CN114934327A - Preparation method of millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte - Google Patents

Preparation method of millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte Download PDF

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Publication number
CN114934327A
CN114934327A CN202210530484.5A CN202210530484A CN114934327A CN 114934327 A CN114934327 A CN 114934327A CN 202210530484 A CN202210530484 A CN 202210530484A CN 114934327 A CN114934327 A CN 114934327A
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millimeter
fibrous
electrode
diameter
aerogel
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赖浩然
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Yangtze River Delta Research Institute of UESTC Huzhou
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Yangtze River Delta Research Institute of UESTC Huzhou
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention relates to the technical field of aerogel electrode manufacturing, in particular to a preparation method of a millimeter-diameter fibrous aerogel electrode fully soaked by gel electrolyte, which comprises the following steps: s1, performing electrostatic spinning on the prepared electrostatic spinning solution of the fibrous aerogel electrode with the millimeter diameter by using electrostatic spinning equipment at normal temperature and with the relative humidity controlled below 30; s2, collecting the fiber aerogel with millimeter diameter by a rotator, and controlling the bulkiness and the loading capacity of the fiber aerogel by controlling the speed and the time of the rotating collection; s3, the millimeter diameter fibrous aerogel can be directly used as fibrous electrode material or can be prepared into fibrous electrode by soaking nano-level active substance dispersion liquid and freeze drying, the state of the fiber in an electric field is regulated by regulating the conductivity of the fiber, the millimeter diameter fibrous aerogel electrode is prepared by one-step method, and the conductivity of the fiber is determined by the kind of macromolecule in the spinning solution and the kind and concentration of the conductive additive.

Description

Preparation method of millimeter-diameter fibrous aerogel electrode fully soaked by gel electrolyte
Technical Field
The invention relates to the technical field of aerogel electrode manufacturing, in particular to a preparation method of a millimeter-diameter fibrous aerogel electrode fully soaked by gel electrolyte.
Background
Aerogel is a solid form, the least dense solid in the world. The density was 3 kg per cubic meter. A common aerogel is the silica aerogel, which was first made by Kistler, the american scientist, in 1931 by betting on his friends. There are various types of aerogels, including silicon-based, carbon-based, sulfur-based, metal oxide-based, metal-based, and the like. aerogel is a combination word where aeroo is an adjective, meaning flying, and gel is obviously a gel. Literally means a gel that can fly. Any gel can be called aerogel as long as it can be dried and the internal solvent is removed, and the shape of the gel can be basically kept unchanged, and the product has high porosity and low density.
The wet spinning method and the fiber template method are wide and effective methods for preparing the porous fibrous electrode, however, the fiber electrode prepared by the method has lower unit length capacity and higher bulk density, and is not beneficial to the infiltration of gel electrolyte, so that the assembled gel all-solid fibrous energy storage device has lower unit length capacity and poorer rate behavior. The invention utilizes the electrostatic spinning process, regulates the conductivity of the fiber, regulates the state of the fiber in an electric field, and prepares the fibrous aerogel electrode with millimeter diameter by a one-step method, the fibrous electrode has the characteristics of adjustable components, high unit length load and controllable filling power, the excellent hydrophilic characteristic and the capillary action of a porous structure are favorable for the infiltration of gel electrolyte, and the assembled gel all-solid fibrous energy storage device has higher unit length capacity and higher multiplying power behavior.
Disclosure of Invention
Technical problem to be solved
The method solves the problems that the fiber electrodes prepared by a wet spinning method and a fiber template method have low unit length capacity and high stacking density, and are not beneficial to the infiltration of gel electrolyte, so that the assembled gel all-solid-state fibrous energy storage device has low unit length capacity and poor multiplying power behavior, and provides a method for preparing a millimeter-diameter fibrous aerogel electrode which is fully infiltrated by gel electrolyte.
(II) technical scheme
A preparation method of a millimeter-diameter fibrous aerogel electrode fully infiltrated with gel electrolyte comprises the following steps:
s1, performing electrostatic spinning on the prepared electrostatic spinning solution of the fibrous aerogel electrode with the millimeter diameter by using electrostatic spinning equipment at normal temperature and with the relative humidity controlled below 30;
s2, collecting the fibrous aerogel with millimeter diameter by a rotator, and controlling the bulkiness and the loading capacity of the fibrous aerogel by controlling the speed and the time of the rotary collection;
s3, the fibrous aerogel with millimeter diameter can be directly used as fibrous electrode material or can be prepared into fibrous electrode by soaking nano-level active substance dispersion liquid and freeze drying.
The preparation method of the millimeter-diameter fibrous aerogel electrode electrospinning solution comprises the following steps:
s1, selecting proper high polymer and conductive additive;
s2, controlling the concentration of the conductive additive; dispersing a conductive additive into a solvent, and then dispersing a polymer to prepare a spinning solution; the conductivity of the fiber is adjusted within the range of 10-14-106S m-1 by adjusting the type and concentration of the conductive additive, the type and concentration of the conductive additive determine the conductivity of the fiber, finally determine the state of the fiber in an electrostatic field, and the concentration of the conductive additive is properly adjusted by judging whether a fibrous aerogel electrode can be collected;
s3, preparing a fiber electrode; the electrostatic spinning fibers are collected through a rotating line of a synchronous motor, the obtained fibrous aerogel can be directly used as an electrode, a nano active substance dispersion liquid can also be soaked, and then the fibrous aerogel electrode with the millimeter diameter and fully soaked by gel electrolyte is prepared through a freeze drying process.
In a preferred embodiment, the electrospinning solution is classified into an aqueous system (including alcohol) and an organic solvent system according to the solvent.
Preferably, the polymer in the water system includes polyvinyl alcohol (PVA), polyethylene oxide (PEO), and cellulose.
As a preferred technical solution, the conductive additive may include alcohol, amine, and carboxylic acid small molecules with low volatility and high conductivity, or may be a water-soluble conductive polymer.
As a preferable embodiment, the polymer of the organic solvent system includes Polyurethane (PU), Polyacrylonitrile (PAN), polylactic acid (PLA), and Polyimide (PI).
As a preferred technical solution, the conductive additive is an electrical additive including alcohols, amines and carboxylic acid small molecules with low volatility and high conductivity, and may also be conductive polymers Polyaniline (PANI), polypyrrole (PPy), polythiophene.
According to a preferable technical scheme, the active substance dispersion liquid comprises MXenes, carbon nanotubes and a conductive polymer aqueous solution.
(III) advantageous effects
The invention has the beneficial effects that:
1. the conductivity of the fiber is determined by the types of macromolecules in the spinning solution and the types and the concentrations of conductive additives.
2. Compared with the fiber electrode prepared by the traditional preparation method, the fibrous aerogel electrode prepared by the method with millimeter diameter has higher unit length capacity and is an excellent candidate material for preparing a wearable fiber energy storage device.
3. The fibrous aerogel electrode with the millimeter diameter prepared by the method has extremely high porosity, can be completely soaked by gel electrolyte to enable the gel electrolyte to show electrochemical behavior similar to that of liquid electrolyte in solid electrolyte, and can be used for a high-capacity and high-rate all-solid fibrous energy storage device.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the preparation of a millimeter diameter fibrous aerogel electrode by modulating fiber conductivity;
FIG. 2 is a water based dope PEDOT, PSS and PEO prepared fibrous aerogel electrode of millimeter diameter;
FIG. 3 is a lower fiber electrode prepared by impregnating carbon nanotubes with a millimeter diameter PAN aerogel containing glycerol as a conductive additive;
Detailed Description
The preparation method of the millimeter-diameter fibrous aerogel electrode fully infiltrated with the gel electrolyte of the present invention is further described with reference to the accompanying drawings, and the present invention is further detailed with reference to the following embodiments:
a preparation method of a millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte comprises the following steps:
s1, performing electrostatic spinning on the prepared electrostatic spinning solution of the fibrous aerogel electrode with the millimeter diameter by using electrostatic spinning equipment at normal temperature and with the relative humidity controlled below 30;
s2, collecting the fibrous aerogel with millimeter diameter by a rotator, and controlling the bulkiness and the loading capacity of the fibrous aerogel by controlling the speed and the time of the rotary collection;
s3, the fibrous aerogel with millimeter diameter can be directly used as fibrous electrode material, or can be prepared into fibrous electrode by soaking nanometer active substance dispersion liquid and freeze drying, wherein the active substance dispersion liquid comprises MXenes, carbon nanotubes and conductive polymer aqueous solution (such as PEDOT: PSS aqueous solution).
The preparation method of the millimeter-diameter fibrous aerogel electrode electrospinning solution comprises the following steps:
s1, selecting proper high polymer and conductive additive;
s2, controlling the concentration of the conductive additive; dispersing a conductive additive into a solvent, and then dispersing a polymer to prepare a spinning solution; adjusting the conductivity of the fibers within the range of 10-14-106S m-1 by adjusting the type and concentration of the conductive additive, wherein the type and concentration of the conductive additive determine the conductivity of the fibers, finally determine the state of the fibers in an electrostatic field, and the concentration of the conductive additive is properly adjusted by whether the fibrous aerogel electrodes can be collected or not;
s3, preparing a fiber electrode; the electrostatic spinning fibers are collected through a rotating line of a synchronous motor, the obtained fibrous aerogel can be directly used as an electrode, a nano active substance dispersion liquid can also be soaked, and then the fibrous aerogel electrode with the millimeter diameter and fully soaked by gel electrolyte is prepared through a freeze drying process.
Further, the electrospinning solution is classified into a water system (including alcohol) and an organic solvent system according to the difference of the solvent.
Further, the polymer in the water system includes polyvinyl alcohol (PVA), polyethylene oxide (PEO), cellulose, and the like.
Further, the conductive additive may include low-volatility and high-conductivity alcohols, amines, and carboxylic acid small molecules such as glycerol, or water-soluble conductive polymers such as PEDOT: PSS.
Further, the organic solvent-based polymer includes Polyurethane (PU), Polyacrylonitrile (PAN), polylactic acid (PLA), Polyimide (PI), and the like.
Further, the conductive additive is an electrical additive including alcohols, amines and small carboxylic acid molecules with low volatility and high conductivity, such as glycerol, and may also be conductive polymers Polyaniline (PANI), polypyrrole (PPy), polythiophene, and the like.
The above embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the spirit and scope of the present invention, and various modifications and improvements made to the technical solutions of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall within the protection scope of the present invention, and the technical contents of the present invention as claimed are all described in the claims.

Claims (8)

1. A preparation method of a millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte is characterized by comprising the following steps of: the method comprises the following steps:
s1, performing electrostatic spinning on the electrostatic spinning solution of the prepared fibrous aerogel electrode with the millimeter diameter by using electrostatic spinning equipment at normal temperature and with the relative humidity controlled below 30;
s2, collecting the fibrous aerogel with millimeter diameter by a rotator, and controlling the bulkiness and the loading capacity of the fibrous aerogel by controlling the speed and the time of the rotary collection;
s3, the fibrous aerogel with millimeter diameter can be directly used as fibrous electrode material, or can be impregnated with nanoscale active substance dispersion liquid and freeze-dried to prepare fibrous electrode.
2. The method of preparing a gel electrolyte fully-infiltrated millimeter-diameter fibrous aerogel electrode of claim 1, comprising: the preparation method of the millimeter-diameter fibrous aerogel electrode electrostatic spinning solution comprises the following steps:
s1, selecting proper polymers and conductive additives;
s2, controlling the concentration of the conductive additive; dispersing a conductive additive into a solvent, and then dispersing a polymer to prepare a spinning solution; adjusting the conductivity of the fibers within the range of 10-14-106Sm-1 by adjusting the type and concentration of the conductive additive, determining the conductivity of the fibers by the type and concentration of the conductive additive, finally determining the state of the fibers in an electrostatic field, and properly adjusting the concentration of the conductive additive by whether a fibrous aerogel electrode can be collected or not;
s3, preparing a fiber electrode; the electrostatic spinning fibers are collected through a rotating line of a synchronous motor, the obtained fibrous aerogel can be directly used as an electrode, a nano active substance dispersion liquid can also be soaked, and then the fibrous aerogel electrode with the millimeter diameter and fully soaked by gel electrolyte is prepared through a freeze drying process.
3. The method of preparing a gel electrolyte fully-infiltrated millimeter-diameter fibrous aerogel electrode of claim 2, comprising: the electrospinning solution is classified into a water system (including alcohol) and an organic solvent system according to the difference of the solvents.
4. The method of preparing a gel electrolyte fully infiltrated millimeter-diameter fibrous aerogel electrode of claim 3, wherein: the polymer in the water system comprises polyvinyl alcohol (PVA), polyethylene oxide (PEO) and cellulose.
5. The method of preparing a gel electrolyte fully infiltrated millimeter-diameter fibrous aerogel electrode of claim 4, wherein: the conductive additive can comprise alcohols, amines and carboxylic acid micromolecules with low volatility and higher conductivity, and can also be water-soluble conductive polymers.
6. The method of preparing a gel electrolyte fully infiltrated millimeter-diameter fibrous aerogel electrode of claim 2, wherein: the organic solvent-based polymer includes Polyurethane (PU), Polyacrylonitrile (PAN), polylactic acid (PLA), and Polyimide (PI).
7. The method of preparing a gel electrolyte fully infiltrated millimeter-diameter fibrous aerogel electrode of claim 6, comprising: the conductive additive is an electric additive which comprises alcohols, amines and carboxylic acid micromolecules with low volatility and higher conductivity, and can also be conductive polymers such as Polyaniline (PANI), polypyrrole (PPy) and polythiophene.
8. The method of preparing a gel electrolyte fully infiltrated millimeter-diameter fibrous aerogel electrode of claim 1, wherein: the active substance dispersion liquid comprises MXenes, carbon nano tubes and a conductive polymer aqueous solution.
CN202210530484.5A 2022-05-16 2022-05-16 Preparation method of millimeter-diameter fibrous aerogel electrode fully infiltrated by gel electrolyte Pending CN114934327A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101147156B1 (en) * 2010-12-30 2012-05-25 한국에너지기술연구원 Preparation method of carbon aerogel sheet
CN105820372A (en) * 2016-03-30 2016-08-03 青岛大学 Conductive aerogel and preparation method thereof
CN111768895A (en) * 2020-07-06 2020-10-13 东华大学 Air-permeable transparent flexible fiber-based surface electrode and preparation method thereof
CN113972368A (en) * 2021-10-25 2022-01-25 东华大学 High-stability fibrous lithium ion battery anode lithium supplement material and preparation and application thereof
CN114409954A (en) * 2021-12-08 2022-04-29 西安理工大学 Preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101147156B1 (en) * 2010-12-30 2012-05-25 한국에너지기술연구원 Preparation method of carbon aerogel sheet
CN105820372A (en) * 2016-03-30 2016-08-03 青岛大学 Conductive aerogel and preparation method thereof
CN111768895A (en) * 2020-07-06 2020-10-13 东华大学 Air-permeable transparent flexible fiber-based surface electrode and preparation method thereof
CN113972368A (en) * 2021-10-25 2022-01-25 东华大学 High-stability fibrous lithium ion battery anode lithium supplement material and preparation and application thereof
CN114409954A (en) * 2021-12-08 2022-04-29 西安理工大学 Preparation method of graphene/ceramic nanofiber/polyvinyl alcohol hybrid aerogel

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HAORAN LAI等: "Macroscale amphiphilic aerogel fibers made from nonwoven nanofibers for large active mass loading", JOURNAL OF POWER SOURCES, vol. 474, pages 1 - 7 *

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