CN112093792B - Preparation method and application of two-dimensional hydrothermal carbon nanosheet material - Google Patents
Preparation method and application of two-dimensional hydrothermal carbon nanosheet material Download PDFInfo
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Abstract
The invention belongs to the technical field of material preparation and synthesis, in particular to a preparation method and application of a two-dimensional hydrothermal carbon nanosheet material, and aims to develop a preparation method of two-dimensional hydrothermal carbon which is simple, easy, high in controllability, environment-friendly and wide in raw material source, synthesized by hydrothermal reaction under the action of mixed aqueous solution of glucose, catalyst and ethylenediamine, the prepared hydrothermal carbon nanosheet can be used as a novel efficient photocatalyst and applied to the preparation of electronic devices such as electrochemical capacitors and the like, the method for preparing the hydrothermal carbon nanosheet by using the hydrothermal method has the advantages of simple preparation process, wide raw material source and large-scale application, develops a new method for preparing the efficient and stable carbon functional material with the nanoscale, and is favorable for promoting industrial development based on material innovation.
Description
Technical Field
The invention belongs to the technical field of preparation and synthesis of materials, and particularly relates to a preparation method and application of a two-dimensional hydrothermal carbon nanosheet material.
Background
The two-dimensional material refers to a material in which electrons can only do plane motion on a two-dimensional nanoscale (1-100 nm). The most typical two-dimensional material, which is also the first experimentally proven one, is graphene, and then some new two-dimensional materials are separated in succession, such as single-element silylene and black phosphorus, tungsten diselenide of transition metal sulfide, magnesium bromide of transition metal dihalide, MXene, metal-organic framework, covalent organic framework, perovskite, and the like. The two-dimensional material has unique photoelectric properties which are not possessed by a plurality of traditional materials, and particularly has great potential in the aspect of constructing high-performance and new-function optoelectronic devices. Meanwhile, the surface area of the material is large, the conductivity is high, the charge migration distance can be shortened, the separation of photo-generated charge carriers can be improved, and the material has wide application prospects in the fields of electrochemistry, memory storage devices, solar cells, biomedicine, polymer nano composite materials and the like.
The hydrothermal carbon (HTCC) is a solid product which is obtained by carrying out hydrothermal carbonization on cheap biomass, takes carbon as a main body and is rich in oxygen-containing functional groups, realizes high-efficiency conversion of biomass resources, and is a novel environment-friendly photocatalyst. The hydrothermal carbon material has wide application in the aspects of environmental remediation, catalyst carriers, lithium batteries, super capacitors and the like. The hydrothermal carbon contains a large number of oxygen-containing functional groups which can adsorb pollutants in the environment. Sp in hydrothermal carbon2Hybrid polyfuran structureThe obtained hydrothermal carbon has semiconductor properties, and can be applied to photocatalytic sterilization, pollutant degradation and photocatalytic water decomposition. Hydrothermal carbon, because of its high fuel ratio, is close to peat and lignite and can be used as a substitute for solid fuels. The porous hydrothermal carbon has large surface area, and the metal can be well dispersed on the hydrothermal carbon, so that agglomeration is avoided. Hydrothermal carbon, which has a parallel layered structure and spherical characteristics, is an ideal choice for electrodes, and its high volumetric capacitance makes it potentially useful for commercial applications in electrochemical capacitors.
Although two-dimensional hydrothermal carbon has potential as an effective photocatalyst and electrocatalyst, no method for preparing two-dimensional hydrothermal carbon material has been reported so far. Therefore, the development of a preparation method of the two-dimensional hydrothermal carbon, which is simple and feasible, has higher controllability, is environment-friendly and has wide raw material sources, is urgently needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a two-dimensional hydrothermal carbon nanosheet material, the preparation method is simple and convenient, the cost is low, the raw material source is wide, and a novel method for preparing a high-efficiency stable carbon functional material with nanoscale is developed.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a two-dimensional hydrothermal carbon nanosheet material, which is obtained by taking an iron oxide nanorod substrate or a silicon wafer substrate as a reaction substrate and performing hydrothermal reaction synthesis under the action of a mixed aqueous solution of glucose, a catalyst and ethylenediamine. The preparation method has the characteristics of low cost, simple operation and capability of preparing a large amount of high-performance two-dimensional hydrothermal carbon nanosheet materials.
Preferably, the preparation method of the iron oxide nanorod substrate comprises the following steps: placing the FTO glass substrate in a mixed aqueous solution of ferric chloride and sodium sulfate for hydrothermal reaction, and calcining the reaction product at high temperature to obtain the FTO glass substrate. The preparation method can obtain the high-quality iron oxide nanorod substrate.
More preferably, when the iron oxide nanorod substrate is prepared, the FTO glass substrate is ultrasonically washed before the hydrothermal reaction. Specifically, the ultrasonic washing is ultrasonic washing with ethanol and acetone alternately for 3 to 6 times.
More preferably, when the iron oxide nanorod substrate is prepared, the temperature of the hydrothermal reaction is 100-160 ℃ and the time is 5-10 hours.
More preferably, in the preparation of the iron oxide nanorod substrate, the concentration of the ferric chloride is 0.2-33.3 mg/mL and the concentration of the sodium sulfate is 3.3-26.7 mg/mL in the mixed aqueous solution of the ferric chloride and the sodium sulfate.
More preferably, when the iron oxide nanorod substrate is prepared, the reaction product is washed and then calcined at high temperature. Specifically, the washing is performed 3 to 6 times by alternately washing with ethanol and distilled water.
More preferably, the high-temperature calcination temperature is 600-1000 ℃ and the time is 8-20 min when the iron oxide nanorod substrate is prepared.
Preferably, when the two-dimensional hydrothermal carbon nanosheet material is prepared, the temperature of the hydrothermal reaction is 120-400 ℃, and the time is 8-15 h.
Preferably, when the two-dimensional hydrothermal carbon nanosheet material is prepared, in the mixed aqueous solution of glucose, the catalyst and ethylenediamine, the concentration of glucose is 2.0-53.3 mg/mL, the concentration of the catalyst is 0.4-13.3 mg/mL, and the concentration of ethylenediamine is 0.8-13.3%.
Preferably, when the two-dimensional hydrothermal carbon nano sheet material is prepared, the catalyst includes but is not limited to ferric chloride, cobalt sulfate and nickel sulfate.
Preferably, when the two-dimensional hydrothermal carbon nanosheet material is prepared, a reaction product of the hydrothermal reaction needs to be washed and dried to obtain the two-dimensional hydrothermal carbon nanosheet material. Specifically, the washing is carried out for 3 to 6 times by alternately washing with ethanol and distilled water, and the drying is carried out for 12 to 36 hours at the temperature of 60 to 90 ℃ in vacuum.
The invention also provides a two-dimensional hydrothermal carbon nanosheet material prepared by the preparation method.
The invention also provides application of the two-dimensional hydrothermal carbon nanosheet material prepared by the preparation method in preparation of electrochemical capacitors. The electrochemical capacitor comprises a catalyst carrier, a lithium battery, a super capacitor and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a two-dimensional hydrothermal carbon nanosheet material, which is characterized in that an iron oxide nanorod substrate or a silicon wafer substrate is used as a reaction substrate and is synthesized through hydrothermal reaction under the action of mixed aqueous solution of glucose, a catalyst and ethylenediamine, and the prepared hydrothermal carbon nanosheet can be used as a novel efficient photocatalyst and is applied to preparation of electronic devices such as electrochemical capacitors.
Drawings
Fig. 1 is a transmission electron microscope image and an atomic force microscope image of hydrothermal carbon nanosheets prepared in example 1;
FIG. 2 is C of hydrothermal carbon nanosheets prepared in example 113A solid-state nuclear magnetic resonance image (a), a Raman spectrum image (b) and an ultraviolet-visible diffuse reflection spectrum image (c);
fig. 3 is an optical photograph of the hydrothermal silicon wafer-based carbon nanoplatelets prepared in example 2;
fig. 4 is a transmission electron micrograph of hydrothermal carbon nanoplates prepared in example 3;
fig. 5 is a transmission electron micrograph of hydrothermal carbon nanoplates prepared in example 4;
fig. 6 is a transmission electron micrograph of hydrothermal carbon nanoplates prepared in example 5;
fig. 7 is a transmission electron micrograph of hydrothermal carbon nanoplates prepared in example 6.
Detailed Description
The following further describes embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Unless otherwise indicated, the reagents, methods, apparatus and equipment used in the following examples are conventional in the art.
Example 1 preparation of two-dimensional hydrothermal carbon nanosheet material using iron oxide nanorod substrate
(1) Weighing 70mg of ferric chloride (3.5mg/mL) and 140mg of sodium sulfate (7.0mg/mL) in 20mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 10min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(2) ultrasonically washing the FTO glass substrate for 5 times by using ethanol and acetone alternately, and putting the FTO glass substrate into the mixed aqueous solution of the reaction kettle in the step (1) for hydrothermal reaction at the reaction temperature of 120 ℃ for 6 hours;
(3) and (3) taking the reaction product obtained in the step (2) as an FTO glass substrate with a yellow surface film, alternately washing the FTO glass substrate with ethanol and distilled water for 5 times, then calcining the product at 800 ℃ for 10min, and taking out the calcined product to obtain the iron oxide nanorod substrate.
(4) Weighing 300mg of glucose (15mg/mL) and 10mg of ferric chloride (0.5mg/mL) and dissolving in 0.5mL of ethylenediamine (2.5%) and 20mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 10min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(5) immersing the iron oxide nanorod substrate obtained in the step (3) into the mixed aqueous solution of the reaction kettle in the step (4) for hydrothermal reaction, wherein the iron oxide nanorod substrate is vertically upward during the hydrothermal reaction, the reaction temperature is 210 ℃, and the temperature is kept for 10 hours;
(6) and (3) alternately washing the reaction product obtained in the step (5) for 5 times by using distilled water and ethanol, finally placing the sample in a vacuum drying oven at 60 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the iron oxide nanorod substrate.
The two-dimensional hydrothermal carbon nanosheet prepared in example 1 was subjected to electron microscope scanning, and the result is shown in fig. 1. The thickness of the prepared hydrothermal carbon nano sheet is 2.07nm, about 10 layers are formed, the thickness of a single layer is about 0.33nm, and the agglomeration phenomenon does not occur. From fig. 2, it can be seen that the prepared hydrothermal carbon nanosheet has a polyfuran structure and a wider absorption wavelength range.
Example 2 preparation of two-dimensional hydrothermal carbon nanosheet material using silicon wafer substrate
(1) Weighing 400mg of glucose (19.05mg/mL) and 20mg of ferric chloride (0.95mg/mL) and dissolving in 1mL of ethylenediamine (4.76%) and 21mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 13min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(2) immersing a silicon wafer into the mixed aqueous solution in the reaction kettle in the step (1) to carry out hydrothermal reaction, wherein the silicon wafer is vertically upward in the reaction, the reaction temperature is 260 ℃, and the temperature is kept for 12 hours;
(3) and (3) alternately washing the reaction product obtained in the step (2) with distilled water and ethanol for 4 times, finally placing the sample in a vacuum drying oven at 65 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the silicon wafer substrate.
The two-dimensional hydrothermal carbon nanosheet of example 2 is photographed optically, and the result is shown in fig. 3, which indicates that the hydrothermal carbon of the two-dimensional hydrothermal carbon nanosheet material prepared by using the silicon wafer as the substrate uniformly and completely covers the silicon wafer, and can be effectively peeled from the nanorod.
Example 3 preparation of iron oxide nanorod substrate-based two-dimensional hydrothermal carbon nanosheet material under the action of cobalt catalyst
(1) Weighing 80mg of ferric chloride (3.8mg/mL) and 150mg of sodium sulfate (7.1mg/mL) in 21mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 12min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(2) ultrasonically washing the FTO glass substrate for 6 times by using ethanol and acetone alternately, and putting the FTO glass substrate into the mixed aqueous solution of the reaction kettle in the step (1) for hydrothermal reaction at the reaction temperature of 125 ℃ for 7 hours;
(3) and (3) taking the reaction product obtained in the step (2) as an FTO glass substrate with a yellow surface film, alternately washing the FTO glass substrate with ethanol and distilled water for 6 times, then placing the product at 850 ℃ for calcining for 15min, and taking out the product to obtain the iron oxide nanorod substrate.
(4) Weighing 350mg of glucose (17.5mg/mL) and 12mg of cobalt sulfate (0.6mg/mL) and dissolving in 0.6mL of ethylenediamine (3%) and 20mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 8min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(5) immersing the iron oxide nanorod substrate obtained in the step (3) into the mixed aqueous solution of the reaction kettle in the step (4) for hydrothermal reaction, wherein the iron oxide nanorod substrate is vertically upward during the hydrothermal reaction, the reaction temperature is 280 ℃, and the temperature is kept for 11 hours;
(6) and (3) alternately washing the reaction product obtained in the step (5) with distilled water and ethanol for 6 times, finally placing the sample in a vacuum drying oven at 70 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the iron oxide nanorod substrate under the action of the cobalt catalyst.
The hydrothermal carbon nanosheet based on the iron oxide nanorod substrate, prepared in example 3, is subjected to electron microscope scanning, and the result is shown in fig. 4, wherein cobalt ions can successfully replace the catalytic action of iron ions, so that hydrothermal carbon is assisted to grow on the iron oxide nanorod to form a two-dimensional hydrothermal carbon material.
Example 4 preparation of two-dimensional hydrothermal carbon nanosheet material based on silicon wafer substrate under the action of nickel catalyst
(1) Weighing 480mg of glucose (24mg/mL) and 12mg of nickel sulfate (0.6mg/mL) and dissolving in 0.8mL of ethylenediamine (4%) and 20mL of deionized water, uniformly mixing at room temperature to obtain a mixed aqueous solution, stirring for 12min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(2) immersing a silicon wafer into the mixed aqueous solution in the reaction kettle in the step (1) to carry out hydrothermal reaction, wherein the silicon wafer is vertically upward in the reaction, the reaction temperature is 300 ℃, and the temperature is kept for 13 hours;
(3) and (3) alternately washing the reaction product obtained in the step (2) with distilled water and ethanol for 4 times, finally placing the sample in a vacuum drying oven at 75 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the silicon wafer substrate under the action of the nickel catalyst.
The hydrothermal carbon nanosheet prepared in example 4 was subjected to electron microscope scanning, and the results are shown in fig. 5. The nickel ions can also successfully replace the catalytic action of iron ions to assist the growth of hydrothermal carbon on a silicon wafer to form a two-dimensional hydrothermal carbon material.
Example 5 preparation of iron oxide nanorod substrate-based two-dimensional hydrothermal carbon nanosheets at different glucose dosages
(1) Weighing 85mg of ferric chloride (3.5mg/mL) and 185mg of sodium sulfate (7.7mg/mL) in 24mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 15min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(2) ultrasonically washing the FTO glass substrate for 5 times by using ethanol and acetone alternately, and putting the FTO glass substrate into the mixed aqueous solution of the reaction kettle in the step (1) for hydrothermal reaction at the reaction temperature of 160 ℃ for 8 hours;
(3) and (3) taking the reaction product obtained in the step (2) as an FTO glass substrate with a yellow surface film, alternately washing the FTO glass substrate with ethanol and distilled water for 5 times, then placing the product at 900 ℃ for calcining for 15min, and taking out the product to obtain the iron oxide nanorod substrate.
(4) Weighing 100mg, 300mg and 500mg of glucose (5mg/mL, 15mg/mL and 25mg/mL) and 10mg of ferric chloride (0.5mg/mL) and dissolving in 2mL of ethylenediamine (10%) and 20mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 15min, and transferring to a 25mL Teflon hydrothermal reaction kettle;
(5) immersing the iron oxide nanorod substrate obtained in the step (3) into the mixed aqueous solution of the reaction kettle in the step (4) for hydrothermal reaction, wherein the iron oxide nanorod substrate is vertically upward during the hydrothermal reaction, the reaction temperature is 350 ℃, and the temperature is kept for 15 hours;
(6) and (3) alternately washing the reaction product obtained in the step (5) for 5 times by using distilled water and ethanol, finally placing the sample in a vacuum drying oven at 90 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the iron oxide nanorod substrate, which is prepared under different glucose consumption.
As shown in fig. 6, when the hydrothermal carbon nanosheet prepared in example 5 is subjected to electron microscope scanning, a small amount of hydrothermal carbon nanosheet is formed when the amount of glucose is insufficient, and aggregation occurs in some regions of the hydrothermal carbon nanosheet network due to excessive glucose, and the optimal amount of glucose is 300 mg.
Example 6 preparation of iron oxide nanorod substrate-based two-dimensional hydrothermal carbon nanosheet material with varying amounts of catalyst
(1) Weighing 75mg of ferric chloride (4.2mg/mL) and 125mg of sodium sulfate (6.9mg/mL) in 18mL of deionized water, uniformly mixing at room temperature to obtain a mixed water solution, stirring for 8min, and transferring to a 20mL Teflon hydrothermal reaction kettle;
(2) ultrasonically washing the FTO glass substrate for 6 times by using ethanol and acetone alternately, and putting the FTO glass substrate into the mixed aqueous solution of the reaction kettle in the step (1) for hydrothermal reaction at the reaction temperature of 115 ℃ for 7 hours;
(3) and (3) taking the reaction product obtained in the step (2) as an FTO glass substrate with a yellow surface film, alternately washing the FTO glass substrate with ethanol and distilled water for 6 times, then placing the product at 780 ℃ for calcining for 12min, and taking out the product to obtain the iron oxide nanorod substrate.
(4) 380mg of glucose (16.5mg/mL), 10mg, 50mg and 100mg of ferric chloride (0.43mg/mL, 2.2mg/mL and 4.3mg/mL) are weighed and dissolved in 1.5mL of ethylenediamine (6.5%) and 23mL of deionized water, and the mixture is uniformly mixed at room temperature to obtain a mixed water solution, stirred for 15min and then transferred to a 25mL Teflon hydrothermal reaction kettle;
(5) immersing the iron oxide nanorod substrate obtained in the step (3) into the mixed aqueous solution of the reaction kettle in the step (4) for hydrothermal reaction, wherein the iron oxide nanorod substrate is vertically upward in the reaction, the reaction temperature is 400 ℃, and the temperature is kept for 12 hours;
(6) and (3) alternately washing the reaction product obtained in the step (5) with distilled water and ethanol for 6 times, finally placing the sample in a vacuum drying oven at 80 ℃ for overnight drying, and taking out to obtain the two-dimensional hydrothermal carbon nanosheet based on the iron oxide nanorod substrate under different catalyst dosage.
The hydrothermal carbon nanosheet prepared in example 6 was subjected to electron microscope scanning, and as a result, as shown in fig. 7, the morphology of the hydrothermal carbon nanosheet was almost unchanged with the increase of the iron ion amount, but the thickness of the hydrothermal carbon nanosheet slightly increased (the average value was increased from 2.8nm to 4.1nm), which indicates that the hydrothermal process is enhanced.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (7)
1. A preparation method of a two-dimensional hydrothermal carbon nanosheet material is characterized in that an iron oxide nanorod substrate or a silicon wafer substrate is used as a reaction substrate and is synthesized through a hydrothermal reaction under the action of a mixed aqueous solution of glucose, a catalyst and ethylenediamine, the concentration of the glucose is 2.0-53.3 mg/mL, the concentration of the catalyst is 0.4-13.3 mg/mL, the concentration of the ethylenediamine is 0.8-13.3%, the catalyst is one of ferric chloride, cobalt sulfate and nickel sulfate, the temperature of the hydrothermal reaction is 120-400 ℃, and the time is 8-15 hours.
2. The preparation method of the two-dimensional hydrothermal carbon nanosheet material as claimed in claim 1, wherein the preparation method of the iron oxide nanorod substrate comprises: placing the FTO glass substrate in a mixed aqueous solution of ferric chloride and sodium sulfate for hydrothermal reaction, and calcining a reaction product at a high temperature of 600-1000 ℃.
3. The method according to claim 2, wherein the FTO glass substrate is ultrasonically washed before the hydrothermal reaction.
4. The method for preparing a two-dimensional hydrothermal carbon nanosheet material according to claim 2, wherein the hydrothermal reaction is carried out at a temperature of 100-160 ℃ for a period of 5-10 hours.
5. The method for preparing a two-dimensional hydrothermal carbon nanosheet material according to claim 2, wherein in the mixed aqueous solution of ferric chloride and sodium sulfate, the concentration of ferric chloride is 0.2-33.3 mg/mL and the concentration of sodium sulfate is 3.3-26.7 mg/mL.
6. The two-dimensional hydrothermal carbon nanosheet material prepared by the preparation method of any one of claims 1 to 5.
7. Use of the two-dimensional hydrothermal carbon nanosheet material of claim 6 in the preparation of an electrochemical capacitor.
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