in solving the above problems, researchers have conducted many studies, such as effectively improving the conductivity of organic materials by compounding with some highly conductive base materials (e.g., graphene, carbon fibers, two-dimensional carbide crystals).
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a polyimide/MXene composite material, and preparation and application thereof.
The PI obtained by the method is uniformly loaded on the MXene substrate, and has the advantages of simple process, mild conditions, low cost and the like. Preparation of carbide with two-dimensional structure prepared by the invention and PMDAThe prepared polyimide composite material as a negative electrode of a sodium-ion battery shows excellent electrochemical performance, and the electrochemical performance is 100 mA.g-1The capacity of the battery can reach 400 mAh.g under charging and discharging current-1At 4A · g-1The lower capacity is 200mAh g-1Excellent rate capability. The method provides good experimental data and theoretical support for the research and application of MXene and organic materials in the field of electrochemistry.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a preparation method of a polyimide/MXene composite material, which comprises the following steps:
(1) adding MXene into N-methylpyrrolidone, and performing ultrasonic mixing to obtain uniformly mixed dispersion liquid;
(2) adding pyromellitic dianhydride, stirring, adding melamine, continuously stirring, and carrying out solvothermal reaction on the obtained mixed solution;
(3) and drying a reaction product obtained by the solvothermal reaction to obtain the target product polyimide/MXene composite material.
Furthermore, in the step (1), before MXene is added into the N-methylpyrrolidone solution, water is removed through rotary evaporation.
Further, the mass ratio of MXene, pyromellitic dianhydride and melamine is 3:3: 1.
Further, in the step (2), after pyromellitic dianhydride is added, stirring for at least 1 h;
after the addition of melamine, the process is stirred for at least 1 h.
Further, in the step (2), the temperature of the solvothermal reaction is 150 ℃ to 200 ℃, and the time is 12-24 h.
Further, in the step (2), the temperature of the solvothermal reaction is 150-180 ℃.
Further, MXene is Ti3C2。
Further, in the step (3), the drying temperature is 80-100 ℃.
The second technical scheme of the invention provides a polyimide/MXene composite material, which is prepared by the preparation method.
The third technical scheme of the invention provides application of the polyimide/MXene composite material, which is used as a negative electrode material of a sodium-ion battery.
With two-dimensional material MXene (Ti)2C3) The two-dimensional composite material is prepared by adding pyromellitic dianhydride and melamine into a base material, reacting the pyromellitic dianhydride and the melamine at high temperature, and growing particles on an MXene lamellar structure in situ.
Compared with the prior art, the invention has the following advantages:
(1) the novel polyimide MXene composite material is prepared by a solvothermal method, and in the solvothermal process, the assembly of an MXene two-dimensional structure and the in-situ uniform polymerization of polyimide on the surface of an MXene substrate can be completed in one step, so that the method is simple and convenient;
(2) the invention takes the pyromellitic dianhydride and the melamine as the organic monomers to prepare the polymer material, the raw materials are designable, and the cost is low;
(3) the novel polyimide MXene composite material prepared by the method has high reversible capacity, very good cycle stability and rate capability, and wide application prospect in the field of lithium ion batteries.
Drawings
FIG. 1 is a morphology diagram of a novel polyimide MXene composite obtained in example 1;
FIG. 2 is a graph of the cycle performance of the novel polyimide MXene composite material obtained in example 1 and the pure polyimide material obtained in comparative example 1 as the negative electrode material of the sodium-ion battery;
FIG. 3 is a graph of rate capability of the novel polyimide MXene composite material obtained in example 1 and the pure polyimide material obtained in comparative example 1 as the negative electrode material of the sodium-ion battery.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, MXene used is Ti3C2The concrete sources are as follows: ti3C2According to the document DOI of 10.1002/smll.201906851.
Otherwise, unless otherwise specified, all the materials or processing techniques are conventional commercial products or conventional processing techniques in the art.
Example 1:
firstly, preparing a two-dimensional carbide crystal-based polyimide composite material:
(1-1) carrying out rotary evaporation on MXene to remove water, adding an N-methylpyrrolidone solution (NMP), and carrying out mixing ultrasonic treatment to form a uniformly mixed dispersion liquid;
(1-2) adding pyromellitic dianhydride to the dispersion, and vigorously stirring for one hour, wherein the mass ratio of 30mg of pyromellitic dianhydride to MXene is 1: 1.
(1-3) adding 10mg of melamine powder into the solution, stirring vigorously for one hour, pouring the mixed solution into a glass liner, and carrying out solvothermal treatment at about 160 ℃ for 24 hours.
Step two, preparing the novel polyimide MXene composite material:
(2-1) drying the material obtained by solvothermal treatment at high temperature to obtain the novel polyimide MXene composite material, wherein the morphology of the novel polyimide MXene composite material is shown in figure 1, the formed polyimide particles are uniformly dispersed on a two-dimensional sheet layer of MXene, and the two-dimensional material can improve the conductivity of the material and ensure that the whole material is more stable in the application process.
(2-2) assembling a sodium ion button type half cell by taking the obtained composite material as a sodium ion cell negative electrode material, mixing the composite material, carbon black (Super-P) and polyvinylidene fluoride (PVDF) according to the weight ratio of 7:2:1, and uniformly coating the mixture on pure copper foil (99.6%) by a coating method to prepare a negative electrode, wherein a pure sodium sheet is used as a counter electrode. Electrochemical test is carried out by utilizing a button type half cell, and a cycle performance diagram and a rate performance diagram of the electrochemical test areAs shown in FIGS. 2 and 3, respectively, it can be seen from FIG. 2 that the negative electrode material of the sodium-ion battery prepared by the invention has a concentration of 100mA mg-1Can always keep 400mAh mg under the current density-1Is excellent and very stable, and the capacity retention rate is also quite high. As can be seen in FIG. 3, the material also possesses good rate capability at 5000mA mg-1It can still have 200mAh mg-1Is very stable and returns to 100mA mg at current density-1The capacity can also reach 400mAh mg-1。
Comparative example 1:
compared to example 1, most of the same, no MXene was added during the experiment.
Referring to fig. 2 and 3, it can be seen that when a pure polyimide material is used as the negative electrode material of the sodium-ion battery, the cycle performance and the rate performance are significantly reduced.
In the above example 1, the temperature of the solvothermal reaction may be adjusted to any value within a limited temperature range such as 150 ℃, 200 ℃, 180 ℃ and the like as required, and the remaining process conditions may be adjusted within a limited range as required in accordance with actual operation.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. The preparation method of the polyimide/MXene composite material is characterized by comprising the following steps:
(1) adding MXene into N-methylpyrrolidone, and performing ultrasonic mixing to obtain uniformly mixed dispersion liquid;
(2) adding pyromellitic dianhydride, stirring, adding melamine, continuously stirring, and carrying out solvothermal reaction on the obtained mixed solution;
(3) and drying a reaction product obtained by the solvothermal reaction to obtain the target product polyimide/MXene composite material.
2. The method for preparing the polyimide/MXene composite material according to claim 1, wherein in the step (1), before adding the MXene into the N-methylpyrrolidone solution, the MXene is subjected to rotary evaporation to remove water.
3. The method for preparing the polyimide/MXene composite material according to claim 1, wherein the mass ratio of MXene, pyromellitic dianhydride and melamine is 3:3: 1.
4. The preparation method of the polyimide/MXene composite material according to claim 1, wherein in step (2), pyromellitic dianhydride is added and then stirred for at least 1 h;
after the addition of melamine, the process is stirred for at least 1 h.
5. The method for preparing polyimide/MXene composite material according to claim 1, wherein in step (2), the temperature of the solvothermal reaction is 150-.
6. The method for preparing polyimide/MXene composite material according to claim 1, wherein the temperature of the solvothermal reaction in step (2) is 150-180 ℃.
7. The method as claimed in claim 1, wherein the MXene is Ti3C2。
8. The method for preparing polyimide/MXene composite material according to claim 1, wherein in step (3), the drying temperature is 80-100 ℃.
9. A polyimide/MXene composite material prepared by the method of any one of claims 1 to 8.
10. The use of the polyimide/MXene composite of claim 9 as a negative electrode material for sodium ion batteries.
CN202010283992.9A 2020-04-10 2020-04-10 polyimide/MXene composite material and preparation and application thereof Pending CN111554889A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010283992.9A CN111554889A (en) 2020-04-10 2020-04-10 polyimide/MXene composite material and preparation and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010283992.9A CN111554889A (en) 2020-04-10 2020-04-10 polyimide/MXene composite material and preparation and application thereof

Publications (1)

Publication Number Publication Date
CN111554889A true CN111554889A (en) 2020-08-18

Family

ID=72004328

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010283992.9A Pending CN111554889A (en) 2020-04-10 2020-04-10 polyimide/MXene composite material and preparation and application thereof

Country Status (1)

Country Link
CN (1) CN111554889A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114725380A (en) * 2022-05-09 2022-07-08 江苏科技大学 Self-supporting polyimide @ MXene flexible film and preparation method and application thereof
CN114806347A (en) * 2022-04-18 2022-07-29 江苏科技大学 Anticorrosive paint and preparation method thereof
CN115020683A (en) * 2022-07-25 2022-09-06 哈尔滨工业大学 Preparation method of TAP/Ti3C2Tx electrode material
CN115101718A (en) * 2022-07-04 2022-09-23 湖北亿纬动力有限公司 Mxene-polyaniline composite negative electrode material and preparation method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5145943A (en) * 1990-12-17 1992-09-08 Ethyl Corporation Production of particulate amide/imide prepolymers
CN104103812A (en) * 2014-07-21 2014-10-15 国家纳米科学中心 Composite flexible electrode material as well as preparation method and application thereof
CN105771935A (en) * 2016-05-25 2016-07-20 中国地质大学（武汉） Porous polyimide/carbon nanotube composite used for adsorbing 2,4-dichlorophenol in water
CN106040191A (en) * 2016-05-23 2016-10-26 华南师范大学 Preparation method of carbon dioxide adsorption material
CN108735999A (en) * 2018-05-29 2018-11-02 上海应用技术大学 A kind of preparation method and applications of the graphene-based N doping carbon-coating composite material of three-dimensional structure
CN110183655A (en) * 2019-05-05 2019-08-30 上海应用技术大学 A kind of preparation method of the organic positive electrode of two dimension carbide crystalline base polyimides
CN110729441A (en) * 2019-10-17 2020-01-24 广东工业大学 MXene/polyimide composite battery diaphragm and preparation method and application thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5145943A (en) * 1990-12-17 1992-09-08 Ethyl Corporation Production of particulate amide/imide prepolymers
CN104103812A (en) * 2014-07-21 2014-10-15 国家纳米科学中心 Composite flexible electrode material as well as preparation method and application thereof
CN106040191A (en) * 2016-05-23 2016-10-26 华南师范大学 Preparation method of carbon dioxide adsorption material
CN105771935A (en) * 2016-05-25 2016-07-20 中国地质大学（武汉） Porous polyimide/carbon nanotube composite used for adsorbing 2,4-dichlorophenol in water
CN108735999A (en) * 2018-05-29 2018-11-02 上海应用技术大学 A kind of preparation method and applications of the graphene-based N doping carbon-coating composite material of three-dimensional structure
CN110183655A (en) * 2019-05-05 2019-08-30 上海应用技术大学 A kind of preparation method of the organic positive electrode of two dimension carbide crystalline base polyimides
CN110729441A (en) * 2019-10-17 2020-01-24 广东工业大学 MXene/polyimide composite battery diaphragm and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HAIYAN DUAN等: ""Semiconducting Crystalline Two-Dimensional Polyimide Nanosheets with Superior Sodium Storage Properties"", 《ACS NANO》 *
QINGLAN ZHAO: ""Pyromellitic dianhydride-based polyimide anodes for sodium-ion batteries"", 《ELECTROCHIMICA ACTA》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114806347A (en) * 2022-04-18 2022-07-29 江苏科技大学 Anticorrosive paint and preparation method thereof
CN114806347B (en) * 2022-04-18 2023-04-21 江苏科技大学 Anticorrosive paint and preparation method thereof
CN114725380A (en) * 2022-05-09 2022-07-08 江苏科技大学 Self-supporting polyimide @ MXene flexible film and preparation method and application thereof
CN115101718A (en) * 2022-07-04 2022-09-23 湖北亿纬动力有限公司 Mxene-polyaniline composite negative electrode material and preparation method and application thereof
CN115020683A (en) * 2022-07-25 2022-09-06 哈尔滨工业大学 Preparation method of TAP/Ti3C2Tx electrode material
CN115020683B (en) * 2022-07-25 2022-11-29 哈尔滨工业大学 Preparation method of TAP/Ti3C2Tx electrode material

Similar Documents

Publication Publication Date Title
US9437870B2 (en) Nano-silicon composite lithium ion battery anode material coated with poly (3,4-ethylenedioxythiophene) as carbon source and preparation method thereof
Sun et al. Sulfur-rich polymeric materials with semi-interpenetrating network structure as a novel lithium–sulfur cathode
CN100347887C (en) Composite graphite negative electrode material for lithium ion secondary cell and its preparation method
CN111554889A (en) polyimide/MXene composite material and preparation and application thereof
CN109326784B (en) Phosphorus doped MoS2Preparation method and application of loaded graphene nanosheet
WO2013097553A1 (en) Lithium ion battery composite electrode material immersed and coated by conducting polymer and preparation method thereof
CN105845936A (en) Preparation method of modified hard carbon negative electrode material for lithium ion battery
CN106450209B (en) A kind of modified graphene aeroge of sulfur loaded and preparation method thereof, application
CN107293710A (en) The preparation method of transition metal oxide/graphene composite material, negative electrode of lithium ion battery, lithium ion battery
CN111446448A (en) Preparation method of polyimide/graphene composite lithium ion battery cathode material based on conjugated carbonyl
CN104300129A (en) Battery, battery cathode, battery cathode material and preparation method thereof
CN102110813B (en) Graphite material at negative pole of lithium ion battery and preparation method thereof
CN113594453B (en) Sodium-ion battery negative electrode material and preparation method thereof
CN105885410A (en) Molybdenum sulfide/polypyrrole/polyaniline ternary composite material as well as preparation method and application thereof
Ma et al. Three-dimensional hierarchical walnut kernel shape conducting polymer as water soluble binder for lithium-ion battery
CN103746094A (en) C-LiFePO4/PTPAn composite material, its application and lithium battery produced by composite material thereof
CN106486670A (en) A kind of method that mesophase pitch Jiao prepares lithium cell cathode material
CN108807894B (en) Polymer precursor converted Si/C lithium ion battery cathode material and preparation method thereof
CN102339988A (en) Lithium ion battery cathode graphite material of high compacted density and preparation method thereof
CN104103808B (en) A kind of lithium ion battery lamellar stannum carbon composite and preparation method thereof
CN113782718A (en) High-voltage lithium ion battery material, lithium ion battery and preparation method thereof
CN111048753B (en) Iron oxide doped phosphorus atom composite material and preparation method and application thereof
CN110556537B (en) Method for improving electrochemical performance of anion-embedded electrode material
CN112520732A (en) Silicon-carbon composite negative electrode material and preparation method thereof
CN109627441B (en) Tubular covalent organic framework polyimide, preparation method thereof and battery application

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200818