CN112954991B - MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof - Google Patents
MXene/metal nanowire composite material and freeze-thaw assembly method and application thereof Download PDFInfo
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- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
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Abstract
The invention discloses an MXene/metal nanowire composite material and a freeze-thaw assembly method and application thereof. The composite material comprises MXene nano-sheets with folds and metal nano-wires, wherein the metal nano-wires are wrapped and fixed by the folds of the MXene nano-sheets to form an embedded 2D/1D structure. The freeze-thaw assembly method comprises the following steps: dispersing MXene powder in water, then intercalating by at least 4 times of freezing-melting operation to obtain MXene nanosheets with wrinkles, adding metal nanowire dispersion liquid, stirring, and then performing freezing-melting operation to complete assembly. The composite material has the advantages of stable structure, high conductivity, good mechanical property and flexibility, and high electromagnetic wave absorption efficiency and reflection efficiency; the material can be automatically assembled by a simple freezing-melting method, does not need to add an activated reaction substance, is simple to operate and good in safety, and can be applied to the field of pressure sensors, electromagnetic shielding or wearable flexible devices.
Description
Technical Field
The invention belongs to the technical field of composite nano materials, and particularly relates to an MXene/metal nanowire composite material and a freeze-thaw assembly method and application thereof.
Background
MXene is a novel sheet-shaped stacked two-dimensional material, has the characteristics of the traditional two-dimensional material, is rich in types of constituent elements, has excellent performance in various fields, and is widely applied to the fields of electrochemistry, electromagnetic shielding, sensors and the like. The compound use of MXene and other materials is always the focus of research, and the composite material is important for improving the conductivity, the environmental stability and the mechanical property. The compounding of MXene and metal nanowires mainly has two modes, one mode is liquid phase and is blended in solution, but the compounding effect is not good, so that the performance is effectively improved; the other is solid phase, MXene is coated on a thin film of the metal nanowires to prepare a blended material, but the mixed material forms an interface between two phases in such a way, and certain properties of the material, such as conductivity, mechanical property, hydrophilicity and the like, are inevitably influenced in application.
Disclosure of Invention
The invention aims to provide an MXene/metal nanowire composite material, a freeze-thaw assembly method and application thereof. The composite material has the advantages of stable structure, high and stable conductivity, good mechanical property, good flexibility, free bending, high electromagnetic wave absorption efficiency and reflection efficiency; can be automatically assembled by a simple freezing-thawing method without adding any activating reaction substance, and has simple operation and good safety.
In order to solve the technical problems, the invention adopts the following technical scheme:
the MXene/metal nanowire composite material comprises MXene nanosheets with folds and metal nanowires, wherein the metal nanowires are wrapped and fixed by the folds of a plurality of MXene nanosheets to form an embedded 2D/1D structure.
According to the scheme, the mass ratio of the metal nanowire to the MXene nanosheet is 1: (1-5).
According to the scheme, the thickness of the MXene nanosheet is 1-15nm.
According to the scheme, the diameter of the metal nanowire is 30-50nm, and the length of the metal nanowire is 100-200 mu m.
According to the scheme, the metal nanowires are silver nanowires, copper nanowires, gold nanowires or tellurium nanowires; the MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Mo 2 CT x Or Nb 3 C 2 T x 。
The freeze-thaw assembly method of the MXene/metal nanowire composite material comprises the following steps:
the MXene powder is dispersed in water and then intercalated through freezing-melting operation for at least 4 times to obtain MXene nanosheets with wrinkles, and then the MXene nanosheets are added with the metal nanowire dispersion liquid and stirred and then subjected to freezing-melting operation to complete assembly, so that the MXene/metal nanowire composite material is obtained.
According to the scheme, the freezing-thawing operation comprises the following steps: gradually cooling the reaction solution to-20 to-30 ℃, freezing for 2-3 hours, taking out, and unfreezing at the temperature of 20-40 ℃. Preferably, the cooling rate is 1-3 deg.C/min.
MXene powder was intercalated by 4-6 freeze-thaw operations after dispersion in water according to the protocol described above.
According to the scheme, the concentration of the MXene powder after being dispersed in water is 1-3mg/ml.
According to the scheme, the concentration of the metal nanowire solution is 0.5-2mg/ml.
According to the scheme, the mass ratio of the metal nanowire to MXene is 1: (1-5).
According to the scheme, the metal nanowires are silver nanowires, copper nanowires, gold nanowires or tellurium nanowires.
According to the scheme, MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Mo 2 CT x Or Nb 3 C 2 T x 。
According to the scheme, the metal nanowire dispersion liquid is added and stirred for 0.5-2h, and then freezing-thawing operation is carried out to complete assembly.
The MXene/metal nanowire composite material is applied to the fields of pressure sensors, electromagnetic shielding or wearable flexible devices.
In the MXene/metal nanowire composite material provided by the invention, the metal nanowire is wrapped and fixed by folds of a plurality of MXene nanosheets to form an embedded 2D/1D structure; the MXene nanosheets are in good contact with the silver nanowires, and the composite material is stable in structure; meanwhile, the one-dimensional silver nanowires are inserted between the two-dimensional MXene material sheet layers, so that effective connection is established between the MXene sheet layers, a conductive network is established, the conductivity of the composite material is obviously improved, and the long-term stability of the conductivity is improved. The composite material has high mechanical strength, and can effectively change the MXene interlamellar spacing and the connection form of the internal conductive network through the change of pressure, thereby outputting different electric signals and playing the effect of a pressure sensor; meanwhile, the flexibility of the MXene material is not influenced, the MXene material can be freely bent, and the MXene material plays a greater role in wearable flexible devices; in addition, the good conductivity and the formation of the wrinkles on the surface of MXene are beneficial to improving the electromagnetic wave absorption efficiency and reflection efficiency of the MXene in the electromagnetic shielding field, so that the integral electromagnetic shielding efficiency is improved; the composite material can be widely applied to the field of pressure sensors, electromagnetic shielding or wearable flexible devices.
The MXene aqueous dispersion is subjected to freezing-thawing operation for multiple times, water molecules expand under freezing due to the action of hydrogen bonds during low-temperature freezing to realize delamination of the MXene, and wrinkles with different sizes are generated on the surface of the MXene under the action of expansion and extrusion of the water molecules through multiple freezing-thawing operations. And then mixing the MXene nanosheets with the folds with the metal nanowire solution, then carrying out freezing-melting operation again, embedding the silver nanowires into the folds generated on the surfaces of the MXene, so that the MXene and the metal nanowires can be automatically assembled, and the stable MXene/metal nanowire composite material is obtained, wherein the silver nanowires and the MXene form a cross-linked interpenetrating network inside, and the electrical property and the stability of the material are improved.
The invention has the beneficial effects that:
1. the MXene/metal nanowire composite material provided by the invention is of an embedded 2D/1D structure, the MXene nanosheets with folds have good contact with the silver nanowires, and a conductive network is constructed; the composite material has stable structure and high conductivity (2440S cm) -1 Pure MXene material is 1500S cm -1 ) The high-strength flexible material has high mechanical strength and good flexibility, and can be widely applied to the field of pressure sensors, electromagnetic shielding or wearable flexible devices.
2. The MXene/metal nanowire composite material with a stable structure can be obtained by layering MXene through the expansion effect of water molecules under freezing, obtaining MXene nanosheets with enough and large irregular wrinkles on the surfaces through multiple freezing-melting operations, providing a deposition space for the one-dimensional material metal nanowires, enabling the one-dimensional material metal nanowires to be more easily coated by MXene, and performing the freezing-melting operation again in the composite process to enable the MXene nanosheets and the metal nanowires to be combined more tightly; the composite material can be obtained by automatic assembly through a simple freezing-melting method, no activating reaction substance is required to be added, the purity is high, the operation is simple, the safety is good, the cost is low, and the method is suitable for industrial production.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) image of wrinkled MXene nanoplatelets prepared by freeze-thaw method in example 1.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1.
Fig. 3 is an elemental analysis (EDS) diagram of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1.
Fig. 4 is the resistance of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1.
Fig. 5 shows the resistance change of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1 within 14 days.
Detailed Description
The following examples are presented to further illustrate the present invention in order to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A freeze-thaw assembly method of an MXene/silver nanowire composite material comprises the following steps:
1) 1.6g of lithium fluoride was dissolved in 20ml of 9mol/L hydrochloric acid under stirring, and 1.2g of Ti was added 3 AlC 2 Slowly adding the mixture into the solution, transferring the mixture into an oil bath kettle, stirring the mixture at the rotating speed of 120 r/min, and heating the mixture to 35 ℃ for reaction for 24 hours; centrifuging, ultrasonic treating, vacuum filtering, drying, etc. to obtain MXene (Ti) 3 C 2 T x ) Black powder of (2).
2) Dispersing MXene powder obtained in the step 1) into a dispersion liquid with the mass concentration of 1mg/ml by using water.
3) Freezing and thawing 5ml of MXene dispersion liquid obtained in the step 2), and specifically comprises the following steps: placing into a refrigerator, gradually cooling to-20 deg.C at a speed of 2 deg.C/min, freezing for 2 hr, completely freezing to obtain ice, and melting at 25 deg.C; and repeating the freezing-melting operation for 4 times to obtain the MXene nanosheet with wrinkles.
4) Adding 1ml of silver nanowire dispersion liquid with the concentration of 1mg/ml into the MXene nanosheets subjected to freeze thawing in the step 3), stirring for one hour, repeating the freezing-thawing operation in the step 3 once, performing vacuum filtration, and performing vacuum drying to obtain the MXene/silver nanowire composite material; wherein the diameter of the silver nanowire is 30nm, and the length of the silver nanowire is 100-200 μm.
Fig. 1 is a Transmission Electron Microscope (TEM) image of wrinkled MXene nanoplatelets prepared by freeze-thaw method in example 1. The figure shows that: the freeze-thawing method can effectively form folds and recesses with different sizes on the surface of MXene, the constructed rugged morphology is favorable for compounding with a one-dimensional material, the contact area can be increased, the composite material can be in a larger contact space, and the conductivity, the environmental stability and the mechanical property of the composite material are favorably improved.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1. The figure shows that: the thickness of the MXene nanosheet is 1-15nm; the surface of the MXene nano-sheet is distributed with a plurality of folds, and the silver nano-wires are inserted between the sheet layers and are wrapped in the sheet layers; MXene and silver nano-wire have good contact, can see that one-dimensional silver nano-wire alternates between two-dimensional MXene material lamella to establish effective connection between MXene lamella. The composite material can be used as a sensor material, and can effectively change the MXene interlamellar spacing and the connection form of the internal conductive network through the change of pressure, so that different electric signals are output, and the effect of a pressure sensor is achieved.
Fig. 3 is an elemental analysis (EDS) diagram of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1. The figure shows that: the elements Ti, C, O and F contained in MXene and Ag in the silver nanowires are detected, which shows that the silver nanowires are successfully coated by the MXene.
Fig. 4 is the resistance of the MXene/silver nanowire composite prepared by the freeze-thaw method in example 1. The figure shows that: the MXene/silver nanowire composite material compounded by the freeze-thawing method constructs a conductive network, and different MXene nanosheets are connected through the silver nanowires, so that the conductivity of the composite material is improved, and the MXene/silver nanowire composite material has high conductivity of 2440S cm -1 Obviously higher than the conductivity of pure MXene material (1500S cm) -1 ) In addition, since the MXene has wrinkles and depressions of different sizes formed on the surface thereof, the incident electromagnetic wave can be effectively absorbed and reflected, thereby playing a role of shielding the electromagnetic wave. In addition, the nano composite material has low density and large specific surface area, and the characteristics are very suitable for the application in the field of electromagnetic shielding, particularly the application in the field of military science and technology as a coating.
Fig. 5 shows the resistance change of the MXene/silver nanowire composite material prepared by the freeze-thaw method in example 1 within 14 days; the figure shows that: the composite material has better stability under natural conditions, and the oxidation process is slowed probably due to the establishment of the conductive network in the composite material and the formation of the surface wrinkles, so that the stability of the conductivity of the composite material under the natural conditions is improved.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The MXene/metal nanowire composite material is characterized by comprising MXene nanosheets and metal nanowires, wherein the metal nanowires are wrapped and fixed by folds of a plurality of MXene nanosheets to form a mosaic 2D/1D structure; wherein the length of the metal nanowire is 100-200 μm.
2. The composite material according to claim 1, wherein the mass ratio of the metal nanowires to the MXene nanosheets is 1: (1-5).
3. The composite material of claim 1, wherein the MXene nanosheets are 1-15nm thick; the diameter of the metal nanowire is 30-50nm.
4. The composite material of claim 1, wherein the metal nanowires are silver nanowires, copper nanowires, gold nanowires, or tellurium nanowires; the MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Mo 2 CT x Or Nb 3 C 2 T x 。
5. The freeze-thaw assembly method of the MXene/metal nanowire composite of any one of claims 1-4, comprising the steps of:
dispersing MXene powder in water, then intercalating by at least 4 times of freezing-melting operation to obtain MXene nanosheets with wrinkles, adding metal nanowire dispersion liquid, stirring, and then performing freezing-melting operation to complete assembly to obtain the MXene/metal nanowire composite material.
6. A freeze-thaw assembly method according to claim 5, wherein the freeze-thaw operation is: gradually cooling the reaction solution to-20 to-30 ℃, freezing for 2-3 hours, taking out, and unfreezing at the temperature of 20-40 ℃.
7. A freeze-thaw assembly method according to claim 5, wherein MXene powder is intercalated by 4-6 freeze-thaw operations after being dispersed in water.
8. A freeze-thaw assembly method according to claim 5, wherein the concentration of MXene powder after dispersion in water is 1-3mg/ml; the concentration of the metal nanowire solution is 0.5-2mg/ml.
9. A freeze-thaw assembly method according to claim 5, wherein the mass ratio of the metal nanowires to MXene is 1: (1-5).
10. Use of the MXene/metal nanowire composite of any one of claims 1-4 in the field of pressure sensors, electromagnetic shielding or wearable flexible devices.
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| CN114400153A (en) * | 2022-02-25 | 2022-04-26 | 上海大学 | MXene-copper nanowire composite material for super capacitor and preparation method thereof |
| CN116574483A (en) * | 2023-05-12 | 2023-08-11 | 黑龙江工程学院 | Preparation method of tellurium nanowire multi-component composite material |
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| CN108168420A (en) * | 2017-12-26 | 2018-06-15 | 中国科学院上海硅酸盐研究所 | A kind of flexible strain transducer based on MXene materials |
| WO2019126031A1 (en) * | 2017-12-22 | 2019-06-27 | Drexel University | Crumpled mesoporous mxene powders synthesized by acid-, base-, or salt-induced crumpling |
| CN112146798A (en) * | 2020-10-08 | 2020-12-29 | 五邑大学 | Preparation method of flexible stress sensor with multi-dimensional microstructure |
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| CN111312434B (en) * | 2020-02-27 | 2021-05-04 | 北京化工大学 | Metal nanowire-based multilayer-structure transparent electromagnetic shielding film and preparation method and application thereof |
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| WO2019126031A1 (en) * | 2017-12-22 | 2019-06-27 | Drexel University | Crumpled mesoporous mxene powders synthesized by acid-, base-, or salt-induced crumpling |
| CN108168420A (en) * | 2017-12-26 | 2018-06-15 | 中国科学院上海硅酸盐研究所 | A kind of flexible strain transducer based on MXene materials |
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