CN110350201B - Light high-conductivity graphene current collector for water-based battery and preparation method thereof - Google Patents
Light high-conductivity graphene current collector for water-based battery and preparation method thereof Download PDFInfo
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- 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
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a light high-conductivity graphene current collector for a water-based battery and a preparation method thereof. The method comprises the following steps: mixing graphite and concentrated sulfuric acid, stirring, pre-oxidizing, sequentially adding hydrogen peroxide and a foaming agent, stirring and mixing uniformly, and standing at room temperature to obtain a large amount of graphene; and rolling the prepared graphene under different pressures under a rolling machine to obtain the light high-conductivity graphene current collector for the water system battery. The invention provides a simple and low-cost realization path for massively preparing light high-conductivity flexible graphene paper, and the whole process only needs a simple physical mixing and dry pressing treatment without any high-temperature or heating complex treatment or any complex instrument and equipment. Compared with the traditional graphene preparation method, the preparation method has the advantage that the acid consumption is reduced, so that the method is a simple and efficient green preparation scheme, and is beneficial to industrial production of the graphene current collector.
Description
Technical Field
The invention relates to the field of graphene-based conductive current collectors for low-temperature energy storage, in particular to a light high-conductivity graphene current collector for a water-based battery and a preparation method thereof.
Background
The lithium ion battery is the chemical energy storage battery with the highest energy density at present. However, the inflammable organic electrolyte causes frequent safety accidents of the lithium ion battery, and accidents such as Tesla electric vehicle ignition, Samsung mobile phone explosion and the like are always in the future. Therefore, a safe, clean aqueous battery is considered to be the best alternative for replacing an organic battery in the future.
The current battery device mainly comprises a positive electrode material, a negative electrode material, a diaphragm, electrolyte, a current collector and a battery shell. The current research article about the battery system mainly focuses on the research of a current collector and electrolyte, and the current collector is a research direction in which scientific researchers pay relatively little attention. In principle, a battery which can be truly industrialized, has good conductive performance, is cheap, is easy to process and has a current collector which is stable in a battery system is the first problem to be considered. Once these problems are solved, it is basically possible to do once and for all.
The current collectors mainly include two types, namely metal-based collectors and carbon-based collectors, wherein the metal-based collectors mainly include copper used as a negative electrode collector and aluminum used as a positive electrode collector, and are very mature in an organic system, but almost all metal-based collectors cannot exist stably due to high reactivity of an aqueous electrolyte. And the metals can play a role in catalyzing and promoting the hydrogen and oxygen evolution reaction of the aqueous electrolyte, so that the stable voltage window of the whole battery is reduced, and the energy density of the final battery is influenced. The current carbon-based current collectors are mainly commercial carbon paper and carbon cloth, and the two current collectors have poor hydrophilicity and can be normally used only by improving the hydrophilicity through pretreatment. And most importantly, the mass of the current collectors is larger than that of the active material coated on the current collectors, and the current research and calculation of the capacity only needs to calculate the amount of the single active material, so that the capacity of the whole battery is greatly reduced if the current collectors are calculated. Therefore, a current collector which is light, highly conductive and stable in an aqueous battery system is urgently required.
Graphene, a novel two-dimensional carbon material, is also a special semiconductor material without a band gap, and has excellent conductivity, excellent flexibility and light unit mass. This series of advantages can exactly meet the use requirements of the ideal current collector of the water-based battery. Also based on this, there have been reports of related documents that graphene is applied as a substrate to flexible devices, which exhibit outstanding electrochemical properties. However, the preparation methods are very complicated and high in cost, and are only suitable for research, but cannot achieve real large-scale production.
Disclosure of Invention
The invention aims to provide a light high-conductivity graphene current collector for a water-based battery and a preparation method thereof, aiming at the defects in the prior art.
The invention aims to provide light-weight high-conductivity flexible graphene paper which can be stably used in a water-based battery system, and compared with the traditional graphene preparation method, the graphene preparation method is simpler and more efficient, has lower cost and is suitable for industrial production.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a light high-conductivity graphene current collector for a water-based battery, which comprises the following steps:
(1) mixing graphite and concentrated sulfuric acid solution, uniformly stirring, and carrying out pre-oxidation treatment to form a mixture;
(2) sequentially adding a hydrogen peroxide solution and a foaming agent into the mixture obtained in the step (1), uniformly stirring, standing at room temperature, and then expanding to obtain graphene powder;
(3) and (3) carrying out rolling treatment (1-50 Mpa) on the graphene powder in the step (2) through a rolling machine to obtain the light high-conductivity graphene current collector for the water system battery.
Further, the graphite in the step (1) is natural crystalline flake graphite, and the granularity of the graphite is 50-5000 meshes; the purity was 99.99%.
Further, the concentrated sulfuric acid solution in the step (1) is a sulfuric acid solution with a mass fraction of more than or equal to 70%.
Further, the mass-to-volume ratio of the graphite to the concentrated sulfuric acid solution in the step (1) is 1-20: 5-300 g/mL; the time of the pre-oxidation treatment is 1-30 min.
Preferably, the stirring time of the step (1) is 1-60min, and the stirring speed is 50-300 r/min.
Further, the concentration of the hydrogen peroxide solution in the step (2) is 30% wt by mass.
Further, the mass-volume ratio of the graphite in the step (1) to the hydrogen peroxide solution in the step (2) is 1-20: 2-200 g/mL.
Further, the foaming agent in the step (2) is more than one of azodicarbonamide, polyurethane, dinitrosopentamethylenetetramine and p-toluenesulfonyl hydrazide; the mass ratio of the graphite in the step (1) to the foaming agent in the step (2) is 1-20: 1-40.
Preferably, the stirring time of the step (2) is 1-60min, and the stirring speed is 50-300 r/min;
further, the standing time in the step (2) is 1-24h, and the standing temperature is room temperature.
Further, the pressure of the rolling treatment in the step (3) is 1-50 MPa.
The light high-conductivity graphene current collector for the water system battery prepared by the method is light and high in conductivity, and the conductivity of the graphene current collector is 0.8-6.3 x10 4 S m -1 。
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the method for preparing the light high-conductivity graphene current collector for the water-based battery, provided by the invention, can be used for puffing a large amount of graphene only by simple physical mixing and room-temperature standing treatment at normal temperature, does not need other complex treatments such as high temperature or heating and the like, and is a simple and cost-effective method;
(2) according to the method for preparing the light high-conductivity graphene current collector for the water-based battery, the amount of introduced acid is less and only 10% -20% of that of a traditional oxidation-reduction method, the discharge treatment pressure of waste liquid and waste acid in the later period is reduced, and the prepared graphene is higher in quality compared with a sample synthesized by the traditional method, so that the method is efficient and clean;
(3) the method for preparing the light high-conductivity graphene current collector for the water-based battery can roll out the high-conductivity light flexible graphene paper under dry pressing, does not need to use complex and precise instruments, and has certain significance for realizing industrial production of the graphene paper as the current collector.
Drawings
Fig. 1 is a microscopic SEM image of the light highly conductive graphene current collector for an aqueous battery obtained in example 1;
fig. 2 is a hydrophilicity test chart of the light high-conductivity graphene current collector for an aqueous battery obtained in example 1;
FIG. 3 is a hydrophilicity test chart of a commercial carbon cloth;
fig. 4 is a hydrophilicity test chart of commercial carbon paper.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, if not specifically detailed, are all those that can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated by the manufacturer, and are regarded as conventional products commercially available.
Example 1
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 1g of 50-mesh natural crystalline flake graphite with 15mL of concentrated sulfuric acid solution for 10 min at a stirring speed of 100 r/min, uniformly stirring, carrying out pre-oxidation treatment for 15min, then sequentially adding 6mL of hydrogen peroxide solution with the mass percentage concentration of 30% and 2g of azodicarbonamide, stirring at a speed of 50 r/min for 3min, uniformly mixing, and standing at room temperature for 10 h to obtain graphene powder after expansion; and then pressing the prepared graphene powder into flexible graphene paper under the pressure of 25 Mpa, namely the light high-conductivity graphene current collector for the water system battery.
Fig. 1 is a microscopic SEM image of a light-weight high-conductivity graphene current collector for an aqueous battery obtained in example 1; as shown in fig. 1, it can be seen that: after the flake graphite is subjected to double puffing of gas generated by decomposition of a foaming agent and hydrogen peroxide, the layers are completely puffed and stripped, the puffing effect is obvious, and the graphene layers can be seen more visually from a scanning electron microscope picture to be relatively transparent, which shows that the number of graphene layers obtained by stripping by the method is relatively small. Other examples the effect observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1.
The prepared light high-conductivity graphene current collector for the water system battery is subjected to dry pressing on a rolling machine to form a 5x 20cm graphene paper strip, the graphene paper is folded for 360 degrees and still well preserved, good flexibility is shown, and the graphene paper is suitable for flexible devices.
Fig. 2, 3 and 4 show the graphene paper strip (5 × 20 cm) and the commercial carbon cloth and the commercial carbon paper, respectivelyThe hydrophilicity comparison test shows that the hydrophilicity of the graphene paper strip is better than that of the commercial carbon cloth and the commercial carbon paper, the wetting angle is only 85 degrees, and the wetting angle is better than that of the commercial carbon cloth and the commercial carbon paper (142.8 degrees and 123.7 degrees), so that the graphene paper strip is favorable for the practical use as a current collector. Meanwhile, the square resistivity of the obtained graphene paper strip is measured to be 0.319 omega/cm by a four-probe test method at room temperature, and the square resistivity is converted to be 6.3x10 4 S m -1 The conductivity of the graphene paper strip is equivalent to that of commercial carbon cloth and commercial carbon paper, and the graphene paper strip has high conductivity and can be used as a current collector. Other embodiments have similar effects to embodiment 1, and refer to fig. 2, fig. 3, and fig. 4.
Example 2
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 0.2g of 300-mesh natural crystalline flake graphite with 1mL of concentrated sulfuric acid solution for 3min, wherein the stirring speed is 50 r/min, uniformly stirring, carrying out pre-oxidation treatment for 5min, then sequentially adding 2mL of hydrogen peroxide solution with the mass percentage concentration of 30% and 0.3g of polyurethane, stirring at the speed of 50 r/min for 1min, uniformly mixing, standing at room temperature for 2h, and expanding to obtain graphene powder; pressing the prepared graphene powder into flexible graphene paper under the pressure of 10Mpa, namely obtaining the light high-conductivity graphene current collector for the water system battery, and measuring the electric conductivity of the obtained graphene current collector at room temperature by a potentiostatic method to be 2.2x10 4 S m -1 . The effect of the light high-conductivity graphene current collector for the aqueous battery obtained in example 2 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light-weight high-conductivity graphene current collector for an aqueous battery prepared in example 2 was similar to that of example 1, and reference can be made to fig. 2.
Example 3
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 0.8g of natural crystalline flake graphite with 500 meshes with 12mL of concentrated sulfuric acid solution for 8min at the stirring speed of 80 r/min, uniformly stirring, and carrying out pre-oxidation treatment 1After 0min, sequentially adding 6ml of hydrogen peroxide solution with the mass percentage concentration of 30% and 1.5g of dinitrosopentamethylenetetramine, stirring at the speed of 50 r/min for 3min, uniformly mixing, and standing at room temperature for 6h to obtain graphene powder through expansion; then pressing the prepared graphene powder into flexible graphene paper under the pressure of 20Mpa, namely, the prepared light high-conductivity graphene current collector for the water system battery, and measuring the electric conductivity of the obtained graphene current collector to be 1.6x10 at room temperature by a potentiostatic method 4 S m -1 . The effect of the light-weight high-conductivity graphene current collector for the water system battery obtained in example 3 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light highly conductive graphene current collector for the aqueous battery obtained in example 3 is similar to that of example 1, and reference can be made to fig. 2.
Example 4
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 1.5g of 1000-mesh natural crystalline flake graphite with 20mL of concentrated sulfuric acid solution for 15min, wherein the stirring speed is 150 r/min, uniformly stirring, carrying out pre-oxidation treatment for 20min, then sequentially adding 12mL of hydrogen peroxide solution with the mass percentage concentration of 30% and 3g of p-toluenesulfonyl hydrazide, stirring at the speed of 150 r/min for 5min, uniformly mixing, standing at room temperature for 16 h, and expanding to obtain graphene powder; then pressing the prepared graphene powder into flexible graphene paper under the pressure of 35 Mpa, namely, the prepared light high-conductivity graphene current collector for the water system battery, and measuring the conductivity of the obtained graphene current collector to be 8.0x10 at room temperature by a potentiostatic method 4 S m -1 . The effect of the light-weight high-conductivity graphene current collector for the water system battery obtained in example 4 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light highly conductive graphene current collector for the aqueous battery obtained in example 4 is similar to that of example 1, and reference can be made to fig. 2.
Example 5
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 2g of 3000-mesh natural crystalline flake graphite with 30 mL of concentrated sulfuric acid solution for 20min at a stirring speed of 200 r/min, uniformly stirring, pre-oxidizing for 30min, sequentially adding 12mL of hydrogen peroxide solution with the mass percentage concentration of 30% and 4g of p-toluenesulfonyl hydrazide, stirring at a speed of 200 r/min for 7 min, uniformly mixing, and standing at room temperature for 24h to obtain the graphene powder after expansion. Pressing the prepared graphene powder into flexible graphene paper under the pressure of 50Mpa, namely obtaining the light high-conductivity graphene current collector for the prepared water system battery, and measuring the electric conductivity of the obtained graphene current collector at room temperature by a potentiostatic method to be 4.5x10 4 S m -1 . The effect of the light-weight high-conductivity graphene current collector for the water system battery obtained in example 5 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light highly conductive graphene current collector for the aqueous battery obtained in example 5 is similar to that of example 1, and reference can be made to fig. 2.
Example 6
A method for preparing a light high-conductivity graphene current collector for an aqueous battery comprises the following steps:
stirring and mixing 0.5g of 5000-mesh natural crystalline flake graphite with 10mL of concentrated sulfuric acid solution for 10 min, wherein the stirring speed is 100 r/min, uniformly stirring, carrying out pre-oxidation treatment for 6min, then sequentially adding 12mL of hydrogen peroxide solution with the mass percentage concentration of 30%, 0.5g of p-toluenesulfonyl hydrazide and 0.6g of dinitrosopentamethylenetetramine, stirring at the speed of 100 r/min for 2min, uniformly mixing, and standing at room temperature for 4h to obtain graphene powder after expansion; then pressing the prepared graphene powder into flexible graphene paper under the pressure of 12 Mpa, namely, the light high-conductivity graphene current collector for the water system battery, and measuring the electric conductivity of the obtained graphene current collector to be 2.4x10 at room temperature by a potentiostatic method 4 S m -1 . The effect of the light high-conductivity graphene current collector for the aqueous battery obtained in example 6 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light-weight high-conductivity graphene current collector for an aqueous battery prepared in example 6 was similar to that of example 1, and reference may be made to fig. 2.
Example 7
A method for preparing a light high-conductivity graphene current collector for a water-based battery comprises the following steps:
stirring and mixing 1.7g of 80-mesh natural crystalline flake graphite with 25mL of concentrated sulfuric acid solution for 30min at a stirring speed of 300r/min, uniformly stirring, carrying out pre-oxidation treatment for 25min, then sequentially adding 18mL of hydrogen peroxide solution with a mass percentage concentration of 30%, 1.5g of azodicarbonamide and 1.8g of polyurethane, stirring at a speed of 300r/min for 4min, uniformly mixing, and standing at room temperature for 18h to obtain the graphene powder after expansion. Then pressing the prepared graphene powder into flexible graphene paper under the pressure of 40Mpa, namely, the light high-conductivity graphene current collector for the water system battery, and measuring the electric conductivity of the obtained graphene current collector to be 5.6x10 at room temperature by a potentiostatic method 4 S m -1 . The effect of the light-weight highly conductive graphene current collector for the aqueous battery obtained in example 7 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. The hydrophilicity of the light highly conductive graphene current collector for the aqueous battery obtained in example 7 is similar to that of example 1, and reference can be made to fig. 2.
Example 8
A method for preparing a light high-conductivity graphene current collector for a water-based battery comprises the following steps:
stirring and mixing 1.2g of 50-mesh natural crystalline flake graphite with 16mL of concentrated sulfuric acid solution for 12min at a stirring speed of 120 r/min, uniformly stirring, carrying out pre-oxidation treatment for 20min, then sequentially adding 8mL of hydrogen peroxide solution with a mass percentage concentration of 30%, 1g of azodicarbonamide and 1.5g of p-toluenesulfonyl hydrazide, stirring at a speed of 120 r/min for 3.5min, uniformly mixing, standing at room temperature for 14h, and puffing to obtain graphene powder. Then pressing the prepared graphene powder into flexible graphene paper under the pressure of 30Mpa, namely, the light high-conductivity graphene current collector for the water system battery, and measuring the electric conductivity of the obtained graphene current collector to be 9.6x10 at room temperature by a potentiostatic method 3 S m -1 . The effect of the light high-conductivity graphene current collector for the aqueous battery obtained in example 8 observed under a scanning electron microscope is similar to that of example 1, and reference can be made to fig. 1. EXAMPLE 8 preparation ofThe hydrophilicity of the obtained lightweight highly conductive graphene current collector for an aqueous battery was similar to that of example 1, and reference can be made to fig. 2.
In summary, according to the preparation method of the light high-conductivity graphene current collector for the water-based battery, the conductivity of the prepared graphene is as high as 6.3x10 3 S m -1 . The conductivity of the graphene paper is higher than that of common metals, and meanwhile, the wetting angle of the graphene paper is smaller than 90 degrees, so that the graphene paper is hydrophilic, and the wettability of the graphene paper is superior to that of commercial carbon cloth and commercial carbon paper. Meanwhile, the prepared light high-conductivity graphene current collector for the water-based battery has good flexibility, and the structure is well preserved even when the current collector is folded by 360 degrees.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (9)
1. A preparation method of a light high-conductivity graphene current collector for a water system battery is characterized by comprising the following steps:
(1) mixing graphite and concentrated sulfuric acid solution, uniformly stirring, and carrying out pre-oxidation treatment to form a mixture;
(2) sequentially adding a hydrogen peroxide solution and a foaming agent into the mixture obtained in the step (1), uniformly stirring, and standing to obtain graphene powder;
(3) carrying out rolling treatment on the graphene powder in the step (2), wherein the pressure of the rolling treatment is 1-50 Mpa; preparing the light high-conductivity graphene current collector for the water-based battery;
the mass volume ratio of the graphite in the step (1) to the hydrogen peroxide solution in the step (2) is 1-20: 2-200 g/mL; the mass ratio of the graphite in the step (1) to the foaming agent in the step (2) is 1-20: 1-40.
2. The preparation method of the light high-conductivity graphene current collector for the water-based battery according to claim 1, wherein the graphite in the step (1) is natural crystalline flake graphite, and the particle size of the graphite is 50-5000 meshes.
3. The method for preparing the light high-conductivity graphene current collector for the water-based battery according to claim 1, wherein the concentrated sulfuric acid solution in the step (1) is a sulfuric acid solution with a mass fraction of 70% or more.
4. The preparation method of the light high-conductivity graphene current collector for the water-based battery according to claim 1, wherein the mass-to-volume ratio of the graphite to the concentrated sulfuric acid solution in the step (1) is 1-20: 5-300 g/mL; the time of the pre-oxidation treatment is 1-30 min.
5. The method for preparing a light-weight high-conductivity graphene current collector for an aqueous battery according to claim 1, wherein the hydrogen peroxide solution in the step (2) has a mass percent concentration of 30% wt.
6. The method for preparing a light-weight highly conductive graphene current collector for an aqueous battery according to claim 1, wherein the foaming agent in the step (2) is one or more selected from azodicarbonamide, polyurethane, dinitrosopentamethylenetetramine, and p-toluenesulfonylhydrazide.
7. The method for preparing a light highly conductive graphene current collector for an aqueous battery according to claim 1, wherein the standing time in the step (2) is 1 to 24 hours.
8. The method for preparing a light highly conductive graphene current collector for an aqueous battery according to claim 1, characterized by step (3).
9. A light highly conductive graphene current collector for water-based batteries produced by the production method according to any one of claims 1 to 8.
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