Synthesis method of conductive gel applied at extremely low temperature
By introducing MXene conductive fillers and catalysts into the hydrogel, combined with specific solvents and reaction conditions, a flexible conductive hydrogel film with high sensitivity and anti-expansion characteristics under a hydration environment was prepared, solving the swelling and signal of the sensor in water. The problem of degeneration is suitable for health monitoring applications.
Patent Information
- Application Number
- CN202310693369.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-13
- Publication Date
- 2024-12-13
AI Technical Summary
Existing hydrogel sensors are prone to swelling in a hydrated environment, resulting in deformation, distortion or irreversible degradation of the output signal, and it is difficult to maintain high sensitivity and anti-expansion characteristics in water.
Using MXene as a conductive filler and catalyst, combined with acrylamide, agar, ammonium persulfate and other materials, a flexible conductive hydrogel film was prepared in binary solvents, and a single layer of MXene nanosheets were obtained through ultrasonic treatment and freeze-drying, and in an oven The reaction is heated to form a hydrogel.
The high sensitivity and anti-expansion characteristics of hydrogels under extremely low temperature conditions are achieved, and the stable sensing performance and conductivity in a hydrated environment is maintained, which is suitable for wearable display health monitoring.
Smart Images
Figure HSA0000297059840000011 
Figure HSA0000297059840000021 
Figure HSA0000297059840000031
Abstract
Description
Technical Field
[0001] The present invention relates to a method for synthesizing a conductive gel for extremely low temperature applications, specifically to a method for synthesizing MXene and a method for preparing a flexible binary solvent conductive hydrogel thereof, and belongs to the field of intelligent wearable devices. Background Art
[0002] Smart technologies based on responsive hydrogels hold great promise for future mechanical engineering applications such as soft robotics and energy storage. This is due to their unique solid-like mechanical elasticity and liquid-like transport behavior. In particular, the hydrogel wearable devices can promote unique skin-like mechanical properties mediated by conformal interactions and high sensitivity. One of the advantages of wearable mechanical sensors is its ability to maintain robust sensing performance under aquatic conditions, such as sweating, raining, swimming, and seabed conditions. It is well known that hydrogels are prone to swelling in hydrated environments, which can lead to unwanted deformation, distortion / interruption of output signals, and irreversible degradation / destruction of overall performance. Hydrogel electronics that can stably operate in hydrated environments are highly demanded but remain to be achieved. Researchers have been working on providing hydrogels with anti-swelling capabilities by introducing hydrophobic segments, carefully designing high cross-linking density, and / or constructing completely hydrophobic environments. Gao and co-workers constructed a hydrogel-based wearable sensor with excellent anti-swelling and sensing properties by copolymerizing hydrophilic and hydrophobic monomers in a mixed solvent consisting of water and dimethyl sulfoxide (DMSO). Unfortunately, the miscibility of DMSO with water initializes the uncontrollable migration of molecules and deteriorates the transport path of carriers, resulting in a loss of sensitivity. Wu et al. developed an ion gel sensor with excellent anti-swelling ability, without explicit molecular exchange between the gel and the external environment. However, the non-aqueous medium and strong molecular interactions severely restricted the migration of ions, resulting in low conductivity and inconsistent sensitivity. How to make hydrogel sensors with high sensitivity anti-swelling properties remains to be explored. Summary of the invention
[0003] The purpose of the present invention is to provide a method for synthesizing a conductive gel for extreme low temperature applications, specifically a method for synthesizing MXene and preparing a flexible wearable binary solvent conductive hydrogel film. MXene has good electrical conductivity and photothermal properties, which is beneficial to the application of flexible hydrogels in wearable display health monitoring. The present invention adopts the following technical solutions:
[0004] The present invention relates to a method for synthesizing a MXene-based binary solvent conductive gel. The characteristic steps are as follows:
[0005] 1) Preparation of MXene: First, weigh the Ti3AlC2 phase and immerse it in HF solution at room temperature to extract aluminum atoms. Then, wash the resulting suspension with deionized water and centrifuge to obtain a multilayer Ti3C2T x Then, the obtained multilayer Ti3C2T x Immerse in dimethyl sulfoxide at room temperature, centrifuge and wash with deionized water several times, and disperse in 200 mL of deionized water. Finally, the suspension was peeled off with an ultrasonic cell disruptor for 4 h and centrifuged at 3500 rpm for 30 min. The black precipitate was then dried by freeze drying under vacuum to obtain a single-layer MXene nanosheet.
[0006] 2) MXene-based binary solvent conductive gel: Add MXene to a mixed binary solvent of deionized water and dimethyl sulfoxide, and then add acrylamide, agar, ammonium persulfate, and methylene bis(acrylamide), stir thoroughly until completely dissolved, and heat in an oven to react to form a hydrogel.
[0007] Preferably, step 1) 10 g of MXene phase is placed in 45% HF solution (100 mL) for 12 h;
[0008] Preferably, in step 2), the mass ratio of deionized water to dimethyl sulfoxide is 1:1, the agar concentration is 2%wt, and the Mxene concentration is 0.5mg / ml;
[0009] The present invention uses acrylamide as a reaction site, MXene as a conductive filler and catalyst, and agar as a reinforcing agent to prepare a wearable flexible binary solvent conductive hydrogel. BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Figure 1 SEM and AFM images of MXene of the present invention
[0011] Figure 2 This is the SEM image of the MXene binary solvent gel of the present invention;
[0012] Figure 3 This is the rheological diagram of the MXene binary solvent gel of the present invention; DETAILED DESCRIPTION
[0013] Two embodiments of the present invention are provided below to further illustrate the present invention, but not to limit the scope of the present invention.
[0014] Example 1
[0015] 1) Preparation of MXene: First, weigh 10g of Ti3AlC2Mxene phase and immerse it in 45% HF solution (100mL) at room temperature for 12h to extract Al atoms. Then, the resulting suspension was washed with deionized water and centrifuged to obtain a Ti3C2Tx powder precipitated as a multilayer. Subsequently, the obtained multilayer Ti3C2Tx was immersed in dimethyl sulfoxide for 24h at room temperature, centrifuged and washed with deionized water several times, and dispersed in 200mL deionized water. Finally, the suspension was peeled off for 4h with an ultrasonic cell disruptor and centrifuged at 3500rpm for 30min. The black precipitate was then dried by freeze drying under vacuum to obtain a monolayer MXene nanosheet.
[0016] 2) Preparation of MXene binary solvent conductive hydrogel: Add 1 ml of MXene aqueous dispersion (5 mg / mL) to a mixed binary solvent of 5 mL of deionized water and 5 mL of dimethyl sulfoxide, then add 2 g of acrylamide, 20 nm of agar, 100 μL of ammonium persulfate solution (100 mg / mL), and 100 μL of methylene bis(acrylamide) aqueous solution (100 mg / mL), stir thoroughly until completely dissolved, and heat the reaction at 60 °C in an oven for 30 min to generate a hydrogel.
[0017] Example 2
[0018] 1) Preparation of MXene: First, weigh 10g of Ti3AlC2Mxene phase and immerse it in 45% HF solution (100mL) at room temperature for 12h to extract Al atoms. Then, the resulting suspension was washed with deionized water and centrifuged to obtain a Ti3C2Tx powder precipitated as a multilayer. Subsequently, the obtained multilayer Ti3C2Tx was immersed in dimethyl sulfoxide for 24h at room temperature, centrifuged and washed with deionized water several times, and dispersed in 200mL deionized water. Finally, the suspension was peeled off for 4h with an ultrasonic cell disruptor and centrifuged at 3500rpm for 30min. The black precipitate was then dried by freeze drying under vacuum to obtain a monolayer MXene nanosheet.
[0019] 2) Preparation of MXene binary solvent conductive hydrogel: Add 0.5 mL of MXene aqueous dispersion (5 mg / mL) to a mixed binary solvent of 4 mL of deionized water and 6 ml of dimethyl sulfoxide, then add 2 g of acrylamide, 20 mg of agar, 100 μL of ammonium persulfate solution (100 mg / mL), and 100 μL of methylene bis(acrylamide) aqueous solution (100 mg / mL), stir thoroughly until completely dissolved, and heat the reaction at 60 °C in an oven for 30 min to generate a hydrogel.
[0020] The present invention is described above by way of example. It should be noted that, without departing from the core of the present invention, any simple deformation, modification or other equivalent replacement that can be made by those skilled in the art without inventive effort falls within the protection scope of the present invention.
Claims
1. A method for synthesizing a conductive gel for extreme low temperature applications.
2. The method for synthesizing transition metal carbides of claim 1, characterized in that the Ti3AlC2Mxene phase is etched with hydrofluoric acid to extract aluminum atoms.
3. Preparation of MXene binary solvent conductive hydrogel: Add 1 ml of MXene aqueous dispersion (5 mg / ml) to a mixed binary solvent of 5 ml of deionized water and 5 ml of dimethyl sulfoxide, then add 2 g of acrylamide, 20 mg of agar, 100 μl of ammonium persulfate solution (100 mg / ml), and 100 μl of methylene bis(acrylamide) aqueous solution (100 mg / ml), stir thoroughly until completely dissolved, and heat the reaction at 60 °C in an oven for 30 min to generate a hydrogel.