CN107973283B - Elastic carbon aerogel and preparation method and application thereof - Google Patents
Elastic carbon aerogel and preparation method and application thereof Download PDFInfo
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- CN107973283B CN107973283B CN201711057227.XA CN201711057227A CN107973283B CN 107973283 B CN107973283 B CN 107973283B CN 201711057227 A CN201711057227 A CN 201711057227A CN 107973283 B CN107973283 B CN 107973283B
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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
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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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
- G01L9/0001—Transmitting or indicating the displacement of elastically deformable gauges by electric, electro-mechanical, magnetic or electro-magnetic means
- G01L9/0002—Transmitting or indicating the displacement of elastically deformable gauges by electric, electro-mechanical, magnetic or electro-magnetic means using variations in ohmic resistance
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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
- 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
- G01L9/04—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 resistance-strain gauges
Abstract
The invention belongs to the field of elastic carbon materials, and discloses an elastic carbon aerogel, and a preparation method and application thereof. Dispersing graphene oxide in water, stirring, ultrasonically dispersing uniformly, and then sequentially freezing by using liquid nitrogen, unfreezing and ultrasonically treating to obtain a graphene oxide suspension; adding nano microcrystalline cellulose, performing ultrasonic treatment, and adding a small molecular carbon source or nitrogen source to obtain a graphene oxide/nano microcrystalline cellulose suspension; freezing by using liquid nitrogen, then freeze-drying, then heating to 500-850 ℃ in an inert atmosphere, and preserving heat for 0-12 hours to obtain the elastic carbon aerogel. The method combines the advantages of the graphene oxide and the nano microcrystalline cellulose, utilizes the dispersing, supporting and carbon connecting effects of the nano microcrystalline cellulose on the graphene oxide, and further combines the carbon connecting effect of a small molecular carbon source or a nitrogen source, so that the obtained carbon aerogel has the characteristics of low density, high compression, high resilience, excellent recycling performance and the like.
Description
Technical Field
The invention belongs to the field of elastic carbon materials, and particularly relates to elastic carbon aerogel and a preparation method and application thereof.
Background
The important role of the elastomeric carbon material in a deformable device depends on its compressive properties, elasticity and fatigue resistance. The planar structure of the two-dimensional nano carbon material has unique advantages in the design of ultrathin electrodes, flexible materials and light base materials. Graphene oxide and graphene, which are representative materials of two-dimensional nanocarbon materials, have high electrical conductivity and certain flexibility, and can realize a large size in an ultra-thin situation, and thus, have attracted much attention in the preparation of carbon materials having good elasticity. At present, methods for preparing an elastic carbon material from graphene or graphene oxide may be classified into a sol-gel method and a freeze casting method. High elasticity Graphene composite carbon aerogels are prepared by cross-linking ethylenediamine and Graphene oxide using sol-gel, drying, carbonization methods, such as Hu et al (Hu, H, et al, ultralight and Highly compatible Graphene aerogels, advanced Materials,2013,25: 2219-23). Li et al (Li, Y, et al. high purity compressive Graphene monolithic via an Improved Hydrothermal process. advanced Materials,2014,26:4789-93) have Improved the sol-gel method, and have successfully prepared the Graphene aerogel with a Macroporous structure by a drying and carbonizing method. Graphene composite Carbon aerogels with better elasticity and fatigue resistance are prepared by Sun et al (Sun, H, et al. multifunctionality, Ultra-Flyweight, synthetic Assembled Carbon aerogels, advanced Materials,2013,25:2554-60) through freeze casting, freeze drying and carbonization. In patent 201510030224.1 (a method for preparing a graphene elastic composite material with a layered structure), graphene oxide nanosheets are added into a water-soluble polymer solution, and the elastic composite material with the layered structure is prepared through oriented freezing, de-icing, drying and carbonizing. However, the addition of the polymer in the above method increases the viscosity of the graphene oxide dispersion liquid, making it difficult for graphene oxide to be well dispersed in an aqueous solution, and thus the resulting carbon material has high density, insufficient degree of compression and flexibility, and limits the high compressibility and sensitive response to minute pressure and strain of the carbon material. Therefore, the key to preparing the graphene oxide and graphene carbon materials with low density, high compression and high elasticity is how to prevent stacking of the graphene oxide and graphene in the dispersion and carbonization processes and form a certain connection between the graphene oxide and graphene layers.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of elastic carbon aerogel.
Another object of the present invention is to provide an elastic carbon aerogel prepared by the above method.
It is a further object of the present invention to provide the use of the above-described elastomeric carbon aerogel in pressure sensing electronic devices.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the elastic carbon aerogel comprises the following preparation steps:
(1) dispersing graphene oxide in water, stirring, ultrasonically dispersing uniformly, and then sequentially freezing, unfreezing and ultrasonically treating the obtained dispersion liquid by using liquid nitrogen to obtain a graphene oxide suspension;
(2) adding nano microcrystalline cellulose into the graphene oxide suspension obtained in the step (1), and adding a small molecular carbon source or a small molecular nitrogen source after ultrasonic treatment to obtain a graphene oxide/nano microcrystalline cellulose suspension;
(3) freezing the graphene oxide/nano microcrystalline cellulose suspension obtained in the step (2) by liquid nitrogen, and then freezing and drying to obtain graphene oxide/nano microcrystalline cellulose composite aerogel;
(4) and (4) heating the composite aerogel obtained in the step (3) to 500-850 ℃ in an inert atmosphere, and preserving heat for 0-12 hours to obtain the elastic carbon aerogel.
Preferably, the concentration of the graphene oxide dispersed in water in the step (1) is 0.005% -0.5%; the stirring time is 1-48 h, and the ultrasonic dispersion time is 1-24 h. More preferably, the concentration of the graphene oxide dispersed in water is 0.1%; the stirring time is 12h, and the ultrasonic dispersion time is 2 h.
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 the graphene oxide in the step (1).
Preferably, the small molecule carbon source or nitrogen source in step (2) is at least one of glucose, urea and melamine; the addition of the micromolecular carbon source or nitrogen source is equivalent to 0.5-8 times of the mass of the graphene oxide.
Preferably, the inert atmosphere in step (4) refers to a nitrogen or argon atmosphere.
Preferably, the temperature rise rate in the step (4) is 0.5-10 ℃/min; more preferably, the temperature is raised to 700 ℃ at the speed of 3-5 ℃/min and is kept for 2 h.
An elastic carbon aerogel is prepared by the method.
The application of the elastic carbon aerogel in a sensing device.
The principle of the invention is as follows: by adding the nano microcrystalline cellulose into the graphene oxide dispersion liquid, the nano microcrystalline 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 dispersibility and suspension performance in water and the like. Different from the method for preparing graphene oxide and the method for adding the high polymer into the graphene elastic carbon material at present, the addition of the nano microcrystalline cellulose plays a unique role: firstly, the nano microcrystalline cellulose has excellent suspension and dispersion properties in water, the viscosity of a solution cannot be increased, the nano microcrystalline cellulose is inserted between graphene oxide layers in the graphene oxide dispersion process to play a role in space separation, and the graphene oxide layers are prevented from being stacked in the solution, in the freezing process and in the carbonization process; secondly, the graphene oxide is supported to prevent the structure from collapsing during freeze drying, so that the low-density aerogel is formed; and thirdly, the carbon aerogel is converted into nano carbon to connect and reduce the graphene layer in the carbonization process, so that the carbon aerogel has good resilience. Therefore, the renewable nano microcrystalline cellulose has unique functions which cannot be achieved by high polymers, and is an ideal material for preparing the high-performance elastic carbon material. The carbon aerogel with the characteristics of low density, high compression, high resilience, excellent recycling performance and the like is prepared by combining the advantages of the graphene oxide and the nano microcrystalline cellulose, utilizing the dispersing, supporting and carbon connecting effects of the nano microcrystalline cellulose on the graphene oxide and further combining the carbon connecting effect of a small molecular carbon source or nitrogen source and freezing, freeze-drying and carbonizing. Due to the structural characteristics, the obtained carbon aerogel can realize sensitive detection on tiny 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) the graphene oxide keeps high dispersion in the preparation process, and stacking is prevented;
(2) the prepared carbon aerogel has low density;
(3) the prepared carbon aerogel has high compressibility, high elasticity and cycling stability;
(4) the prepared carbon aerogel has stable conductivity;
(5) the prepared carbon aerogel has ultrahigh sensitivity to micro deformation, wide sensing range and excellent cycling stability, and can be widely applied to the sensing field.
Drawings
FIG. 1 is a graph of height versus stress-strain for an elastic carbon aerogel prepared in example 1, before and after compression.
FIG. 2 stress-strain curves of the elastic carbon aerogel prepared in example 1 at 99% compressive strain for runs 1, 10, and 100.
FIG. 3 is a graph of normalized resistance at different strains at 10, 1000, and 10000 compressions (left) versus current stability at 1-10000 compressions (right) for the elastomeric carbon aerogel prepared in example 1.
FIG. 4 is a graph showing the results of the induction of 1 μm micro deformation by the elastic carbon aerogel prepared in example 1.
FIG. 5 is a graph showing the results of sensing the elastic carbon aerogel prepared in example 1 at a minute weight of 10mg (corresponding to a minute pressure of 0.25 Pa).
FIG. 6 stress-strain curves of elastic carbon aerogel prepared in example 2 at compressive strain of 70% at 1 st, 10 th, 1000 th and 10000 th.
FIG. 7 stress-strain curves of 1 st, 10 th, 1000 th, and 10000 th times of the elastic carbon aerogel prepared in example 3, when the compressive strain is 70%.
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) Dispersing graphene oxide in a certain amount of water with the concentration of 0.1%, stirring for 12 hours, and then performing ultrasonic dispersion for 2 hours; performing liquid nitrogen freezing and unfreezing treatment, and then performing ultrasonic treatment again for 0.5 hour; and circularly freezing, unfreezing and ultrasonically treating for 2 times to obtain the graphene oxide suspension.
(2) Adding nano microcrystalline cellulose with the mass 4 times that of the graphene oxide into the graphene oxide suspension obtained in the step (1), and performing ultrasonic treatment for 0.5 hour again; adding glucose with the mass 2 times of that of the graphene oxide to obtain the graphene oxide/nano microcrystalline cellulose suspension.
(3) And (3) placing the graphene oxide/nano microcrystalline cellulose suspension in a plastic box, attaching the box to the outer wall of a metal box, and pouring liquid nitrogen into the metal box for freezing. And after the solution is completely frozen, carrying out freeze drying to obtain the graphene/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 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.
The elastic carbon aerogel prepared in the example has an ultralow density of 2.92mg/cm3. FIG. 1 is a graph of the height versus stress-strain curve (d) of the elastic carbon aerogel prepared in this example before cyclic compression (a), compression 1000 times (b), and compression 10000 times (c). After 1000 times of cyclic compression, no obvious plastic deformation occurs, and after 10000 times of cyclic compression, the carbon aerogel can still keep 91.8 percent of the initial height, which shows that the material has excellent elasticity and structural stability. FIG. 2 is a graph of stress-strain curves for the elastic carbon aerogel prepared in this example at 99% compressive strain for 1 st, 10 th, and 100 th cycles with nearly full compression (99% strain) for 100 th cycles, indicating a high degree of compressibility of the material. FIG. 3 shows the elastic carbon prepared in this exampleNormalized resistance (left) of the aerogel under different strains under 10 th, 1000 th and 10000 th compression and a current stability (right) chart of 1-10000 th compression, wherein the normalized resistance is almost unchanged under 10 th, 1000 th and 10000 th compression; and the current stability after 10000 times of compression is excellent, which shows that the material has good structural stability and conductive stability. FIG. 4 is a graph showing the results of the sensing of the elastic carbon aerogel prepared in this example on a 1 μm micro deformation. FIG. 5 is a graph showing the results of the sensing of the elastic carbon aerogel prepared in this example to a minute weight of 10mg (corresponding to a minute pressure of 0.25 Pa). As can be seen from the results of FIGS. 4 and 5, the obtained carbon aerogel can sensitively sense the micro deformation and pressure, which indicates that the material has ultrahigh sensitivity.
Example 2
(1) Dispersing graphene oxide in a certain amount of water with the concentration of 0.1%, stirring for 24 hours, and then performing ultrasonic dispersion for 1 hour; performing liquid nitrogen freezing and thawing treatment, and then performing ultrasonic treatment again for 1 hour; and circularly freezing, unfreezing and ultrasonically treating for 3 times to obtain the graphene oxide suspension.
(2) Adding nano microcrystalline cellulose with the mass 4 times that of the graphene oxide into the graphene oxide suspension obtained in the step (1), and performing ultrasonic treatment for 0.5 hour again; adding glucose which is 5 times of the mass of the graphene oxide to obtain the graphene oxide/nano microcrystalline cellulose suspension.
(3) And (3) placing the graphene oxide/nano microcrystalline cellulose suspension in a plastic box, attaching the box to the outer wall of a metal box, and pouring liquid nitrogen into the metal box for freezing. And after the solution is completely frozen, carrying out freeze drying to obtain the graphene/nano microcrystalline cellulose composite aerogel.
(4) And (3) placing the obtained composite aerogel in a tubular furnace, heating to 700 ℃ at the speed of 3 ℃/min in the nitrogen atmosphere, and preserving heat for 2 hours to obtain the elastic carbon aerogel.
The elastic carbon aerogel obtained in the embodiment has ultralow density of 3.98mg/cm3. Stress-strain curves of the prepared elastic carbon aerogel at compression strain of 70% at 1 st, 10 th, 1000 th and 10000 th are shown in fig. 6. Shows that the material has excellent performanceCompressibility, resilience.
Example 3
(1) Dispersing graphene oxide in a certain amount of water with the concentration of 0.1%, stirring for 12 hours, and then performing ultrasonic dispersion for 2 hours; performing liquid nitrogen freezing and unfreezing treatment, and then performing ultrasonic treatment again for 0.5 hour; and circularly freezing, unfreezing and ultrasonically treating for 2 times to obtain the graphene oxide suspension.
(2) Adding nano microcrystalline cellulose with the mass 4 times that of the graphene oxide into the graphene oxide suspension obtained in the step (1), and performing ultrasonic treatment for 0.5 hour again; and adding urea with the mass 2 times that of the graphene oxide to obtain the graphene oxide/nano microcrystalline cellulose suspension.
(3) And (3) placing the graphene oxide/nano microcrystalline cellulose suspension in a plastic box, attaching the box to the outer wall of a metal box, and pouring liquid nitrogen into the metal box for freezing. And after the solution is completely frozen, carrying out freeze drying to obtain the graphene/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 elastic carbon aerogel obtained in the embodiment has ultralow density of 2.60mg/cm3. Stress-strain curves of the prepared elastic carbon aerogel at compression strain of 70% at 1 st, 10 th, 1000 th and 10000 th are shown in fig. 7. 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 (7)
1. The preparation method of the elastic carbon aerogel is characterized by comprising the following preparation steps:
(1) dispersing graphene oxide in water, stirring, ultrasonically dispersing uniformly, and then sequentially freezing, unfreezing and ultrasonically treating the obtained dispersion liquid by using liquid nitrogen to obtain a graphene oxide suspension;
(2) adding nano microcrystalline cellulose into the graphene oxide suspension obtained in the step (1), and adding a small molecular carbon source or a small molecular nitrogen source after ultrasonic treatment to obtain a graphene oxide/nano microcrystalline cellulose suspension;
(3) freezing the graphene oxide/nano microcrystalline cellulose suspension obtained in the step (2) by liquid nitrogen, and then freezing and drying to obtain graphene oxide/nano microcrystalline cellulose composite aerogel;
(4) heating the composite aerogel obtained in the step (3) to 500-850 ℃ in an inert atmosphere, and preserving heat for 0-12 hours to obtain elastic carbon aerogel;
the adding amount of the nano microcrystalline cellulose in the step (2) is 1-10 times of the mass of the graphene oxide in the step (1);
in the step (2), the micromolecular carbon source or nitrogen source is at least one of glucose, urea and melamine; the addition of the micromolecular carbon source or nitrogen source is equivalent to 0.5-8 times of the mass of the graphene oxide.
2. The method of claim 1, wherein the carbon aerogel further comprises: in the step (1), the concentration of the graphene oxide dispersed in water is 0.005% -0.5%; the stirring time is 1-48 h, and the ultrasonic dispersion time is 1-24 h.
3. The method of claim 1, wherein the carbon aerogel further comprises: the nano microcrystalline cellulose in the step (2) is obtained by taking cellulose as a raw material and performing acid hydrolysis or oxidative degradation.
4. The method of claim 1, wherein the carbon aerogel further comprises: the inert atmosphere in the step (4) is nitrogen or argon atmosphere.
5. The method of claim 1, wherein the carbon aerogel further comprises: and (4) the temperature rising rate in the step (4) is 0.5-10 ℃/min.
6. An elastomeric carbon aerogel, comprising: prepared by the method of any one of claims 1 to 5.
7. The use of an elastomeric carbon aerogel according to claim 6 in a sensing device.
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