CN109095449B - Carbon aerogel with ultrahigh linear sensitivity, preparation thereof and application thereof in sensor - Google Patents
Carbon aerogel with ultrahigh linear sensitivity, preparation thereof and application thereof in sensor Download PDFInfo
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- CN109095449B CN109095449B CN201810972732.5A CN201810972732A CN109095449B CN 109095449 B CN109095449 B CN 109095449B CN 201810972732 A CN201810972732 A CN 201810972732A CN 109095449 B CN109095449 B CN 109095449B
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- mxene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Abstract
The invention belongs to the technical field of flexible carbon materials, and discloses a carbon aerogel with ultrahigh linear sensitivity, and a preparation method and application thereof in a sensor. The method comprises the following steps: (1) in water, carrying out ultrasonic stripping and dispersion on MXene materials to obtain MXene suspension; (2) adding the nano microcrystalline cellulose into the suspension, performing ultrasonic treatment, freezing by using liquid nitrogen, and performing freeze drying to obtain the composite aerogel; and carbonizing the composite aerogel in an inert atmosphere to obtain the elastic carbon aerogel. The preparation method combines the advantages of MXene and nano microcrystalline cellulose, utilizes the dispersing, supporting and connecting effects of the nano microcrystalline cellulose on the MXene and the strengthening effect of the MXene lamella on the aerogel, and prepares the carbon aerogel with the characteristics of high compression, high resilience, excellent recycling performance, ultrahigh linear sensitivity and the like through freezing, freeze drying and carbonization. The carbon aerogel of the present invention is applied to sensing electronic devices.
Description
Technical Field
The invention belongs to the technical field of flexible carbon materials, and particularly relates to carbon aerogel with ultrahigh linear sensitivity, a preparation method thereof and application thereof in a sensor.
Background
The important role of flexible carbon materials in sensing devices depends on their compressive properties, elasticity, fatigue resistance and sensitivity. The planar structure of the two-dimensional nano material has unique advantages in the design of ultrathin electrodes, flexible materials and light base materials. MXene as a novel material in a two-dimensional nano carbon material has high conductivity and certain flexibility, and can realize large size under the condition of ultrathin. Therefore, the method has great prospect in preparing flexible materials with excellent sensing performance. The traditional carbon-based flexible material mostly uses graphene and carbon nano tubes as raw materialsAs a substrate, such as graphene/carbon nanotube composite (19.8 kPa)-1) (Jianan M, Xia K, Wang Q, et al. Flexible and high Sensitive substrates on biological Functional structures, 2017,27(9):1606066.), graphene paper (17.2 kPa)-1) (Tao L Q, Zhang K N, Tian H, et al, graphene-Paper Pressure Sensor for Detecting Human motion. acs Nano,2017,11(9):8790.), graphene/polydimethylsiloxane (1.80 kPa. RTM.: 8790.)-1) (Bae G Y, Pak S W, Kim D, et al, Linear and high Pressure-Sensitive Electronic Skin Based on a biological infected Structural array. advanced Materials,2016,28(26): 5300-. However, since the graphene and the carbon nanotube are easy to form defects in the preparation process, the material has strong dependence on high-quality graphene or carbon nanotube, and the pressure sensor prepared by the method mostly uses a flexible substrate, so that the pressure sensor has large recognizable stress and is difficult to realize sensitive sensing under micro stress.
Therefore, the key to preparing the ultrahigh-sensitivity carbon aerogel is to realize high-sensitivity sensing of stress by combining a flexible carbon material substrate with a reasonable structure.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of carbon aerogel with ultrahigh linear sensitivity.
Another object of the present invention is to provide a carbon aerogel having ultra-high linear sensitivity prepared by the above method.
It is a further object of the present invention to provide the use of the above ultra-high linear sensitivity carbon aerogels in sensors, particularly pressure sensing electronics.
The purpose of the invention is realized by the following technical scheme:
a preparation method of carbon aerogel with ultrahigh linear sensitivity comprises the following steps:
(1) in water, carrying out ultrasonic stripping and dispersion on MXene materials to obtain MXene suspension;
(2) adding the nano microcrystalline cellulose into the MXene suspension obtained in the step (1), and performing ultrasonic treatment to obtain MXene/nano microcrystalline cellulose suspension;
(3) carrying out liquid nitrogen freezing on the MXene/nano microcrystalline cellulose suspension obtained in the step (2), and then carrying out freeze drying to obtain MXene/nano microcrystalline cellulose composite aerogel;
(4) and (4) heating the composite aerogel obtained in the step (3) to 500-1200 ℃ in an inert atmosphere, and preserving heat for 0-12 hours to obtain the elastic carbon aerogel.
The MXene material in the step (1) is Ti3C2。
The concentration of MXene in the MXene suspension in the step (1) is 0.01-5 wt%, and preferably 0.1%; the ultrasonic stripping time is 0.1-24 hours, preferably 2 hours.
Preferably, the nano microcrystalline cellulose in the step (2) is obtained by using cellulose as a raw material and performing acid hydrolysis or oxidative degradation; more preferably, the nanocrystalline cellulose is obtained by hydrolysis of cellulose with 65% sulphuric acid.
Preferably, the addition amount of the nano microcrystalline cellulose in the step (2) is 1-10 times of the mass of MXene in the step (1).
Preferably, the inert atmosphere in step (4) refers to at least one of nitrogen or argon atmosphere.
Preferably, the temperature rise rate in the step (4) is 0.1-50 ℃/min; more preferably, the temperature is raised to 700 ℃ at the speed of 3-5 ℃/min and is kept for 2 h.
A carbon aerogel having high linear sensitivity is prepared by the above method.
The carbon aerogel with high linear sensitivity is applied to a sensor, in particular to a stress sensor.
The principle of the invention is as follows: by combining the advantages of the cellulose nano-crystallite and MXene, the nano-crystallite cellulose is derived from renewable resources and has the advantages of high specific surface area, light weight, abundant surface groups, excellent mechanical strength, low cost, renewability, environmental friendliness, excellent water dispersibility and suspension performance and the like. MXene serving as a novel two-dimensional material has a wide application prospect in the fields of adsorption separation, energy storage, sensing, electrocatalysis and the like due to excellent physical and chemical properties such as excellent conductivity, thermal stability, excellent flexibility and the like. Different from the existing method for preparing elastic carbon materials such as graphene oxide, graphene and carbon nano tubes, the nanocrystalline cellulose and MXene have good synergistic effect: the MXene dispersion liquid is filled with the nano microcrystalline cellulose to play a role in space separation, so that the MXene lamella is prevented from being stacked in the solution, in a freezing process and in a carbonization process; the nano microcrystalline cellulose is converted into nano carbon to be connected with the MXene sheet in the carbonization process, so that the carbon aerogel has good resilience performance, and meanwhile, the MXene sheet can assist the nano microcrystalline cellulose to form a sheet structure in the freeze drying process, so that the nano microcrystalline cellulose is prevented from being interwoven, and the material has excellent cyclic compression performance. The preparation method combines the advantages of MXene and nano microcrystalline cellulose, utilizes the dispersing, supporting and connecting effects of the nano microcrystalline cellulose on the MXene, and prepares the carbon aerogel with high compression, high resilience, excellent recycling performance, ultrahigh linear sensitivity and the like through freezing, freeze drying and carbonization. Due to the structural characteristics, the obtained carbon aerogel can realize high-sensitivity detection on micro pressure and strain and can 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) MXene maintains high dispersion during preparation, and stacking is prevented;
(2) the prepared carbon aerogel has high compressibility, high elasticity and cycling stability;
(3) the prepared carbon aerogel has ultrahigh linear sensitivity;
(4) the prepared carbon aerogel has ultrahigh sensitivity to micro deformation and excellent circulating stability, and can be widely applied to the field of sensing.
Drawings
FIG. 1 is a graph of the current response of the elastic carbon aerogel with ultra-high linear sensitivity prepared in example 1 at different degrees of bending (a) and stress-strain curves at different compressive strains (b is 10% -60% at different compressive strains, c is 60% -90% compressive strain);
FIG. 2 is a stress-strain graph of 10 th, 100 th, 1000 th and 10000 th times at a compressive strain of 50% for the elastic carbon aerogel having ultra-high linear sensitivity prepared in example 1;
FIG. 3 is a graph of the current response of the ultra-high linear sensitivity elastic carbon aerogel prepared in example 2 at 10%, 30%, 50%, 70% and 90% compressive strain;
FIG. 4 is the current sensing cycling stability at 50% compressive strain of the ultra-high linear sensitivity elastomeric carbon aerogel prepared in example 2;
FIG. 5 is a graph showing the linear sensitivity (a) of the elastic carbon aerogel having ultra-high linear sensitivity prepared in example 2 at a stress of more than 10 Pa and the linear sensitivity (b) at a stress of less than 10 Pa;
fig. 6 shows the current induction of the elastic carbon aerogel with ultra-high linear sensitivity prepared in example 3 on the pulse signal of human body.
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) Adding the material into ultrapure water or deionized water, and then ultrasonically stripping and dispersing for 2 hours to obtain MXene suspension with the concentration of 0.05 wt%;
(2) adding nano microcrystalline cellulose with the mass 3 times of that of MXene into the MXene suspension obtained in the step (1), and performing ultrasonic treatment for 0.5 hour again to obtain MXene/nano microcrystalline cellulose suspension;
(3) placing the MXene/nano microcrystalline cellulose suspension in a plastic box, placing the box on the outer wall of a metal box, pouring liquid nitrogen into the metal box for freezing (freezing for 15 minutes), and freeze-drying after the solution is completely frozen (-52 ℃, 24 hours) to obtain the MXene/nano microcrystalline cellulose composite aerogel;
(4) and (3) placing the composite aerogel in a tube furnace, heating to 600 ℃ at the speed of 3 ℃/min in the nitrogen atmosphere, and preserving heat for 4 hours to obtain the elastic carbon aerogel.
The obtained carbon aerogel has excellent elasticity, and the compression performance of the elastic carbon aerogel is performed on an electronic universal tester, and a 50N sensor is used.
Fig. 1 is a graph of the current response of the elastic carbon aerogel with ultra-high linear sensitivity prepared in example 1 at different degrees of bending (a) and stress-strain curves at different compressive strains (b is 10% -60% at different compressive strains, and c is 60% -90% compressive strain). FIG. 1(a) is a graph showing the current response of the elastic carbon aerogel prepared in this example at different degrees of bending. Under different bending degrees, the material has different current responses, and shows that the material has excellent elasticity and structural stability and can be applied to wearable electronic devices. FIG. 1(b) is a stress-strain curve of a material at different compressive strains of 10% to 60%, indicating that the material has a wide strain range and excellent compressibility. Fig. 1(c) is a stress-strain curve at different strains from 60% to 90% compression, indicating that the material has high compressibility. The cyclic compression performance of the elastic carbon aerogel prepared in this example is shown in fig. 2 (fig. 2 is a stress-strain curve diagram of 10 th, 100 th, 1000 th and 10000 times of the elastic carbon aerogel with ultrahigh linear sensitivity prepared in example 1 when the compressive strain is 50%), and after 10000 times of cyclic compression under 50% compressive strain, the maximum stress of the material can still be maintained at 87.9%, indicating that the material has excellent cyclic stability.
Example 2
(1) Mixing MXene (Ti)3C2) Adding into ultrapure water or deionized water, and then ultrasonically stripping and dispersing for 1 hour to obtain MXene suspension with the concentration of 0.1 wt%;
(2) adding nano microcrystalline cellulose with the mass 5 times of that of MXene into the MXene suspension obtained in the step (1), and performing ultrasonic treatment for 1 hour again to obtain MXene/nano microcrystalline cellulose suspension;
(3) placing the MXene/nano microcrystalline cellulose suspension in a plastic box, placing the box on the outer wall of a metal box, pouring liquid nitrogen into the metal box for freezing (freezing for 15 minutes), and freeze-drying after the solution is completely frozen (-52 ℃, 24 hours) to obtain the MXene/nano microcrystalline cellulose composite aerogel;
(4) and (3) placing the obtained composite aerogel in a tubular furnace, heating to 700 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The stress-current, strain-current induction and sensitivity test of the obtained elastic carbon aerogel with ultrahigh linear sensitivity are carried out on an electronic universal tester, and a 50N sensor is used; the electrochemical workstation was used to record the current change upon compression.
The elastic carbon aerogel obtained in the embodiment has excellent current response behavior and extremely high linear sensitivity.
Fig. 3 is the current response of the elastic carbon aerogel obtained in this example at 10%, 30%, 50%, 70% and 90% compressive strain, respectively, and shows that the material has a wide sensing range. The current sensing cycling stability of the elastic carbon aerogel of the embodiment under 50% compressive strain is shown in fig. 4, and after 2000 cycles of compression, the current signal is not obviously reduced, which indicates that the sensing material has excellent current sensing cycling stability. FIG. 5 is a graph showing the linear sensitivity (a) of the elastic carbon aerogel having ultra-high linear sensitivity prepared in example 2 at a stress of more than 10 Pa and the linear sensitivity (b) at a stress of less than 10 Pa. The linear sensitivity of the elastic carbon aerogel obtained in the embodiment in different pressure ranges can reach 114.64kPa when the stress is less than 10 Pa-1Sensitivity of 42.92kPa at > 10 Pa-1。
Example 3
(1) Mixing MXene (Ti)3C2) Adding the mixture into ultrapure water or deionized water, and then ultrasonically stripping and dispersing for 4 hours to obtain MXene suspension with the concentration of 1 wt%;
(2) adding nano microcrystalline cellulose with the mass 4 times of that of MXene into the MXene suspension obtained in the step (1), and performing ultrasonic treatment for 3 hours again to obtain MXene/nano microcrystalline cellulose suspension;
(3) placing the MXene/nano microcrystalline cellulose suspension in a plastic box, placing the box on the outer wall of a metal box, pouring liquid nitrogen into the metal box for freezing (freezing for 15 minutes), and freeze-drying after the solution is completely frozen (-52 ℃, 24 hours) to obtain the MXene/nano microcrystalline cellulose composite aerogel;
(4) and (3) placing the obtained composite aerogel in a tubular furnace, heating to 700 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The wearing test of the obtained aerogel with ultrahigh sensitivity is detected by a digital source meter.
The carbon aerogel obtained by the embodiment has ultrahigh sensitivity, and can be applied to wearable electronic equipment. The prepared elastic carbon aerogel is applied to wearable electronic equipment. Fig. 6 shows the current induction of the elastic carbon aerogel with ultra-high linear sensitivity prepared in example 3 on the pulse signal of human body. As shown in fig. 6, the pulse signal of the human body can be clearly sensed, which indicates that the carbon aerogel prepared in this embodiment can be applied to flexible electronic devices.
Compared with the carbon aerogel applied by the application number 201711057227.X patent, the elastic carbon aerogel prepared by the invention has better stability (the height retention of the material applied by the application number 201711057227.X patent is 91.8% after being circulated for 10000 times, the stress retention is 71.2%, and the height retention of the material applied by the application number 201711057227.X patent is 95.4% after being compressed for 10000 times, and the stress retention is 87.9%), and has linear sensitivity which is not possessed by the application number 201711057227.X patent application.
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 (9)
1. A method for preparing carbon aerogel with linear sensitivity is characterized in that: the method comprises the following steps:
(1) in water, carrying out ultrasonic stripping and dispersion on MXene materials to obtain MXene suspension;
(2) adding the nano microcrystalline cellulose into the MXene suspension obtained in the step (1), and performing ultrasonic treatment to obtain MXene/nano microcrystalline cellulose suspension; the MXene material in the step (1) is Ti3C2；
(3) Carrying out liquid nitrogen freezing on the MXene/nano microcrystalline cellulose suspension obtained in the step (2), and then carrying out freeze drying to obtain MXene/nano microcrystalline cellulose composite aerogel;
(4) and (4) heating the composite aerogel obtained in the step (3) to 500-1200 ℃ in an inert atmosphere, and preserving heat for 0-12 hours to obtain the elastic carbon aerogel.
2. The method of preparing a carbon aerogel having linear sensitivity according to claim 1, wherein:
the concentration of MXene in the MXene suspension in the step (1) is 0.01-5 wt%.
3. The method of preparing a carbon aerogel having linear sensitivity according to claim 1, wherein: the addition amount of the nano microcrystalline cellulose in the step (2) is 1-10 times of the mass of MXene in the step (1).
4. The method of preparing a carbon aerogel having linear sensitivity according to claim 1, wherein: the ultrasonic stripping time in the step (1) is 0.1-24 hours;
the inert atmosphere in the step (4) is at least one of nitrogen or argon atmosphere.
5. The method of preparing a carbon aerogel having linear sensitivity according to claim 1, wherein: the nano microcrystalline cellulose in the step (2) is obtained by taking cellulose as a raw material and performing acid hydrolysis or oxidative degradation.
6. The method of preparing a carbon aerogel having linear sensitivity according to claim 1, wherein: the temperature rise rate in the step (4) is 0.1-50 ℃/min.
7. A carbon aerogel having linear sensitivity obtained by the production method according to any one of claims 1 to 6.
8. The use of the carbon aerogel with linear sensitivity of claim 7 in a sensor.
9. Use according to claim 8, characterized in that: the sensor is a stress sensor.
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