CN109851313B - High-sensitivity and wide-linear-sensing-range compressible composite carbon aerogel and preparation and application thereof - Google Patents
High-sensitivity and wide-linear-sensing-range compressible composite carbon aerogel and preparation and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of elastic carbon materials, and discloses a compressible composite carbon aerogel with high sensitivity and a wide linear sensing range, and preparation and application thereof. The method comprises the following steps: 1) dispersing MXene nanosheets in water to obtain MXene suspension; 2) uniformly mixing water-soluble trivalent ferric salt, acid and MXene suspension with chitosan, freezing, and drying to obtain composite aerogel; 3) carrying out heat treatment on the composite aerogel in an inert atmosphere to obtain composite carbon aerogel; the heat treatment is heating to 500-1200 ℃ and keeping the temperature for 0-12 h. The method is simple and environment-friendly; the prepared carbon aerogel has high compressibility, high resilience and excellent cycle stability; meanwhile, the prepared carbon aerogel has ultrahigh sensitivity and wide-range linear sensing and is applied to sensing devices.
Description
Technical Field
The invention belongs to the field of elastic carbon materials, and particularly relates to a compressible composite carbon aerogel with high sensitivity and a wide linear sensing range, and a preparation method and application thereof.
Background
The compressible elastic carbon aerogel can be assembled into a piezoresistive sensor to be applied to the fields of human-computer interaction, biomedical monitoring, motion detection and the like due to the performance of converting external pressure or strain into a current signal in the compression process. The traditional compressible carbon material is mostly constructed by nano carbon materials such as carbon nano tubes, graphene and derivatives thereof, nano carbon composite materials and the like. However, the nano carbon materials are sourced from non-renewable petrochemical resources, face the problems of environmental pollution, unsustainability and the like, and are complex in preparation method and high in cost.
MXene, as a new two-dimensional material, has unique physicochemical properties including high charge carrier mobility, metal conductivity, excellent mechanical properties and the like, and is widely used in the fields of energy storage, electromagnetic shielding, separation membranes and the like. The relevant research in the field of MXene sensing performance and sensors is also related to documents. There is a report in the literature of MXene/rGO aerogels with a reticulated structure (3D synergistic MXene/Reduced Graphene Oxide Aerogel for aPiezoresistive sensor. Acs Nano2018) that are compressible. However, the maximum compression amount of the aerogel is only 60%, high linear sensitivity cannot be obtained in a wide pressure or strain range, the application range is limited, and the service life is difficult to guarantee; and the sensitivity is low (22.56 kPa)-1) Applications are also limited. In addition, the graphene oxide is adopted, so that the cost of the material is high, and the practical application is difficult to realize. Biomass is an ideal raw material for constructing low-cost and sustainable carbon materials as a renewable carbon source with abundant reserves and low price in the nature. However, due to the difficulty of structural design, great shrinkage during carbonization and brittleness of derived carbon of a single biomass raw material, the mechanical properties of the material are poor, and the material is difficult to apply industrially. Therefore, the preparation of the carbon material with high elasticity, excellent fatigue resistance, high sensitivity and wide-range linear sensing has great significance in the aspect of wearable sensing devices.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a compressible composite carbon aerogel with excellent fatigue resistance, high sensitivity and wide linear sensing range and a preparation method thereof. The compressible composite carbon aerogel disclosed by the invention has the characteristics of excellent fatigue resistance, high sensitivity and wide linear sensing range.
It is another object of the present invention to provide the use of the above-described compressible composite carbon aerogel in sensing devices, particularly pressure sensing electronic devices.
The purpose of the invention is realized by the following technical scheme:
a preparation method of compressible composite carbon aerogel with high sensitivity and wide linear sensing range comprises the following steps:
1) dispersing MXene nanosheets in water to obtain MXene suspension;
2) uniformly mixing water-soluble trivalent ferric salt, acid and MXene suspension with chitosan, freezing, and drying to obtain composite aerogel;
3) carrying out heat treatment on the composite aerogel in an inert atmosphere to obtain composite carbon aerogel; the heat treatment is to heat the mixture to 500-1200 ℃ and keep the temperature for 0-12 h.
The temperature of the heat treatment is preferably 600-900 ℃, and more preferably 700-900 ℃; the time of the heat treatment is preferably 1 to 3 hours.
The MXene nano-sheet in the step 1) is Ti3C2. The concentration of the MXene suspension in the step 1) is 0.5-10 mg/mL, preferably 1-5 mg/mL.
The water-soluble ferric salt in the step 2) is more than one of ferric trichloride, ferric nitrate and ferric sulfate containing or not containing crystal water; preferably ferric chloride.
The acid in the step 2) is glacial acetic acid, dilute hydrochloric acid and dilute sulfuric acid, preferably glacial acetic acid;
the temperature of the freezing treatment in the step 2) is-200 to-160 ℃. The drying is freeze drying, and the temperature is more than or equal to-60 ℃.
The mol volume ratio of the water-soluble ferric salt to the MXene suspension in the step 2) is (0.0005-0.1) mol: 1L, preferably (0.001 to 0.005) mol/L.
The volume ratio of the acid to the MXene suspension in the step 2) is (0.1-2): 100.
the mass-to-volume ratio of the chitosan to the MXene suspension in the step 2) is (0.02-2) g:100mL, preferably 0.1-1 g:100mL, more preferably 0.5 g:100 mL.
The composite aerogel in the step 2) is prepared by the following method:
a) mixing water-soluble trivalent ferric salt and acid with MXene suspension to obtain acidic MXene suspension;
b) and dissolving chitosan in the acidic MXene suspension, performing ultrasonic treatment, freezing treatment and drying to obtain the composite aerogel.
The inert atmosphere in the step 3) refers to at least one of nitrogen or argon.
When the heat treatment is carried out in the step 3), the temperature rising rate is 0.1-50 ℃/min; more preferably at 3 to 5 ℃/min.
The compressible composite carbon aerogel with high sensitivity and wide linear sensing range is prepared by the method.
The compressible composite carbon aerogel with high sensitivity and wide linear sensing range is applied to sensing devices, particularly pressure sensing electronic devices.
The principle of the invention is as follows: (1) due to the existence of chitosan macromolecules, MXene nanosheets are prevented from being directly re-stacked, and adjacent MXene nanosheets are connected through combination or bridging, so that a continuous layered structure is formed; (2) ion interaction between the protonated chitosan and the MXene nanosheets with negative charges and a large number of hydrogen bonds are connected, so that the MXene nanosheets are wrapped by the chitosan and connected, and are welded into aerogel with a three-dimensional structure in the carbonization process; (3) the wave-shaped laminated structure ensures that the material has excellent elastic deformation performance, and can output stable current response signals from tiny pressure or strain by changing the contact area between the sheets.
The preparation method of the invention is greatly different from the prior method for preparing the elastic carbon material: firstly, the biomass chitosan is selected as the raw material, so that the use of nano carbon materials such as carbon nano tubes, graphene and the like with complex preparation process and high cost is avoided, and the material has the advantages of environmental friendliness, reproducibility, low price, simple preparation and the like; secondly, in the carbonization process, MXene nanosheets are epitaxially welded by chitosan derived carbon to enhance the bonding strength of the MXene nanosheets; and thirdly, the MXene nanosheets are helpful to form a lamellar structure in the freezing process, and the shrinkage phenomenon structure of the chitosan is converted into a wave-shaped lamellar carbon skeleton in the carbonization process. In addition, MXene can also be used as a nano-support material to effectively prevent the volume of the material from greatly shrinking in the carbonization process. The two have synergistic effect to prevent the collapse of the structure, so that the carbon aerogel has good resilience. The invention combines the advantages of chitosan and MXene two-dimensional nanosheets, utilizes the supporting effect of MXene on chitosan chains and the connecting effect of chitosan derived carbon on the structure, and prepares the carbon aerogel with the characteristics of high compression, high resilience, excellent recycling performance, high sensitivity, wide-range linear sensing and the like through oriented freezing, freeze drying and carbonization. And the structural characteristics enable the obtained carbon aerogel to realize high-sensitivity and wide-range linear sensing and be applied to various pressure sensing electronic devices.
The preparation method and the obtained elastic carbon aerogel have the following advantages and beneficial effects:
(1) the preparation process is simple and environment-friendly;
(2) the prepared carbon aerogel has high compressibility, high elasticity and excellent cycle stability;
(3) the prepared carbon aerogel has stable conductivity;
(4) the prepared carbon aerogel has ultrahigh sensitivity, wide sensing range and excellent cycling stability, and can be widely applied to the sensing field.
Drawings
FIG. 1 is a stress-strain graph of the elastic carbon aerogel prepared in example 1 compressed for ten cycles at different compressive strains; the upper graph in the figure is a photograph before compression, after 99% compression and after rebound;
FIG. 2 is a stress-strain diagram (a) and maximum stress and height retention (b) of the elastic carbon aerogel prepared in example 1 after 150000 cycles of cyclic compression at a compressive strain of 50%; the upper picture in a is a photograph before and after compression;
FIG. 3 is a graph showing the sensitivity of the elastic carbon aerogel prepared in example 1 in a range of 0 to 5kPa (strain amount of 0 to 70% with respect to the height of the material);
FIG. 4 is a graph (a) showing the results of sensing a slight stress (1Pa) and a slight strain (corresponding to 0.05% of the height of the material) in the elastic carbon aerogel prepared in example 1;
FIG. 5 is a graph showing the results of the response of the elastic carbon aerogel prepared in example 1 to bending; the test is carried out at normal temperature and normal pressure, and the numerical values of 30,60,90 and the like in the figure represent the bending angle applied to the obtained aerogel; the lower right hand picture is a photograph of a curved carbon aerogel;
FIG. 6 is a stress-strain graph of the elastic carbon aerogel prepared in example 2 at 70% compressive strain at times 1, 100, 300, and 500; the top right picture is a photograph of carbon aerogel before and after 500 cycles of compression;
FIG. 7 is a stress-strain graph of the elastic carbon aerogel prepared in example 3 at 70% compressive strain at times 1, 10, 100, 300, and 500; the upper right panel is a photograph of carbon aerogel before and after 500 cycles of compression.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Mixing MXene (Ti)3C2) Placing the suspension in water for ultrasonic dispersion to obtain 50mL of MXene suspension with the concentration of 1 mg/mL;
(2) 0.05g FeCl3·6H2Dissolving O and 500 mu l of glacial acetic acid in the MXene suspension to obtain acidic MXene suspension;
(3) slowly adding 0.25g of chitosan into the suspension under high-speed stirring (500r/min), stirring at high speed until the chitosan is dissolved, and performing ultrasonic treatment for 20 minutes (above 300 Hz) to obtain MXene/chitosan suspension;
(4) freezing MXene/chitosan suspension with liquid nitrogen (-196 deg.C, treating to completely freeze to ice, generally about 20 min), and freeze drying (-58 deg.C, 0.22mbar, till completely drying) to obtain composite aerogel;
(5) and (3) placing the obtained composite aerogel in a tube furnace, heating to 800 ℃ at the speed of 3 ℃/min in the argon atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The compression performance, compression-resistance and compression-current induction behaviors of the obtained elastic carbon aerogel are performed on an electronic universal testing machine, and a 100N sensor is used; a high-precision multimeter is adopted to record the resistance of the material during compression; the electrochemical workstation was used to record the current change upon compression.
FIG. 1 is a stress-strain graph of the elastic carbon aerogel prepared in this example compressed for ten cycles at different compressive strains. The material can withstand a compression of 99% while keeping the height substantially unchanged, indicating that the material has excellent elasticity. FIG. 2 is a stress-strain diagram (a) and maximum stress and height retention (b) of the elastic carbon aerogel prepared in this example after 150000 cycles of cyclic compression at a compressive strain of 50%. The high retention of the material after 150000 cycles of compression was as high as 91.6%, indicating excellent structural stability of the material. FIG. 3 is a graph showing the results of the sensing of the elastic carbon aerogel prepared in this example under a pressure of 0 to 5kPa (0 to 70% strain corresponding to the height of the material) against a relatively large pressure (i.e., the sensitivity of the elastic carbon aerogel under a pressure of 0 to 5 kPa). The material has a linear detection range of 5kPa, the stress corresponds to the strain of the material of up to 70 percent, and the material can still keep stable linear signal output under large-amplitude compression. Fig. 4 is a graph (a) showing the results of sensing a slight stress (1Pa) and a graph (b) showing the results of sensing a slight strain (corresponding to 0.05% of the height of the material) in the elastic carbon aerogel prepared in this example. The obtained carbon aerogel can sensitively sense micro pressure and deformation, and the combination of the figure shows that the material has ultrahigh sensitivity and wide application range. FIG. 5 is a graph showing the results of the response of the elastic carbon aerogel prepared in this example to bending; the test was carried out at normal temperature and pressure, and the numerical values of 30,60,90, etc. represent the bending angles applied to the resulting aerogels. The material can output different signal values for different bending angles, and the potential application of the material in the detection of the bending angles is indicated.
Example 2
(1) Placing MXene in water for ultrasonic dispersion to obtain 50mL of MXene suspension with the concentration of 3 mg/mL;
(2) 0.03g of FeCl3·6H2Dissolving O and 300 mu l of glacial acetic acid (anhydrous acetic acid) in the MXene suspension to obtain acidic MXene suspension;
(3) slowly adding 0.15g of chitosan into the obtained suspension under high-speed stirring, stirring at high speed until the chitosan is dissolved, and performing ultrasonic treatment for 20 minutes to obtain MXene/chitosan suspension;
(4) freezing the MXene/chitosan suspension with liquid nitrogen, and freeze-drying (-58 deg.C, 0.22mbar, till completely drying) after the solution is completely frozen to obtain composite aerogel;
(5) and (3) placing the obtained composite aerogel in a tube furnace, heating to 800 ℃ at the speed of 3 ℃/min in the argon atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The stress-strain curves of the elastic carbon aerogel prepared in this example at 70% compressive strain at cycles 1, 100, 300, and 500 are shown in fig. 6. The material has excellent compressibility and rebound resilience.
Example 3
(1) Placing MXene in water for ultrasonic dispersion to obtain 50mL of MXene suspension with the concentration of 5 mg/mL;
(2) 0.05g FeCl3·6H2Dissolving O and 500 mu l of glacial acetic acid in the MXene suspension to obtain acidic MXene suspension;
(3) slowly adding 0.25g of chitosan into the obtained suspension under high-speed stirring, stirring at high speed until the chitosan is dissolved, and performing ultrasonic treatment for 20 minutes to obtain MXene/chitosan suspension;
(4) freezing the MXene/chitosan with liquid nitrogen, and freeze-drying (-58 deg.C, 0.22mbar, till completely drying) after the solution is completely frozen to obtain composite aerogel;
(5) and (3) placing the obtained composite aerogel in a tube furnace, heating to 800 ℃ at the speed of 3 ℃/min in the argon atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
Stress-strain curves of the elastic carbon aerogel prepared in the example at the compression strain of 70% at cycles 1, 10, 100, 300 and 500 are shown in fig. 7. The material has excellent compressibility and rebound resilience.
Example 4
(1) Mixing MXene (Ti)3C2) Placing the suspension in water for ultrasonic dispersion to obtain 50mL of MXene suspension with the concentration of 1 mg/mL;
(2) 0.05g FeCl3·6H2Dissolving O and 500 mu l of glacial acetic acid in the MXene suspension to obtain acidic MXene suspension;
(3) slowly adding 0.25g of chitosan into the obtained suspension under high-speed stirring (500r/min), stirring at high speed until the chitosan is dissolved, and performing ultrasonic treatment for 20 minutes (300 Hz) to obtain MXene/chitosan suspension;
(4) freezing the MXene/chitosan suspension with liquid nitrogen, and freeze-drying (-58 deg.C, 0.22mbar, till completely drying) after the solution is completely frozen to obtain composite aerogel;
(5) and (3) placing the obtained composite aerogel in a tube furnace, heating to 700 ℃ at the speed of 3 ℃/min in the argon atmosphere, and preserving heat for 4 hours to obtain the elastic carbon aerogel.
The elastic carbon aerogel prepared by the embodiment can bear 80% of compression amount and keep the height basically unchanged, and the height basically does not change after 1000 cycles of compression when the compression strain is 50%. The material has excellent compressibility and rebound resilience.
Example 5
(1) Placing MXene in water for ultrasonic dispersion to obtain 50mL of MXene suspension with the concentration of 5 mg/mL;
(2) 0.05g FeCl3·6H2Dissolving O and 500 mu l of glacial acetic acid in the MXene suspension to obtain acidic MXene suspension;
(3) slowly adding 0.25g of chitosan into the obtained suspension under high-speed stirring, stirring at high speed until the chitosan is dissolved, and performing ultrasonic treatment for 20 minutes to obtain MXene/chitosan suspension;
(4) freezing the MXene/chitosan with liquid nitrogen, and freeze-drying (-58 deg.C, 0.22mbar, till completely drying) after the solution is completely frozen to obtain composite aerogel;
(5) and (3) placing the obtained composite aerogel in a tubular furnace, heating to 900 ℃ at the speed of 5 ℃/min in the argon atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The elastic carbon aerogel prepared by the embodiment can bear 90% of compression amount and keep the height basically unchanged, and the height basically does not change after 5000 cycles of compression when the compression strain is 50%. The material has excellent compressibility and rebound resilience.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of compressible composite carbon aerogel with high sensitivity and wide linear sensing range is characterized by comprising the following steps: the method comprises the following steps:
1) dispersing MXene nanosheets in water to obtain MXene suspension;
2) uniformly mixing water-soluble trivalent ferric salt, acid and MXene suspension with chitosan, freezing, and drying to obtain composite aerogel;
3) carrying out heat treatment on the composite aerogel in an inert atmosphere to obtain composite carbon aerogel; the heat treatment is to heat the mixture to 500-1200 ℃ and keep the temperature for 0-12 h.
2. The method of claim 1, wherein the method comprises the steps of: the temperature of the heat treatment in the step 3) is 600-900 ℃;
the concentration of the MXene suspension in the step 1) is 0.5-10 mg/mL;
the molar volume ratio of the water-soluble ferric salt to the MXene suspension in the step 2) is (0.0005-0.1) mol: 1L;
the mass-to-volume ratio of the chitosan to the MXene suspension in the step 2) is (0.02-2) g:100 mL.
3. The method of claim 2, wherein the method comprises the steps of: the concentration of the MXene suspension is 1-5 mg/mL; the temperature of the heat treatment in the step 3) is 700-900 ℃.
4. The method of claim 1, wherein the method comprises the steps of: the volume ratio of the acid to the MXene suspension in the step 2) is (0.1-2): 100, respectively;
the time of heat treatment in the step 3) is 1-3 h.
5. The method of claim 1, wherein the method comprises the steps of: the MXene nano-sheet in the step 1) is Ti3C2；
The water-soluble ferric salt in the step 2) is more than one of ferric trichloride, ferric nitrate and ferric sulfate containing or not containing crystal water;
in the step 2), the acid is glacial acetic acid, dilute hydrochloric acid and dilute sulfuric acid.
6. The method of claim 5, wherein the method comprises the steps of: the water-soluble ferric salt in the step 2) is ferric trichloride containing crystal water or not containing crystal water;
in the step 2), the acid is glacial acetic acid.
7. The method of claim 1, wherein the method comprises the steps of: the temperature of the freezing treatment in the step 2) is-200 to-160 ℃;
the drying in the step 2) is freeze drying, and the temperature is more than or equal to-60 ℃;
the inert atmosphere in the step 3) refers to at least one of nitrogen or argon;
when the heat treatment is carried out in the step 3), the temperature rising rate is 0.1-50 ℃/min.
8. A compressible composite carbon aerogel with high sensitivity and wide linear sensing range, which is obtained by the preparation method of any one of claims 1 to 7.
9. The use of the highly sensitive, wide linear sensing range compressible composite carbon aerogel according to claim 8 in a sensing device.
10. Use according to claim 9, characterized in that: the sensing device is a pressure sensing electronic device.
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| CN110628155B (en) * | 2019-09-27 | 2022-01-04 | 中国科学院深圳先进技术研究院 | MXene/metal composite aerogel, preparation method and application thereof, and thermal interface material comprising MXene/metal composite aerogel |
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| CN112911920B (en) * | 2021-02-08 | 2022-09-02 | 浙江环龙新材料科技有限公司 | Preparation method of MXene-carbon aerogel/TPU composite material |
| CN114414109B (en) * | 2022-01-26 | 2023-03-21 | 北京化工大学 | Preparation method of flexible wearable pressure sensor with language recognition function and product thereof |
| CN114620706B (en) * | 2022-02-10 | 2023-08-08 | 深圳市丽德宝纸品有限公司 | Wood-based carbon sponge with high-efficiency electromagnetic shielding performance and preparation method and application thereof |
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