A preparation method of an aerogel-like carbon-based composite fibrous electrode prepared by a normal pressure drying method
By controlling the solvent evaporation rate through atmospheric pressure drying, and utilizing additives such as alcohols and carboxylic acids, as well as glycerol-modified polyacrylonitrile aerogel templates, aerogel-like carbon-based composite fibrous electrodes were prepared. This solved the problem of high energy consumption in freeze drying and achieved low-cost and high-efficiency preparation.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- YANGTZE DELTA REGION INST OF UNIV OF ELECTRONICS SCI & TECH OF CHINE (HUZHOU)
- Filing Date
- 2022-11-28
- Publication Date
- 2026-05-29
AI Technical Summary
Existing fibrous aerogel electrodes require a freeze-drying process to prepare, which is energy-intensive and has strict requirements for continuous production.
An aerogel-like carbon-based composite fibrous electrode was prepared by using an atmospheric pressure drying method and controlling the solvent evaporation rate, and by using volatile alcohols, carboxylic acids or amines and glycerol-modified polyacrylonitrile aerogel as a template.
It achieves similar electrochemical performance and flexibility to the freeze-drying method, with a simple process, low cost, and is suitable for widespread application.
Smart Images

Figure CN115798945B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of aerogel-like electrode fabrication technology, and more particularly to a method for preparing aerogel-like carbon-based composite fibrous electrode by atmospheric pressure drying. Background Technology
[0002] Carbon-based composite fibrous aerogels, with their lightweight, flexible, and weavable properties, are excellent candidate materials for fabricating wearable fiber batteries. However, fibrous aerogel electrodes often require freeze-drying, a relatively energy-intensive process that demands continuous production. This invention presents an aerogel-like carbon-based fibrous electrode prepared under normal pressure by controlling the solvent evaporation rate. It exhibits similar electrochemical properties and similar bulkiness and flexibility to freeze-dried carbon-based composite fibrous aerogels. This preparation method is simple, low-cost, and facilitates widespread application. Summary of the Invention
[0003] (a) Technical problems to be solved
[0004] To address the issue that existing fibrous aerogel electrodes often require freeze-drying, which is a relatively energy-intensive process and requires continuous production, a method for preparing aerogel-like carbon-based composite fibrous electrodes using atmospheric pressure drying is provided.
[0005] (II) Technical Solution
[0006] A method for preparing an aerogel-like carbon-based composite fibrous electrode by atmospheric pressure drying includes the following steps:
[0007] Step 1: Prepare an aqueous dispersion of carbon nanoparticles with adjustable evaporation rate; add volatile alcohols, carboxylic acids or amines to the aqueous dispersion of carbon nanotubes or carbon nanoparticles in a certain proportion;
[0008] Step 2: Prepare aerogel-like carbon-based fiber electrode; impregnate glycerol-modified polyacrylonitrile aerogel into the carbon nanoparticle dispersion obtained in step 1, and obtain the aerogel-like carbon-based fiber electrode by atmospheric pressure drying under tension, and determine the carbon nanoparticle dispersion system by the characteristics of the electrode.
[0009] Step 3: Prepare aerogel-like carbon-based composite fibrous electrode; based on the first step, disperse other polymers or inorganic nanomaterials in the active material to obtain a composite nano-dispersion, and repeat the second step to obtain the aerogel-like carbon-based composite fibrous electrode.
[0010] As a preferred technical solution, carbon particle nano-aqueous dispersions or carbon nanotube aqueous dispersions can be obtained through particle dispersion or by direct purchase.
[0011] As a preferred technical solution, the solid content in the carbon particle nano-aqueous dispersion or the carbon nanotube aqueous dispersion is about 10%.
[0012] As a preferred technical solution, in the second step, glycerol-modified polyacrylonitrile aerogel is used as a template to prepare an aerogel-like carbon-based fibrous electrode through impregnation and atmospheric pressure drying. The type and concentration of alcohol or carboxylic acid are determined by the morphology and electrochemical performance of the electrode.
[0013] As a preferred technical solution, the aerogel-like carbon-based composite fibrous electrode obtained in the third step is heat-treated to make it lose its hydrophilicity, thereby obtaining a water-resistant aerogel-like carbon-based composite fibrous electrode.
[0014] As a preferred technical solution, the alcohol can be isopropanol, and the carboxylic acid can be acetic acid.
[0015] (III) Beneficial Effects
[0016] The beneficial effects of this invention are as follows:
[0017] 1. The aerogel-like carbon-based fibrous electrode of the present invention is prepared by means of atmospheric pressure drying and by controlling the solvent evaporation rate. It has similar electrochemical properties and similar fluffiness and flexibility to the carbon-based composite fibrous aerogel prepared by freeze drying. The preparation method has the characteristics of simple process, low cost and is conducive to promotion and application.
[0018] 2. This invention utilizes alcohols, carboxylic acids, or amines that are easily volatile and miscible with water as additives, and adds them to an aqueous dispersion of carbon particles or carbon nanotubes to prepare a carbon-based active substance dispersion. Using glycerol-modified polyacrylonitrile aerogel as a template, an aerogel-like carbon-based composite fibrous electrode is prepared by impregnation and atmospheric pressure drying.
[0019] 3. The evaporation rate of the solvent determines the maintenance of the original shape of the template and thus affects the flexibility of the electrode. When the solvent is mainly water, the solvent evaporation rate is slow. The interaction forces and capillary action during evaporation will destroy the original structure of the template, thus causing the prepared electrode to lose its flexibility. By controlling the evaporation rate of the solvent by adjusting the additives, electrodes prepared by atmospheric pressure drying can have similar electrochemical performance to those prepared by freeze drying. Attached Figure Description
[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0021] Figure 1 This is a digital photograph of carbon nanoparticles and PANI:PSS composite aerogel fiber electrodes prepared by stretching, fixing and natural drying.
[0022] Figure 2 This is a scan image of a carbon nanoparticle and PANI:PSS composite aerogel fiber electrode;
[0023] Figure 3 yes Figure 2 A magnified view of a portion of the image;
[0024] Figure 4 Electrochemical behavior of carbon nanoparticles and PANI:PSS composite aerogel fibers as capacitor electrodes under different charge and discharge currents; Detailed Implementation
[0025] The preparation method of the aerogel-like carbon-based composite fibrous electrode by atmospheric pressure drying according to the present invention will be further described below with reference to the accompanying drawings. The present invention will be further described in detail below with reference to the embodiments:
[0026] As attached Figure 1-4 The diagram shows a method for preparing an aerogel-like carbon-based composite fibrous electrode using an atmospheric pressure drying method, comprising the following steps:
[0027] Step 1: Prepare an aqueous dispersion of carbon nanoparticles with adjustable evaporation rate; add volatile alcohols, carboxylic acids or amines to the aqueous dispersion of carbon nanotubes or carbon nanoparticles in a certain proportion;
[0028] Step 2: Prepare aerogel-like carbon-based fiber electrode; impregnate glycerol-modified polyacrylonitrile aerogel into the carbon nanoparticle dispersion obtained in step 1, and obtain the aerogel-like carbon-based fiber electrode by atmospheric pressure drying under tension, and determine the carbon nanoparticle dispersion system by the characteristics of the electrode.
[0029] Step 3: Prepare aerogel-like carbon-based composite fibrous electrode; based on the first step, disperse other polymers or inorganic nanomaterials in the active material to obtain a composite nano-dispersion, and repeat the second step to obtain the aerogel-like carbon-based composite fibrous electrode.
[0030] Furthermore, carbon particle nano-aqueous dispersions or carbon nanotube aqueous dispersions can be obtained through particle dispersion or by direct purchase.
[0031] Furthermore, the solid content in the aqueous dispersion of carbon particles or carbon nanotubes is around 10%.
[0032] Furthermore, in the second step, glycerol-modified polyacrylonitrile aerogel is used as a template to prepare aerogel-like carbon-based fibrous electrode through impregnation and atmospheric pressure drying processes. The type and concentration of alcohol or carboxylic acid are determined by the morphology and electrochemical performance of the electrode.
[0033] Furthermore, the aerogel-like carbon-based composite fibrous electrode obtained in the third step is heat-treated to remove its hydrophilicity, resulting in a water-resistant aerogel-like carbon-based composite fibrous electrode.
[0034] Furthermore, the alcohol can be isopropanol, and the carboxylic acid can be acetic acid.
[0035] It should be noted that the first step involves dispersing a 10% (w / w) formic acid and a 5% (w / w) PANI:PSS solution into a 10% (w / w) aqueous dispersion of carbon nanoparticles to prepare a mixed slurry.
[0036] Step 2: The glycerol-modified polyacrylonitrile aerogel is impregnated into the carbon nanoparticle dispersion obtained in Step 1. Under tension, it is dried at atmospheric pressure to obtain an aerogel-like carbon-based fiber electrode. Due to the supporting effect of the carbon nanoparticle material and a suitable evaporation rate, the entire electrode does not show significant collapse. Its digital photograph is shown below. Figure 1 As shown, Figure 2 The electrode showed no obvious collapse, and its gel-like structure facilitated the wetting of the gel electrolyte. A further magnified image is shown below. Figure 3 The diagram also demonstrates its porous nature. When used as a capacitor electrode, it exhibits excellent electrochemical behavior, as shown in the data... Figure 4 As shown, at a scan rate of 1 mA cm -1 Capacity per unit length can reach 373 mF cm -1 .
[0037] It should be noted that PANI:PSS can be impregnated and loaded after impregnation with carbon nanoparticles, or it can be prepared into a mixed solution with carbon nanoparticles and loaded in one step.
[0038] The above embodiments are merely descriptions of preferred embodiments of the present invention and are not intended to limit the concept and scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the design concept of the present invention should fall within the protection scope of the present invention. The technical content for which protection is sought in the present invention has been fully described in the claims.
Claims
1. A method for preparing an aerogel-like carbon-based composite fibrous electrode using an atmospheric pressure drying method, characterized in that: Includes the following steps: Step 1: Prepare an aqueous carbon nanoparticle dispersion with adjustable evaporation rate; Volatile alcohols and carboxylic acids are added to a carbon nanoparticle dispersion, wherein the solid content of the carbon nanoparticle dispersion is 10%. Step 2: Preparation of aerogel-like carbon-based fibrous electrode; Glyceryl modified polyacrylonitrile aerogel is impregnated into the carbon nanoparticle dispersion obtained in Step 1, and the aerogel-like carbon-based fibrous electrode is obtained by atmospheric pressure drying while maintaining tension. The carbon nanoparticle dispersion system is determined by the characteristics of the electrode. Using glyceryl modified polyacrylonitrile aerogel as a template, the aerogel-like carbon-based fibrous electrode is prepared by impregnation and atmospheric pressure drying. The type and concentration of alcohol or carboxylic acid are determined by the morphology and electrochemical performance of the electrode. Step 3: Prepare aerogel-like carbon-based composite fibrous electrode; Based on the first step, repeat the second step in carbon nanoparticle dispersion and PANI:PSS solution to obtain aerogel-like carbon-based composite fibrous electrode. Heat treat the obtained aerogel-like carbon-based composite fibrous electrode to make it lose its hydrophilicity and obtain a water-resistant aerogel-like carbon-based composite fibrous electrode. The alcohol is isopropanol, and the carboxylic acid is acetic acid.
2. The method for preparing an aerogel-like carbon-based composite fibrous electrode by atmospheric pressure drying as described in claim 1, characterized in that: The carbon nanoparticle dispersion can be obtained through particle dispersion or by direct purchase.