CN114014306A - Preparation method and application of oxygen-enriched layered porous graphene - Google Patents
Preparation method and application of oxygen-enriched layered porous graphene Download PDFInfo
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Abstract
The invention discloses a preparation method and application of oxygen-enriched layered porous graphene, and belongs to the technical field of graphene electrodes. The preparation method of the oxygen-enriched layered porous graphene comprises the following steps: adding potassium ferrate into the graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, drying the mixed liquid, cooling to room temperature to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in an HCl solution, washing with distilled water, and freeze-drying to obtain the oxygen-enriched layered porous graphene. The oxygen-enriched layered porous graphene prepared by the method has large specific surface area and rich micropores and mesopores, lays a structural foundation for excellent electrochemical performance of an electrode sample, generates in-plane pores on a graphene sheet layer, and oxygen-containing functional groups generated around the in-plane pores can contribute additional pseudo capacitance to the total capacitance.
Description
Technical Field
The invention relates to a preparation method and application of oxygen-enriched layered porous graphene, and belongs to the technical field of graphene electrodes.
Background
Graphene shows excellent properties as a novel electrode material in many fields. However, in practical application, graphene is easy to have a serious accumulation phenomenon through van der waals force and pi-pi interaction, so that the actual specific surface area of graphene is reduced, the transmission of electrolyte ions is hindered, and the utilization rate of graphene is reduced. Aiming at the problem, a porous structure is prepared on a graphene sheet layer to provide a transmission shortcut for the electrolyte, so that the transmission of the electrolyte is effectively promoted, and the utilization rate of the graphene is improved.
In general, the performance of supercapacitors is highly dependent on the pore structure of the electrode material and the electrolyte accessible specific surface area, since the greater the surface area in contact with the electrolyte, the easier the diffusion of ions. Therefore, due to the highly open porous structure of the porous graphene, the electrolyte can contact the surface of the porous network, and the porous graphene becomes a hot spot for research on electrode materials of the super capacitor. The porous material made of graphene has obvious advantages compared with other porous carbon materials. Firstly, the excellent thermal and chemical stability of graphene enables these materials to withstand harsh environments; secondly, the gaps in the porous graphene material are beneficial to the rapid diffusion of electrolyte, and the excellent conductivity enables the porous graphene material to become an ideal current collector for rapidly transmitting carriers in a porous frame; thirdly, the high mechanical strength of the graphene with the large length-diameter ratio is beneficial to improving the stability of the porous framework and preventing the collapse or shrinkage of the porous structure; fourthly, graphene derivatives with oxygen-containing functional groups, such as Graphene Oxide (GO) and reduced graphene oxide (rGO), can serve as adsorption substrates for various organic or inorganic composite materials, providing opportunities for constructing different graphene-based porous materials. These excellent properties make porous graphene materials key components for high performance electrochemical energy storage and conversion devices (e.g., lithium ion batteries, supercapacitors). However, the existing preparation process of porous graphene is harsh in conditions and complex in preparation process, and the obtained product cannot meet the requirements of electrochemical storage and conversion with higher performance, so that the porous graphene with a larger specific surface area has important significance in the electrochemical field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method and application of oxygen-enriched layered porous graphene, wherein the graphene oxide is modified by using potassium ferrate and HCl solution, so that the prepared porous graphene has large specific surface area, rich micropores and mesopores and more excellent performance.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of oxygen-enriched layered porous graphene, which comprises the following steps: mixing potassium ferrate (K)2FeO4) Adding the mixture into Graphene Oxide (GO) dispersion liquid, uniformly mixing to obtain a mixed liquid, cooling to room temperature after the mixed liquid reacts to obtain oxygen-enriched layered porous graphene (HLGH) hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in HCl solution, washing with distilled water, and freeze-drying to obtain the oxygen-enriched layered porous graphene (HLGH).
Further, the concentration of the graphene oxide dispersion liquid is 0.5-5 mg/mL.
Further, the feed-liquid ratio of the potassium ferrate to the graphene oxide dispersion liquid is 10-50 mg: 15 mL.
Further, the reaction temperature is 100-180 ℃, and the reaction time is 6-12 h.
Further, the concentration of the HCl solution is 3-8 mol/L.
Further, the soaking time is 12-48 h.
Further, it was washed with distilled water to neutrality.
Further, freeze-drying.
The invention also provides the oxygen-enriched layered porous graphene prepared by the preparation method.
The invention also provides application of the oxygen-enriched layered porous graphene in electrode materials.
The invention discloses the following technical effects:
the invention adopts green potassium ferrate (K)2FeO4) The graphene oxide porous graphene material can be used as a pore-forming agent, so that the prepared porous graphene has a large specific surface area and abundant micropores and mesopores, and a structural foundation is laid for the excellent electrochemical performance of an electrode sample. The hydrochloric acid soaking can remove ferric oxide generated by hydrothermal reaction, in addition, an in-plane hole is generated on the graphene sheet layer, and oxygen-containing functional groups generated around the in-plane hole can contribute additional pseudo capacitance to the total capacitance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is an SEM of the oxygen-rich layered porous graphene material prepared in example 1, wherein a is an SEM image at 200nm and b is an SEM image at 10 μm;
FIG. 2 is a TEM of the oxygen-rich layered porous graphene material prepared in example 1, wherein a is a TEM image at 20nm and b is a TEM image at 5 nm;
FIG. 3 shows N of the oxygen-rich layered porous graphene material in example 1 of the present invention2Adsorption and desorption curve graphs;
FIG. 4 is a pore size distribution diagram of an oxygen-rich layered porous graphene material in example 1 of the present invention;
fig. 5 is an X-ray diffraction spectrum (XRD) of the oxygen-enriched layered porous graphene material according to example 1 of the present invention;
FIG. 6 is an X-ray photoelectron spectroscopy (XPS) of the oxygen-rich layered porous graphene material of example 1 of the present invention; wherein a is an XPS total spectrum, and b is a high-resolution O1s spectrum of the oxygen-enriched layered porous graphene material;
FIG. 7 is a cycle Curve (CV) of the oxygen-rich layered porous graphene material of example 1 of the present invention at different scan rates;
FIG. 8 is a specific capacitance graph of the oxygen-rich layered porous graphene carbon material prepared in example 1 of the present invention at different current densities;
fig. 9 is an ac impedance diagram of the oxygen-rich layered porous graphene material prepared in example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
Dispersing graphene oxide by using water to enable the concentration of the graphene oxide dispersion liquid to be 2mg/mL, adding 30mg of potassium ferrate into 15mL of the graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, transferring the mixed liquid into a 20mL Teflon-lined stainless steel high-pressure reaction kettle, placing the reaction kettle in an oven, keeping the temperature at 180 ℃ for 12 hours, cooling the reaction kettle to room temperature to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in 6mol/L HCl solution for 48 hours, repeatedly washing the hydrogel with distilled water to be neutral, and freeze-drying to obtain the oxygen-enriched layered porous graphene material.
Example 2
Dispersing graphene oxide by using water to enable the concentration of the graphene oxide dispersion liquid to be 0.5mg/mL, adding 50mg of potassium ferrate into 15mL of the graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, transferring the mixed liquid into a 20mL Teflon-lined stainless steel high-pressure reaction kettle, placing the reaction kettle in an oven, keeping the temperature of the reaction kettle at 160 ℃ for 6 hours, cooling the reaction kettle to room temperature to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in 8mol/L HCl solution for 12 hours, repeatedly washing the hydrogel with distilled water to be neutral, and freeze-drying to obtain the oxygen-enriched layered porous graphene material.
Example 3
Dispersing graphene oxide by using water to enable the concentration of the graphene oxide dispersion liquid to be 5mg/mL, adding 10mg of potassium ferrate into 15mL of the graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, transferring the mixed liquid into a 20mL Teflon-lined stainless steel high-pressure reaction kettle, placing the reaction kettle in an oven, keeping the temperature at 100 ℃ for 12 hours, cooling the reaction kettle to room temperature to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in 3mol/L HCl solution for 48 hours, repeatedly washing the hydrogel with distilled water to be neutral, and freeze-drying to obtain the oxygen-enriched layered porous graphene material.
Example 4
Dispersing graphene oxide by using water to enable the concentration of the graphene oxide dispersion liquid to be 4mg/mL, adding 20mg of potassium ferrate into 15mL of graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, transferring the mixed liquid into a 20mL Teflon-lined stainless steel high-pressure reaction kettle, placing the reaction kettle in an oven, keeping the temperature at 180 ℃ for 7 hours, cooling the reaction kettle to room temperature to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in 6mol/L HCl solution for 20 hours, repeatedly washing the hydrogel with distilled water to be neutral, and freeze-drying to obtain the oxygen-enriched layered porous graphene material.
Comparative example 1
The only difference from example 1 is that 60mg of potassium ferrate was added to 15mL of graphene oxide dispersion.
Comparative example 2
The only difference from example 1 is that the graphene oxide was dispersed with water such that the concentration of the graphene oxide dispersion was 6 mg/mL.
Comparative example 3
The only difference from example 1 is that it was placed in an oven and kept at 200 ℃ for 8 h.
Comparative example 4
The only difference is that the solution is soaked in HCl solution with concentration of 10mol/L as in example 1.
Comparative example 5
The only difference from example 1 is that the solution was soaked in HCl for 10 h.
Comparative example 6
The only difference from example 1 is that the step of washing with distilled water repeatedly to neutrality is omitted.
1. Structural characterization of oxygen-rich layered porous graphene material prepared in example 1
1.1 Transmission scanning Electron microscope analysis of oxygen-enriched layered porous graphene Material
The oxygen-rich layered porous graphene material in example 1 is characterized by its morphology by using a field emission scanning electron microscope, and its SEM photograph is shown in fig. 1, where a is an SEM image with a scale of 200nm, and b is an SEM image with a scale of 10 μm, and a macroscopically ordered layer-by-layer self-assembled structure and a three-dimensional porous structure can be clearly seen from fig. 1, and thus it belongs to layered porous graphene.
1.2 Transmission Electron microscopy analysis of oxygen-enriched layered porous graphene materials
FIG. 2 is a TEM photograph of the oxygen-rich layered porous graphene material of example 1, wherein a is a TEM image at 20nm and b is a TEM image at 5nm, and it can be seen from FIG. 2a that the material is composed of thin and wrinkled multi-layered graphene due to Fe2O3Some holes can be observed on the graphene sheet layer, and fig. 2b also proves that the material is formed by multilayer graphene nanoRice flakes.
1.3N2Adsorption and desorption analysis
FIG. 3 shows N of the oxygen-rich layered porous graphene material in example 1 of the present invention2And (3) an adsorption and desorption curve, wherein the adsorption isotherm of the sample is a mixed isotherm of type I and type IV. BET specific surface area of 556.3m2 g-1At lower specific pressure (type I, P/P)0<0.2), the adsorption amount shows a remarkable rising trend, and the existence of micropores in the material is indicated. In addition, at higher specific pressures (type IV, 0.2)<P/P0<0.9) a hysteresis loop is present, which indicates the presence of capillary condensation, which is characteristic of the presence of mesopores in the material, indicating the presence of pores of different pore sizes in the material.
Fig. 4 is a pore size distribution diagram of the oxygen-rich layered porous graphene material in example 1 of the present invention. As can be seen from FIG. 4, the micropores are mainly concentrated at 0.86nm, and the mesoporous size is between 2-10 nm. The micropores can provide larger accessible specific surface area of electrolyte, and the mesopores can provide a low-resistance channel for rapid ion migration, which indicates that the material provides structural guarantee for high-performance electrode materials.
1.4X-ray diffraction Pattern (XRD) analysis
Fig. 5 is an X-ray diffraction spectrum (XRD) of the oxygen-enriched layered porous graphene material of example 1 of the present invention. The broader diffraction peak on the XRD spectrum of the material appears at 23.1 ° 2 θ, which is attributed to the graphitic carbon (002) crystal plane. The (002) peak intensity of the material is significantly weaker and broader than that of conventional graphene gels due to the presence of in-plane pores on the randomly stacked graphene lamellae. Moreover, the (002) peak of the sample is obviously shifted to a small angle compared with the traditional graphene gel (2 theta is 24.3 degrees), which shows that the interlayer spacing (0.43nm) of the multilayer oxygen-enriched graphene material is larger than that of the traditional graphene gel (0.41nm), and the increase of the interlayer spacing is more favorable for electrolyte ions to enter between material layers, so that the accessible surface area of the electrolyte is increased.
1.5X-ray photoelectron Spectroscopy (XPS) analysis
Fig. 6 is an X-ray photoelectron spectroscopy (XPS) of the oxygen-rich layered porous graphene material of example 1 of the present invention. The XPS summary spectrum (FIG. 6a) shows a clear C1s peak (284.5eV) and a relatively weak O1s peak (532.5eV), indicating that the material is free of other impurities. Fig. 6b shows a high resolution O1s spectrum of the material, which can be decomposed into three different types of oxygen peaks, C ═ O/C (O) O (532.1eV), C — O — C (533.7eV), and — OH (535.4 eV). Experiments and calculation show that the oxygen-rich layered porous graphene material prepared in example 1 has higher total content of electrochemically active oxygen-containing functional groups than that of traditional graphene.
2. Electrochemical performance test
2.1 preparation of supercapacitor electrodes
4.7mg (85% and 15% of each of the graphene material and the acetylene black in mass percent) of the mixed solid powder of the graphene material and the acetylene black prepared in examples 1 to 4 and comparative examples 1 to 6 was added to 0.4mL of a Nafion solution with a mass fraction of 0.25 wt% to be ultrasonically dispersed to form a suspension. Then 6. mu.L of the suspension was dropped on the surface of a glassy carbon electrode by using a pipette gun, and the suspension was dried at room temperature and used for testing.
2.2 electrochemical Performance testing
The graphene materials prepared in examples 1 to 4 and comparative examples 1 to 6 are used as working electrodes, carbon rods are used as counter electrodes, and saturated calomel electrodes are used as reference electrodes to form a three-electrode system. With 1mol/L of H2SO4The solution is used as an electrolyte solution, and the potential window range is-0.3-0.7V.
Wherein, the cycling Curves (CV) of the oxygen-rich layered porous graphene of example 1 at different scan rates are shown in fig. 7. It can be seen from fig. 7 that all CV curves appear as rectangles with a pair of redox peaks, with a stronger redox peak at +0.4V, attributable to a more complete conductive network and electroactive oxygen-containing functional groups generated after etching. The CV curve of the comparative example had the same shape as that of example 1, but the background current was smaller than that of example 1.
Fig. 8 shows the specific capacitance of the oxygen-rich layered porous graphene carbon material prepared in example 1 of the present invention at different current densities. The specific capacitance of the sample was calculated to be 329.5F/g when the current density was 1A/g. The material prepared in example 1 has higher specific capacitance and potential of being used as an electrode material of a super capacitor, which is consistent with the test result of cyclic voltammetry. The specific capacitance of the comparative example is smaller than that of example 1.
FIG. 9 is an AC impedance diagram of the oxygen-rich layered porous graphene material prepared in example 1 of the present invention, wherein the frequency range is 0.01 Hz to 105 Hz. It can be seen that in the high frequency region, the intercept along the real axis on the Nyquist plot is small; in the low frequency region, the sample electrode has a more straight, oblique line, indicating. The oxygen-rich layered porous graphene material prepared in the example 1 has the advantages of fast current response, low polarization degree, fast oxidation-reduction reaction and good capacitance characteristic in the electrochemical process. Whereas the Nyquist plot of the comparative example is in the high frequency region, the intercept along the real axis is larger; in the low frequency region, the inclination of the line is large, indicating that the sample of the comparative example has high equivalent series internal resistance and diffusion resistance.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. The preparation method of the oxygen-enriched layered porous graphene is characterized by comprising the following steps of: adding potassium ferrate into the graphene oxide dispersion liquid, uniformly mixing to obtain a mixed liquid, cooling to room temperature after the mixed liquid reacts to obtain oxygen-enriched layered porous graphene hydrogel, soaking the oxygen-enriched layered porous graphene hydrogel in an HCl solution, washing with distilled water, and freeze-drying to obtain the oxygen-enriched layered porous graphene.
2. The preparation method according to claim 1, wherein the concentration of the graphene oxide dispersion liquid is 0.5-5 mg/mL.
3. The preparation method according to claim 1, wherein the feed-to-liquid ratio of the potassium ferrate to the graphene oxide dispersion is 10-50 mg: 15 mL.
4. The preparation method according to claim 1, wherein the reaction temperature is 100-180 ℃ and the reaction time is 6-12 h.
5. The method according to claim 1, wherein the concentration of the HCl solution is 3 to 8 mol/L.
6. The preparation method according to claim 1, wherein the soaking time is 12-48 h.
7. The method according to claim 1, wherein the reaction mixture is washed with distilled water to neutrality.
8. An oxygen-rich layered porous graphene prepared by the preparation method of any one of claims 1 to 7.
9. The use of the oxygen-rich layered porous graphene of claim 8 in an electrode material.
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