CN109265191B - Preparation method and application of nano onion carbon/carbon fiber composite electrode material - Google Patents
Preparation method and application of nano onion carbon/carbon fiber composite electrode material Download PDFInfo
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- CN109265191B CN109265191B CN201810917288.7A CN201810917288A CN109265191B CN 109265191 B CN109265191 B CN 109265191B CN 201810917288 A CN201810917288 A CN 201810917288A CN 109265191 B CN109265191 B CN 109265191B
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Abstract
The invention discloses a preparation method of a nano onion carbon/carbon fiber composite electrode material, which comprises the steps of loading transition metal salt in phenolic-based active carbon fibers subjected to pre-nitric acid treatment by an impregnation method, then carrying out high-temperature treatment to obtain a composite material of carbon fiber loaded nano onion carbon coated metal simple substance particles, and then washing away the metal particles by using an acid solution to finally obtain the nano onion carbon loaded carbon fiber composite electrode material. The preparation method is simple and effective, has good repeatability, low price of the used raw materials and small enlargement effect of the preparation process, and is convenient for large-batch preparation. The nano onion carbon is generated in situ under the condition of not introducing other carbon sources by utilizing the catalytic action of the metal simple substance under the high-temperature condition, the harsh requirements of other preparation conditions are overcome, and the method has good production prospect. The prepared nano onion carbon has the advantages of high specific surface area, high conductivity and good electrochemical stability.
Description
Technical Field
The invention belongs to the technical field of composite electrode material preparation, and relates to a preparation method and application of a nano onion carbon/carbon fiber composite electrode material.
Background
With the rapid development of society and the rapid increase of population, the consumption and demand of energy are increasing day by day, and the development of an efficient, convenient and stable energy storage technology becomes one of the keys of clean energy utilization. With the technology progress, people are pursuing portable electronic devices with portability, entertainment and health, and the corresponding energy storage devices are promoted to develop towards high specific energy, light weight, softness, cleanness, safety and the like.
In the field of flexible energy storage, flexible carbon-based electrodes represented by carbon fiber cloth are widely concerned, and have the advantages of excellent foldable bending performance, excellent electric conductivity, higher loadable specific surface area, light weight and the like. Meanwhile, the electrode material based on the carbon fiber cloth is also applied to other energy storage and conversion fields such as electrocatalysis and the like, and a certain progress is made.
Nano onion carbon (onion-carbon) is a member of fullerene family, which is formed by nesting concentric graphite sphere layers and belongs to carbon allotropes. The nano onion carbon has large specific surface area, high conductivity, good mechanical stability, thermal stability and electrochemical stability. The excellent performances enable the material to have good application prospects in various fields, such as lithium ion batteries, fuel cells, dye-sensitized solar cells, super capacitors, electrochemical hydrogen storage, microwave absorption, lubrication, catalysis and other fields.
At present, few reports of the nano onion carbon effective load on the flexible carbon fiber for preparing the composite electrode exist, and the general method for preparing the nano onion carbon has the disadvantages of high process difficulty, high cost, low yield and difficulty in large-scale production.
Therefore, the preparation method of the nano onion carbon/carbon fiber composite electrode material is provided for solving the problems.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method and application of a nano onion carbon/carbon fiber composite electrode material.
The invention achieves the above objects by the following technical solutions,
a preparation method of a nano onion carbon/carbon fiber composite electrode material comprises the following steps:
1) carrying out pre-nitric acid treatment on the carbon fiber to obtain pre-treated carbon fiber;
2) loading transition metal salt in the pretreated carbon fiber obtained in the step 1) by using an impregnation method to obtain the pretreated carbon fiber loaded with the transition metal salt;
3) carrying out high-temperature treatment on the transition metal salt loaded carbon fiber obtained in the step 2) to obtain a carbon fiber loaded nano onion carbon coated metal simple substance particle composite material;
4) and washing away the metal simple substance particles of the composite material in the step 3) by using an acid solution to obtain the carbon fiber composite electrode material loaded with the nano onion carbon.
Furthermore, the pre-nitric acid treatment in the step 1) is to immerse the carbon fiber in concentrated nitric acid, wherein the immersion temperature is 40-120 ℃, and the immersion time is 4-24 h.
Furthermore, the pretreated carbon fiber is phenolic-based activated carbon fiber.
Further, the transition metal in the step 2) is any one or combination of more of Ti, Mn, Fe, Co, Ni, Cu, Zn, Mo, Sn and Pb.
Further, the transition metal salt in the step 2) is any one or more of nitrate, nitrite, sulfate, sulfite, chloride, fluoride and acetate of the transition metal.
Furthermore, the dipping time of the dipping method in the step 2) is 6-48h, the dipping temperature is 10-60 ℃, the solvent for dipping is one or the combination of two of water, methanol, ethanol, acetone and ether, and the concentration of the transition metal salt is 0.05-2 mol/L. The structure and the morphology of the nano onion carbon can be effectively regulated and controlled by regulating the dipping temperature, the dipping time and the concentration of the salt solution, and the nano onion carbon has the advantages of high yield, uniform morphology and structure and low impurity content.
Furthermore, the high-temperature treatment in the step 3) is carried out under the inert gas atmosphere, the treatment temperature is 600-1500 ℃, and the heat preservation time is 0.5-5 h.
Furthermore, the acid solution in the step 4) is hydrochloric acid, nitric acid or sulfuric acid, and the concentration is 0.1-3 mol/L.
Further, the carbon fibers in step 1) are flexible carbon fibers. The nano onion carbon grows on the flexible carbon fiber in situ to form a composite electrode with flexible performance and good electrochemical performance, so that the nano onion carbon has wide application prospect in the field of flexible energy storage.
The invention principle is as follows: loading transition metal salt in the phenolic aldehyde group activated carbon fiber treated by the pre-nitric acid through an impregnation method, then obtaining a composite material of carbon fiber loaded with nano onion carbon and wrapped with metal simple substance particles through high-temperature treatment, and then washing away the metal particles by using an acid solution to finally obtain the carbon fiber composite electrode material loaded with the nano onion carbon.
Has the advantages that: the preparation method of the nano onion carbon/carbon fiber composite electrode material is simple and effective, has good repeatability, low price of the used raw materials and small enlargement effect of the preparation process, and is convenient for large-batch preparation. The nano onion carbon is generated in situ under the condition of not introducing other carbon sources by utilizing the catalytic action of the metal simple substance under the high-temperature condition, the harsh requirements of other preparation conditions are overcome, and the method has good production prospect. The prepared nano onion carbon has the advantages of high specific surface area, high conductivity and good electrochemical stability.
Drawings
FIG. 1 is a photograph of a nano-onion carbon/carbon fiber composite electrode material prepared in example 1;
fig. 2 and 3 are SEM images of the nano onion carbon/carbon fiber composite electrode material prepared in example 1;
fig. 4 and 5 are TEM images of the nano onion carbon/carbon fiber composite electrode material prepared in example 2;
fig. 6 is a capacitance performance curve of the nano onion carbon/carbon fiber composite electrode material prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the nano onion carbon/carbon fiber composite electrode material comprises the following steps:
1) carrying out pre-nitric acid treatment on the carbon fiber to obtain pre-treated carbon fiber; preferably, the pre-nitric acid treatment in the step 1) is to immerse the carbon fibers in concentrated nitric acid, wherein the immersion temperature is 40-120 ℃, and the immersion time is 4-24 h. Preferably, the pretreated carbon fibers are phenolic-based activated carbon fibers.
2) Loading transition metal salt in the pretreated carbon fiber obtained in the step 1) by using an impregnation method to obtain the pretreated carbon fiber loaded with the transition metal salt; preferably, the transition metal in step 2) is any one or more of Ti, Mn, Fe, Co, Ni, Cu, Zn, Mo, Sn and Pb.
Preferably, the transition metal salt in step 2) is any one or more of nitrate, nitrite, sulfate, sulfite, chloride, fluoride and acetate of transition metal.
Preferably, the impregnation time of the impregnation method in the step 2) is 6-48h, the impregnation temperature is 10-60 ℃, the solvent for impregnation is one or a combination of two of water, methanol, ethanol, acetone and diethyl ether, and the concentration of the transition metal salt is 0.05-2 mol/L. The structure and the morphology of the nano onion carbon can be effectively regulated and controlled by regulating the dipping temperature, the dipping time and the concentration of the salt solution, and the nano onion carbon has the advantages of high yield, uniform morphology and structure and low impurity content.
3) Carrying out high-temperature treatment on the transition metal salt loaded carbon fiber obtained in the step 2) to obtain a carbon fiber loaded nano onion carbon coated metal simple substance particle composite material; preferably, the high-temperature treatment in the step 3) is carried out under the inert gas atmosphere, the treatment temperature is 600-1500 ℃, and the heat preservation time is 0.5-5 h.
4) And washing away the metal simple substance particles of the composite material in the step 3) by using an acid solution to obtain the carbon fiber composite electrode material loaded with the nano onion carbon. Preferably, the acid solution in the step 4) is hydrochloric acid, nitric acid or sulfuric acid, and the concentration is 0.1-3 mol/L.
The invention principle is as follows: loading transition metal salt in the phenolic aldehyde group activated carbon fiber treated by the pre-nitric acid through an impregnation method, then obtaining a composite material of carbon fiber loaded with nano onion carbon and wrapped with metal simple substance particles through high-temperature treatment, and then washing away the metal particles by using an acid solution to finally obtain the carbon fiber composite electrode material loaded with the nano onion carbon.
The invention has the following advantages and effects:
1. the preparation process flow is simple and effective, the repeatability is good, the price of the used raw materials is low, the expansion effect of the preparation process is small, and the preparation process is convenient for large-batch preparation. The nano onion carbon is generated in situ under the condition of not introducing other carbon sources by utilizing the catalytic action of the metal simple substance under the high-temperature condition, the harsh requirements of other preparation conditions are overcome, and the method has good production prospect.
2. The structure and the morphology of the nano onion carbon can be effectively regulated and controlled by regulating the temperature, the heat preservation time and the concentration of the salt solution, and the nano onion carbon has the advantages of high yield, uniform morphology and structure and low impurity content.
3. The prepared nano onion carbon has the advantages of high specific surface area, high conductivity and good electrochemical stability. The nano onion carbon grows on the flexible carbon fiber in situ to form a composite electrode with flexible performance and good electrochemical performance, so that the nano onion carbon has wide application prospect in the field of flexible energy storage.
Example 1:
the nano onion carbon/carbon fiber composite electrode material is prepared according to the prior art.
(1) Immersing a certain amount of carbon fibers in concentrated nitric acid, keeping the temperature in an oven at 80 ℃ for 9 hours, taking out, and cleaning with water and ethanol;
(2) and soaking the treated carbon fiber in 0.5mol/L cobalt acetate water solution for 24h under the water bath condition of 60 ℃, taking out and drying in an oven at 60 ℃.
(3) And (3) placing the carbon fiber loaded with the cobalt acetate in a tubular furnace for calcination, wherein the treatment temperature is 900 ℃, the heat preservation time is 5 hours, and the protective atmosphere is argon.
(4) And (3) soaking the calcined sample in 1mol/L dilute nitric acid solution, washing away the cobalt simple substance, taking out the carbon fiber, cleaning and drying to obtain the carbon fiber flexible electrode material loaded with the nano onion carbon.
Fig. 1 shows a physical photograph of the nano onion carbon/carbon fiber composite electrode material, which has better mechanical flexibility and certain mechanical strength and can meet the folding and bending requirements of a common flexible device under working conditions. Fig. 2 and 3 are scanning electron microscope images of the prepared nano onion carbon/carbon fiber composite electrode material, which show that the treated carbon fiber has rich pore structure and specific surface area, and can provide more electrochemical active sites, thereby being beneficial to providing higher electrochemical performance.
Example 2:
the nano onion carbon/carbon fiber composite electrode material is prepared according to the prior art.
(1) Immersing a certain amount of carbon fibers in concentrated nitric acid, keeping the temperature in an oven at 90 ℃ for 6 hours, taking out the carbon fibers, and washing the carbon fibers with water and ethanol;
(2) and soaking the treated carbon fiber in 0.1mol/L ethanol solution of nickel nitrate, soaking for 12h under the condition of water bath at 30 ℃, taking out and drying in an oven at 60 ℃.
(3) And (3) calcining the carbon fiber loaded with the cobalt acetate in a tubular furnace at the treatment temperature of 1200 ℃, keeping the temperature for 3 hours and under the protection atmosphere of argon-hydrogen mixed gas.
(4) And soaking the calcined sample in 0.3mol/L dilute hydrochloric acid solution, washing away the nickel simple substance, taking out the carbon fiber, cleaning and drying to obtain the carbon fiber flexible electrode material loaded with the nano onion carbon.
As shown in fig. 4 and 5, the prepared nano onion carbon/carbon fiber composite electrode material is characterized by a high-resolution transmission electron microscope, and images show the micro-morphology structure of the nano onion carbon, so that the nano onion carbon has good uniformity, stable structure and clear graphite lamellar structure.
In addition, the obtained nano onion carbon/carbon fiber composite electrode material is used as a working electrode, a capacitance performance test is carried out under a three-electrode system, and a cyclic voltammetry curve in 6mol/L potassium hydroxide electrolyte is shown in fig. 6. The capacity of the nano onion carbon/carbon fiber composite electrode calculated according to the CV curve is as high as 180F/g, which is higher than the reported values of most of the existing documents, and the electrode material has better rate performance and cycling stability.
Claims (6)
1. The preparation method of the nano onion carbon/carbon fiber composite electrode material is characterized by comprising the following steps of:
1) carrying out pre-nitric acid treatment on the carbon fiber to obtain pre-treated carbon fiber; in the step 1), the pre-nitric acid treatment is to immerse the carbon fibers in concentrated nitric acid, wherein the immersion temperature is 40-120 ℃, and the immersion time is 4-24 h;
2) loading transition metal salt in the pretreated carbon fiber obtained in the step 1) by using an impregnation method to obtain the pretreated carbon fiber loaded with the transition metal salt; the transition metal salt in the step 2) is any one or combination of more of nitrate, nitrite, sulfate, sulfite, chloride salt, fluoride salt and acetate of the transition metal, and the concentration of the transition metal salt is 0.05-2 mol/L; the dipping time of the dipping method in the step 2) is 6-48h, the dipping temperature is 10-60 ℃, and the solvent selected for dipping is one or the combination of two of water, methanol, ethanol, acetone and ether;
3) carrying out high-temperature treatment on the transition metal salt loaded carbon fiber obtained in the step 2) to obtain a carbon fiber loaded nano onion carbon coated metal simple substance particle composite material; the high-temperature treatment in the step 3) is carried out in an inert gas atmosphere at the treatment temperature of 600-1500 ℃ and the heat preservation time of 0.5-5 h;
4) and washing away the metal simple substance particles of the composite material in the step 3) by using an acid solution to obtain the carbon fiber composite electrode material loaded with the nano onion carbon.
2. The preparation method of the nano onion carbon/carbon fiber composite electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: the pretreated carbon fiber is phenolic activated carbon fiber.
3. The preparation method of the nano onion carbon/carbon fiber composite electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step 2), the transition metal is Ti, Mn, Fe, Co, Ni, Cu, Zn, Mo,
Any one or combination of more of Sn and Pb.
4. The preparation method of the nano onion carbon/carbon fiber composite electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: the acid solution in the step 4) is hydrochloric acid, nitric acid or sulfuric acid, and the concentration is 0.1-3 mol/L.
5. The preparation method of the nano onion carbon/carbon fiber composite electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: the carbon fiber in the step 1) is flexible carbon fiber.
6. The application of the nano onion carbon/carbon fiber composite electrode material is characterized in that the nano onion carbon/carbon fiber composite electrode material is applied to a flexible carbon fiber composite electrode.
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