CN113355718A - MXene/GO composite coating and preparation method and application thereof - Google Patents

MXene/GO composite coating and preparation method and application thereof Download PDF

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Publication number
CN113355718A
CN113355718A CN202110635660.7A CN202110635660A CN113355718A CN 113355718 A CN113355718 A CN 113355718A CN 202110635660 A CN202110635660 A CN 202110635660A CN 113355718 A CN113355718 A CN 113355718A
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mxene
composite coating
preparation
coating
deposition
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李章朋
苗晓南
王金清
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Qingdao Center Of Resource Chemistry & New Materials (qingdao Research Development Center Lanzhou Institute Of Chemical Physics Chinese Academy Of Sciences)
Lanzhou Institute of Chemical Physics LICP of CAS
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Qingdao Center Of Resource Chemistry & New Materials (qingdao Research Development Center Lanzhou Institute Of Chemical Physics Chinese Academy Of Sciences)
Lanzhou Institute of Chemical Physics LICP of CAS
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Priority to CN202110635660.7A priority Critical patent/CN113355718A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/02Electrophoretic coating characterised by the process with inorganic material
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/20Pretreatment

Abstract

The invention provides an MXene/GO composite coating and a preparation method and application thereof, belonging to the technical field of nano composite materials. The method comprises the following steps: dispersing MXene and graphene oxide in water to obtain an MXene/GO mixed solution; carrying out electrophoretic deposition by taking the polar plates as a cathode and an anode and the MXene/GO mixed solution as a deposition medium to obtain a deposition coating; and drying the deposited coating to obtain the MXene/GO composite coating. The MXene/GO composite coating prepared by the electrophoretic deposition method is uniform and flat in surface and controllable in thickness, and meanwhile, under the action of an electric field, the MXene and GO with negative charges are combined with a polar plate more firmly, so that the MXene/GO composite coating has excellent antifriction and wear resistance performances, and a high-quality composite coating can be obtained quickly.

Description

MXene/GO composite coating and preparation method and application thereof
Technical Field
The invention relates to the technical field of nano composite materials, in particular to an MXene/GO composite coating and a preparation method and application thereof.
Background
Since the discovery of graphene, two-dimensional materials show excellent physical, chemical, electronic and optical properties due to their unique two-dimensional layered structures, and have wide application prospects in the fields of energy storage, catalysis, sensors, optoelectronic devices, and the like. Graphene Oxide (GO) is an important derivative of graphene, has a graphene-like structure, and has rich oxygen-containing functional groups on the surface, such as hydroxyl, carbonyl, carboxyl and the like. Due to the existence of the functional groups, the surface of GO is negatively charged, the defect of poor hydrophilicity of the graphene material is overcome, and the GO is favorably modified.
In recent years, a novel two-dimensional material MXene has attracted much attention. MXene is the generic term for transition metal carbides, nitrides or carbonitrides, which are obtained by etching MAX precursors with hydrofluoric acid. General expression for MXene is Mn+1XnTxWherein M is a transition metal element, X is a carbon element or a nitrogen element, and T is a surface group, such as-F, -OH, and ═ O. MXene has a graphene-like structure, low shear strength and self-lubricating property, is widely used as a solid lubricant, a lubricating oil additive and a phase-reinforced material, and has a wide application prospect in the friction field.
Surface coating is a common method when two-dimensional materials are used as solid lubricants. The surface coatings commonly used today are prepared by drop casting, spin coating, spray coating and layer-by-layer self-assembly. However, these methods have disadvantages that the production process takes a long time and the resulting coating layer has poor adhesion to the substrate.
Disclosure of Invention
In view of the above, the present invention aims to provide an MXene/GO composite coating, and a preparation method and an application thereof. The invention utilizes electrophoretic deposition to ensure that MXene and GO are combined with the polar plate more firmly, and the polar plate has excellent antifriction and wear-resistant performances and simple preparation process.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an MXene/GO composite coating, which comprises the following steps:
dispersing MXene and graphene oxide in water to obtain an MXene/GO mixed solution;
carrying out electrophoretic deposition by taking the polar plates as a cathode and an anode and the MXene/GO mixed solution as a deposition medium to obtain a deposition coating;
and drying the deposited coating to obtain the MXene/GO composite coating.
Preferably, the total concentration of the MXene/GO mixed solution is 1 mg/mL.
Preferably, the mass ratio of MXene to graphene oxide is 1: 1.5-1.5: 1.
Preferably, the MXene is etched in Ti by acid and fluorine salt3AlC2The acid is hydrochloric acid, and the fluorine salt is LiF.
Preferably, the graphene oxide is prepared by a modified Hummers method.
Preferably, the voltage of the electrophoretic deposition is 30-40V, and the time is 20-40 min.
Preferably, the plate is a silicon wafer, and the silicon wafer is further treated by a piranha solution before use.
Preferably, the dispersion is carried out under the condition of ultrasound, the power of the ultrasound is 32-40 KHz, and the time is 30-60 min.
The invention also provides the MXene/GO composite coating prepared by the preparation method in the technical scheme.
The invention also provides application of the MXene/GO composite coating in the technical scheme in the field of friction lubrication.
The invention provides a preparation method of an MXene/GO composite coating, which comprises the following steps: dispersing MXene and graphene oxide in water to obtain an MXene/GO mixed solution; carrying out electrophoretic deposition by taking the polar plates as a cathode and an anode and the MXene/GO mixed solution as a deposition medium to obtain a deposition coating; and drying the deposited coating to obtain the MXene/GO composite coating. The invention provides a method for quickly and simply preparing an MXene/GO composite coating, wherein the surface of an MXene nanosheet has negative charges, the GO has a negative Zeta potential in an aqueous solution, a constant voltage is applied between two polar plates through an electrophoretic deposition technology so as to generate a constant electric field, and under the action of the constant electric field, two materials can move towards the same direction, so that the two materials can be simultaneously deposited on the same conductive substrate, so that the MXene and GO are well compounded. The electrophoretic deposition method provided by the invention is convenient to operate, simple in process, easy to obtain required experimental equipment and experimental conditions, environment-friendly and environment-friendly, and avoids pollution to the environment.
Drawings
FIG. 1 is an optical picture of an MXene/GO composite coating prepared in example 1;
fig. 2 is a scanning electron microscope image (surface and cross-section) of the MXene/GO composite coating prepared in example 1, wherein the inset is a scanning electron microscope image of the cross-section;
FIG. 3 is a change curve of the friction coefficient of MXene/GO composite coatings prepared in examples 1-3 with time;
fig. 4 is a graph of the coefficient of friction versus time for the MXene/GO composite coatings prepared in examples 4 and 5.
Detailed Description
The invention provides a preparation method of an MXene/GO composite coating, which comprises the following steps;
dispersing MXene and graphene oxide in water to obtain an MXene/GO mixed solution;
carrying out electrophoretic deposition by taking the polar plates as a cathode and an anode and the MXene/GO mixed solution as a deposition medium to obtain a deposition coating;
and drying the deposited coating to obtain the MXene/GO composite coating.
MXene and graphene oxide are dispersed in water to obtain an MXene/GO mixed solution.
In the invention, the total concentration of the MXene/GO mixed solution is preferably 1 mg/mL.
In the invention, the preferable mass ratio of MXene to graphene oxide is 1: 1.5-1.5: 1, and more preferably 1:1.5, 1.5:1 or 1:1.
In the present invention, the MXene is preferably used to etch Ti with acid and fluoride salt3AlC2Preferably, the acid is hydrochloric acid and the fluoride salt is LiF. In the present invention, the concentration of the hydrochloric acid is preferably 6 mol/L. The specific preparation method of MXene is not particularly limited in the present invention, and can be performed by a method well known to those skilled in the art.
In the present invention, the graphene oxide is preferably prepared by a modified Hummers method. The specific preparation method of the graphene oxide is not particularly limited, and can be performed by a method known to those skilled in the art.
In the present invention, the water is preferably ultrapure water.
In the invention, the dispersion is preferably carried out under the condition of ultrasound, the power of the ultrasound is preferably 32-40 KHz, and the time is preferably 30-60 min.
After the MXene/GO mixed solution is obtained, the invention takes the polar plate as the cathode and the anode, and takes the MXene/GO mixed solution as the deposition medium to carry out electrophoretic deposition, thus obtaining the deposition coating.
In the invention, the voltage of the electrophoretic deposition is preferably 30-40V, more preferably 35V, and the time is preferably 20-40 min, more preferably 25-35 min, and most preferably 30 min.
In the invention, the power supply used in the electrophoretic deposition is preferably a direct current power supply, and the distance between the cathode and the anode is preferably 10-15 mm.
In the present invention, the plate is preferably a silicon wafer, which preferably further comprises a treatment with a piranha solution before use. In the present invention, the time of the treatment is preferably 30 min. In the invention, the surface of the silicon wafer can be provided with hydroxyl by using the piranha solution.
In the present invention, the size of the silicon wafer is preferably 2cm × 1 cm.
After the deposition coating is obtained, the MXene/GO composite coating is obtained by drying the deposition coating.
In the invention, the drying temperature is preferably 20-30 ℃, more preferably 25 ℃, and the time is preferably 3-5 h, more preferably 4 h.
The invention also provides the MXene/GO composite coating prepared by the preparation method in the technical scheme.
The invention also provides application of the MXene/GO composite coating in the technical scheme in the field of friction lubrication.
To further illustrate the present invention, the MXene/GO composite coating provided by the present invention, its preparation method and application are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1:
step one, dispersing MXene and GO in ultrapure water, and performing ultrasonic treatment for 30min at the ultrasonic power of 40KHz to obtain a uniformly mixed MXene/GO solution with the concentration of 1mg/mL, wherein the mass ratio of MXene to GO is 1:1.
And step two, soaking the monocrystalline silicon wafer in a piranha solution (concentrated sulfuric acid: 30% hydrogen peroxide: 7:3(V: V)) for 30 min. And taking the treated silicon wafer as a cathode and an anode, wherein the distance between the cathode and the anode bipolar plate is 15mm, and carrying out electrophoretic deposition for 30min under the voltage of 35V by using the mixed solution of MXene/GO as a deposition medium.
And step three, drying the deposited coating at 25 ℃ for 4h to obtain the MXene/GO composite coating with the ratio of MXene to GO being 1:1.
FIG. 1 is an optical picture of an MXene/GO composite coating prepared in example 1; fig. 2 is a scanning electron microscope image (surface and cross section) of the MXene/GO composite coating prepared in example 1, and the inset in fig. 2 is a scanning electron microscope image of the cross section.
Example 2:
step one, dispersing MXene and GO in ultrapure water, and performing ultrasonic treatment for 30min at the ultrasonic power of 40KHz to obtain a uniformly mixed MXene/GO solution with the concentration of 1mg/mL, wherein the mass ratio of MXene to GO is 1.5: 1.
And step two, soaking the monocrystalline silicon wafer in a piranha solution (concentrated sulfuric acid: 30% hydrogen peroxide: 7:3(V: V)) for 30 min. And taking the treated silicon wafer as a cathode and an anode, wherein the distance between the cathode and the anode bipolar plate is 15mm, and carrying out electrophoretic deposition for 30min under the voltage of 35V by using the mixed solution of MXene/GO as a deposition medium.
And step three, drying the deposited coating at room temperature of 25 ℃ for 4 hours to obtain the MXene/GO composite coating with the ratio of MXene to GO being 1.5: 1.
Example 3:
step one, dispersing MXene and GO in ultrapure water, and performing ultrasonic treatment for 30min at the ultrasonic power of 40KHz to obtain a uniformly mixed MXene/GO solution with the concentration of 1mg/mL, wherein the mass ratio of MXene to GO is 1: 1.5.
And step two, soaking the monocrystalline silicon wafer in a piranha solution (concentrated sulfuric acid: 30% hydrogen peroxide: 7:3(V: V)) for 30 min. And taking the treated silicon wafer as a cathode and an anode, wherein the distance between the cathode and the anode bipolar plate is 15mm, and carrying out electrophoretic deposition for 30min under the voltage of 35V by using the mixed solution of MXene/GO as a deposition medium.
And step three, drying the deposited coating at room temperature of 25 ℃ for 4 hours to obtain the MXene/GO composite coating with the ratio of MXene to GO being 1: 1.5.
The change of the friction coefficient of the MXene/GO composite coatings prepared in examples 1-3 with time is shown in FIG. 3. As can be seen from FIG. 3, the MXene/GO composite coating prepared by the electrophoretic deposition method has excellent friction performance. At the same time, the ratio of MXene to GO also has a significant impact on the friction performance of the composite coating, wherein when MXene: GO is 1:1 (example 1), the friction coefficient is the lowest, and the average friction coefficient is reduced by 5.6% and 31.8% compared with the average friction coefficient of the coatings prepared in examples 2 and 3, respectively.
Example 4:
step one, dispersing MXene and GO in ultrapure water, and performing ultrasonic treatment for 30min at the ultrasonic power of 40KHz to obtain a uniformly mixed MXene/GO solution with the concentration of 1mg/mL, wherein the mass ratio of MXene to GO is 1:1.
And step two, soaking the monocrystalline silicon wafer in a piranha solution (concentrated sulfuric acid: 30% hydrogen peroxide: 7:3(V: V)) for 30 min. And taking the treated silicon wafer as a cathode and an anode, wherein the distance between the cathode and the anode bipolar plate is 10mm, and carrying out electrophoretic deposition for 20min under the voltage of 30V by using the mixed solution of MXene/GO as a deposition medium.
And step three, drying the deposited coating at the temperature of 30 ℃ for 3h to obtain the MXene/GO composite coating.
Example 5:
step one, dispersing MXene and GO in ultrapure water, and performing ultrasonic treatment for 60min at the ultrasonic power of 32KHz to obtain a uniformly mixed MXene/GO solution with the concentration of 1mg/mL, wherein the mass ratio of MXene to GO is 1:1.
And step two, soaking the monocrystalline silicon wafer in a piranha solution (concentrated sulfuric acid: 30% hydrogen peroxide: 7:3(V: V)) for 30 min. And taking the treated silicon wafer as a cathode and an anode, wherein the distance between the cathode and the anode bipolar plate is 15mm, and carrying out electrophoretic deposition for 40min under the voltage of 40V by using the mixed solution of MXene/GO as a deposition medium.
And step three, drying the deposited coating at the temperature of 20 ℃ for 5 hours to obtain the MXene/GO composite coating.
The friction coefficient of MXene/GO composite coatings prepared in examples 4 and 5 is shown in FIG. 4 with time. As can be seen from FIG. 4, the friction performance of the MXene/GO composite coating prepared under different voltages is different, the MXene/GO composite coating prepared under the voltage of 30V fails at 300s, and the MXene/GO composite coating prepared under the voltage of 40V still stably operates at 1000 s. The difference in friction properties is mainly manifested in the bearing time, and the friction coefficient does not differ much during smooth running, which may be related to the thickness of the obtained coating at different voltages.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (10)

1. A preparation method of an MXene/GO composite coating is characterized by comprising the following steps:
dispersing MXene and graphene oxide in water to obtain an MXene/GO mixed solution;
carrying out electrophoretic deposition by taking the polar plates as a cathode and an anode and the MXene/GO mixed solution as a deposition medium to obtain a deposition coating;
and drying the deposited coating to obtain the MXene/GO composite coating.
2. The preparation method of claim 1, wherein the total concentration of the MXene/GO mixed solution is 1 mg/mL.
3. The preparation method of claim 1 or 2, wherein the mass ratio of MXene to graphene oxide is 1: 1.5-1.5: 1.
4. The method according to claim 1 or 2, wherein the MXene is subjected to acid and villiaumite etching to etch Ti3AlC2The acid is hydrochloric acid, and the fluorine salt is LiF.
5. The production method according to claim 1, wherein the graphene oxide is produced by a modified Hummers method.
6. The preparation method according to claim 1, wherein the voltage of the electrophoretic deposition is 30-40V, and the time is 20-40 min.
7. The method of claim 1, wherein the plate is a silicon wafer, and the silicon wafer further comprises a treatment with a piranha solution before use.
8. The preparation method according to claim 1, wherein the dispersion is carried out under ultrasonic conditions, wherein the ultrasonic power is 32-40 KHz and the ultrasonic time is 30-60 min.
9. MXene/GO composite coating prepared by the preparation method of any one of claims 1 to 8.
10. Use of the MXene/GO composite coating of claim 9 in the field of friction lubrication.
CN202110635660.7A 2021-06-08 2021-06-08 MXene/GO composite coating and preparation method and application thereof Pending CN113355718A (en)

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CN116618266A (en) * 2023-05-30 2023-08-22 中国科学院兰州化学物理研究所 Wear-resistant and corrosion-resistant composite coating and preparation method and application thereof

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CN113800519A (en) * 2021-10-19 2021-12-17 中国科学院兰州化学物理研究所 Preparation method and application of MXene-based composite lubricating coating
CN114551888A (en) * 2022-04-26 2022-05-27 北京三川烯能科技有限公司 Method for inhibiting lithium precipitation of lithium ion battery negative electrode, slurry, negative electrode, battery and vehicle
CN114957915A (en) * 2022-05-11 2022-08-30 西安理工大学 Preparation method of graphene/MXene/epoxy resin composite material
CN116618266A (en) * 2023-05-30 2023-08-22 中国科学院兰州化学物理研究所 Wear-resistant and corrosion-resistant composite coating and preparation method and application thereof
CN116618266B (en) * 2023-05-30 2024-02-20 中国科学院兰州化学物理研究所 Wear-resistant and corrosion-resistant composite coating and preparation method and application thereof

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