CN109095449A - A kind of carbon aerogels and its preparation and application in the sensor with superelevation linear sensitivity - Google Patents
A kind of carbon aerogels and its preparation and application in the sensor with superelevation linear sensitivity Download PDFInfo
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- CN109095449A CN109095449A CN201810972732.5A CN201810972732A CN109095449A CN 109095449 A CN109095449 A CN 109095449A CN 201810972732 A CN201810972732 A CN 201810972732A CN 109095449 A CN109095449 A CN 109095449A
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- mxene
- carbon aerogels
- linear sensitivity
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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 material, a kind of carbon aerogels with superelevation linear sensitivity and its preparation and application in the sensor are disclosed.Method: (1) in water, MXene material is subjected to ultrasound removing dispersion, obtains MXene suspension；(2) nano micro crystal cellulose is added in suspension, is ultrasonically treated, liquid nitrogen frozen, freeze-drying obtains composite aerogel；Composite aerogel is carbonized in an inert atmosphere, obtains elastic carbon aerogels.The advantage of present invention combination MXene and nano micro crystal cellulose, dispersion, support and connection function using nano micro crystal cellulose to MXene, invigoration effect in conjunction with MXene lamella to aeroge is prepared for high compression by freezing, freeze-drying and carbonization, height is sprung back, it is excellent that performance is recycled and has the carbon aerogels of the characteristics such as superelevation linear sensitivity.Carbon aerogels of the invention are applied to Sense Electronics.
Description
Technical field
The invention belongs to the technical fields of flexible carbon material, and in particular to a kind of carbon airsetting with superelevation linear sensitivity
Glue and preparation method thereof and application in the sensor.
Background technique
Important function of the flexible carbon material in senser element depends on its compression performance, elasticity, fatigue resistance and spirit
Sensitivity.It is only that the planar structure of two-dimension nano materials has it in the design of ultrathin electrodes, flexible material and lightweight basis material
Special advantage.MXene has high conductivity and certain flexibility as the new material in two-dimensional nano-carbon material, can be super
Big size is realized in the case where thin.Therefore, there is huge prospect in terms of preparing the flexible material with excellent sensing capabilities.
Traditional carbon-based flexible material uses graphene and carbon nanotube as substrate, such as Graphene/carbon nanotube composite material more
(19.8kPa-1)(Jian M,Xia K,Wang Q,et al.Flexible and Highly Sensitive Pressure
Sensors Based on Bionic Hierarchical Structures.Advanced Functional
Materials, 2017,27 (9): 1606066.), graphene paper (17.2kPa-1)(Tao L Q,Zhang K N,Tian H,et
al.Graphene-Paper Pressure Sensor for Detecting Human Motions.Acs Nano,2017,
11 (9): 8790.), graphene/dimethyl silicone polymer (1.80kPa-1)(Bae G Y,Pak S W,Kim D,et
al.Linearly and Highly Pressure-Sensitive Electronic Skin Based on a
Bioinspired Hierarchical Structural Array.Advanced Materials,2016,28(26):
5300-5306.) etc..But due to graphene and carbon nanotube defect easy to form during the preparation process, material is to high-quality
Graphene or carbon nanotube have strong accordance with tolerance, and pressure sensor obtained uses flexible substrates more in the above method, can know
Other stress is larger, it is difficult to realize the sensing sensitive under minimal stress.
Therefore, it is real using flexible carbon material substrate combination Rational structure for preparing the key of the carbon aerogels of hypersensitivity
The highly sensitive sensing of existing stress.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing one kind has
The preparation method of superelevation linear sensitivity carbon aerogels.
It is prepared by the above method with superelevation linear sensitivity another object of the present invention is to provide a kind of
Carbon aerogels.
A further object of the present invention is to provide the application of the carbon aerogels of above-mentioned superelevation linear sensitivity in the sensor,
Application especially in pressure sensing electronic device.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the carbon aerogels with superelevation linear sensitivity, includes the following steps:
(1) in water, MXene material is subjected to ultrasound removing dispersion, obtains MXene suspension；
(2) nano micro crystal cellulose is added in MXene suspension obtained by step (1), ultrasonic treatment obtains MXene/
Nano micro crystal cellulose suspension；
(3) MXene/ nano micro crystal cellulose suspension obtained by step (2) is subjected to liquid nitrogen frozen, is then freeze-dried,
Obtain MXene/ nano micro crystal cellulose composite aerogel；
(4) by the composite aerogel that step (3) obtains be warming up in an inert atmosphere 500~1200 DEG C and keep the temperature 0~
12h obtains elastic carbon aerogels.
MXene material described in step (1) is Ti3C2。
In MXene suspension described in step (1) concentration of MXene be 0.01wt%~5wt%, preferably 0.1%；It is super
The time of sound removing is 0.1~24 hour, preferably 2h.
Preferably, nano micro crystal cellulose described in step (2) is to pass through sour water solution or oxidation by raw material of cellulose
Degradation obtains；It is highly preferred that the nano micro crystal cellulose is obtained by 65% sulphuric acid hydrolysis cellulose.
Preferably, the additional amount of nano micro crystal cellulose described in step (2) be step (1) in MXene mass 1~
10 times.
Preferably, inert atmosphere described in step (4) refers at least one of nitrogen or argon atmosphere.
Preferably, the rate of heating described in step (4) is 0.1~50 DEG C/min；More preferably with the speed of 3~5 DEG C/min
Rate is warming up to 700 DEG C and keeps the temperature 2h.
A kind of carbon aerogels with High Linear sensitivity, are prepared by the above method.
The application of the carbon aerogels of above-mentioned High Linear sensitivity in the sensor, the especially application in strain gauge.
The principle of the present invention are as follows: pass through the advantage of both cellulose-binding nano microcrystalline and MXene, nano micro crystal cellulose
From reproducible resource, have high-specific surface area, lightweight, surface group abundant, excellent mechanical strength, it is low at
Originally, the advantages that renewable, environmental-friendly, dispersion performance and suspendability are excellent in water.And MXene is as a kind of novel two
Material is tieed up, because it is with excellent physicochemical properties such as excellent electric conductivity, thermal stability and excellent flexibilities, in absorption point
It has broad application prospects from, fields such as energy storage, sensing and electro-catalysis.Graphene oxide, graphene are prepared with current
And the method for the elastic carbon material such as carbon nanotube is different, nano micro crystal cellulose and MXene have a good synergistic effect: one
It is that nano micro crystal cellulose has excellent suspension, dispersion performance in water, and not will increase the viscosity of solution, at MXene points
In dispersion liquid be inserted into nano micro crystal cellulose play the role of space obstacle, prevent MXene lamella in the solution, in refrigerating process and
The stacking of carbonisation；Nano micro crystal cellulose is transformed into nano-sized carbon to connect MXene piece in carbonisation, so that carbon airsetting
Glue has good resilience performance, while MXene lamella can be formed in freezing dry process with aided nano microcrystalline cellulose
Lamellar structure prevents nano micro crystal cellulose from interweaving, so that material has excellent circulation compression performance.The present invention combines
The advantage of MXene and nano micro crystal cellulose, dispersion, support and connection function using nano micro crystal cellulose to MXene are led to
It crosses freezing, freeze-drying and carbonization and is prepared for that high compression, high rebound, that performance is recycled is excellent and have superelevation linear sensitivity
Etc. characteristics carbon aerogels.Since the carbon aerogels with above-mentioned architectural characteristic, obtained can be realized to slight pressure and strain
Highly sensitive detection, can be applied to various pressure sensing electronic devices.
Preparation method and gained elasticity carbon aerogels of the invention have the following advantages that and the utility model has the advantages that
(1) preparation process MXene keeps the dispersion of height, prevents from stacking；
(2) carbon aerogels prepared have high-compressibility, high resiliency and cyclical stability；
(3) carbon aerogels prepared have the linear sensitivity of superelevation；
(4) carbon aerogels prepared not only have the sensitivity of superelevation to miniature deformation, and cyclical stability is excellent, can be wide
It is general to be applied to sensory field.
Detailed description of the invention
Fig. 1 is to have the elastic carbon aerogels of superelevation linear sensitivity under differently curved degree prepared by embodiment 1
Current-responsive figure (a) and under different compression strains stress-strain curve (b be the compression strain of 10%-60% difference under, c is
60%-90% compression strain)；
Fig. 2 is that the elastic carbon aerogels prepared by embodiment 1 with superelevation linear sensitivity in compression strain are 50%
When the 10th, 100,1000 and 10000 stress-strain curve；
Fig. 3 be elastic carbon aerogels prepared by embodiment 2 with superelevation linear sensitivity 10%, 30%,
50%, the current-responsive under 70% and 90% compression strain；
Fig. 4 is to have the elastic carbon aerogels of superelevation linear sensitivity under 50% compression strain prepared by embodiment 2
Electric current incude cyclical stability；
Fig. 5 is to have the elastic carbon aerogels of superelevation linear sensitivity when stress is greater than 10 pa prepared by embodiment 2
Linear sensitivity (a) and stress less than 10 pa when linear sensitivity (b)；
Fig. 6 is to have the elastic carbon aerogels of superelevation linear sensitivity to human pulse signal prepared by embodiment 3
Electric current induction.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) by MXene (Ti3C2) material is added in ultrapure water or deionized water, then ultrasound removing dispersion 2 hours, obtain
The MXene suspension for being 0.05wt% to concentration；
(2) it will be equivalent to 3 times of MXene mass of nano micro crystal cellulose and be added to MXene suspension obtained by step (1)
In, ultrasound 0.5 hour, obtains MXene/ nano micro crystal cellulose suspension again；
(3) above-mentioned MXene/ nano micro crystal cellulose suspension is placed in plastic casing, box is lain in outside metal box
Wall pours into liquid nitrogen in metal box and is freezed (icing, 15 minutes), is freezed after having freezed completely to solution
MXene/ nano micro crystal cellulose composite aerogel is made in dry (- 52 DEG C, for 24 hours)；
(4) composite aerogel is placed in tube furnace, is warming up to 600 DEG C simultaneously with the rate of 3 DEG C/min in nitrogen atmosphere
Heat preservation 4 hours, obtains elastic carbon aerogels.
Gained carbon aerogels have excellent elasticity, and the compression performance electronic universal tester of elastic carbon aerogels is enterprising
Row, uses the sensor of 5 0N.
Fig. 1 is to have the elastic carbon aerogels of superelevation linear sensitivity under differently curved degree prepared by embodiment 1
Current-responsive figure (a) and under different compression strains stress-strain curve (b be the compression strain of 10%-60% difference under, c is
60%-90% compression strain).Fig. 1 (a) is that the electric current under the elastic differently curved degree of carbon aerogels prepared by the present embodiment is rung
Ying Tu.Under differently curved degree, there is different current-responsives, show that material has excellent elasticity and structural stability,
It can be applied to wearable electronic device.Fig. 1 (b) is load-deformation curve of the material under 10%-60% difference compression strain,
Show that material has wide range of strain and excellent compressibility.Under Fig. 1 (c) is differently strained when 60%-90% compresses
Stress-strain diagram, show material have high-compressibility.The circulation compression performance of elasticity carbon aerogels manufactured in the present embodiment
(Fig. 2 is that the elastic carbon aerogels prepared by embodiment 1 with superelevation linear sensitivity are in compression strain as shown in Figure 2
10th, 100,1000 and 10000 stress-strain curve when 50%), it is followed under 50% compression strain by 10000 times
After ring compression, the maximum stress of material remains to reservation 87.9%, shows that material has excellent cyclical stability.
Embodiment 2
(1) by MXene (Ti3C2) be added in ultrapure water or deionized water, then ultrasound removing dispersion 1 hour, obtains concentration
For the MXene suspension of 0.1wt%；
(2) it will be equivalent to 5 times of MXene mass of nano micro crystal cellulose and be added to MXene suspension obtained by step (1)
In, ultrasound 1 hour, obtains MXene/ nano micro crystal cellulose suspension again；
(3) above-mentioned MXene/ nano micro crystal cellulose suspension is placed in plastic casing, box is lain in outside metal box
Wall pours into liquid nitrogen in metal box and is freezed (icing, 15 minutes), is freezed after having freezed completely to solution
MXene/ nano micro crystal cellulose composite aerogel is made in dry (- 52 DEG C, for 24 hours)；
(4) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the rate of 5 DEG C/min
700 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
Stress-electric current, strain-electric current induction and the spirit of the resulting elastic carbon aerogels with superelevation linear sensitivity
Sensitivity test carries out on electronic universal tester, uses the sensor of 5 0N；Electricity when compressing is noted down using electrochemical workstation
Rheology.
Elastic carbon aerogels obtained by the present embodiment have excellent current-responsive behavior and high linear sensitivity.
Fig. 3 is elastic carbon aerogels obtained by the present embodiment respectively in 10%, 30%, 50%, 70% and 90% compression strain
Under current-responsive, illustrate material with wide induction range.The elastic carbon aerogels of the present embodiment are in 50% compression strain
Under electric current induction cyclical stability as shown in figure 4, after the compression of 2000 circulations, current signal shows without being substantially reduced
There is this sensing material excellent electric current to incude cyclical stability.Fig. 5 is to have superelevation linearly sensitive prepared by embodiment 2
Linear sensitivity when linear sensitivity (a) and stress of the elastic carbon aerogels of degree when stress is greater than 10 pa are less than 10 pa
(b).Linear sensitivity of the elastic carbon aerogels within the scope of different pressures obtained by the present embodiment, sensitivity is in stress less than 10
Up to 114.64kPa when pa-1, sensitivity is 42.92kPa when being greater than 10 pa-1。
Embodiment 3
(1) by MXene (Ti3C2) be added in ultrapure water or deionized water, then ultrasound removing dispersion 4 hours, obtain dense
Degree is the MXene suspension of 1wt%；
(2) it will be equivalent to 4 times of MXene mass of nano micro crystal cellulose and be added to MXene suspension obtained by step (1)
In, ultrasound 3 hours, obtain MXene/ nano micro crystal cellulose suspension again；
(3) above-mentioned MXene/ nano micro crystal cellulose suspension is placed in plastic casing, box is lain in outside metal box
Wall pours into liquid nitrogen in metal box and is freezed (icing, 15 minutes), is freezed after having freezed completely to solution
MXene/ nano micro crystal cellulose composite aerogel is made in dry (- 52 DEG C, for 24 hours)；
(4) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the rate of 5 DEG C/min
700 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The wearing test of the aeroge of the obtained sensitivity with superelevation is detected by digital sourcemeter.
Carbon aerogels obtained by the present embodiment have the sensitivity of superelevation, can be applied in wearable electronic.It is prepared
Elastic carbon aerogels be applied to wearable electronic.Fig. 6 is the bullet prepared by embodiment 3 with superelevation linear sensitivity
Property carbon aerogels the electric current of human pulse signal is incuded.As shown in fig. 6, the available clear induction of the pulse signal of human body,
Show that carbon aerogels manufactured in the present embodiment can be applied among flexible electronic device.
Carbon aerogels of the elasticity carbon aerogels prepared by the present invention relative to application number 201711057227.X patent application,
With better stability, (height after material circulation 10000 times of application number 201711057227.X patent application is left
91.8%, stress is left 71.2%；Material of the invention is highly left the reservation of 95.4%, stress after compressing 10000 times
87.9%) linear sensitivity, and with application number 201711057227.X patent application not having.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of the carbon aerogels with superelevation linear sensitivity, characterized by the following steps:
(1) in water, MXene material is subjected to ultrasound removing dispersion, obtains MXene suspension；
(2) nano micro crystal cellulose is added in MXene suspension obtained by step (1), ultrasonic treatment obtains MXene/ nanometers
Microcrystalline cellulose suspension；
(3) MXene/ nano micro crystal cellulose suspension obtained by step (2) is subjected to liquid nitrogen frozen, is then freeze-dried, obtains
MXene/ nano micro crystal cellulose composite aerogel；
(4) composite aerogel that step (3) obtains is warming up to 500~1200 DEG C in an inert atmosphere and keeps the temperature 0~12h, is obtained
To elastic carbon aerogels.
2. the preparation method of the carbon aerogels with superelevation linear sensitivity according to claim 1, it is characterised in that:
MXene material described in step (1) is Ti3C2；
The concentration of MXene is 0.01wt%~5wt% in MXene suspension described in step (1).
3. the preparation method of the carbon aerogels with superelevation linear sensitivity according to claim 1, it is characterised in that: step
(2) additional amount of nano micro crystal cellulose described in is 1~10 times of MXene mass in step (1).
4. the preparation method of the carbon aerogels with superelevation linear sensitivity according to claim 1, it is characterised in that: step
(1) time of ultrasound removing is 0.1~24 hour in；
Inert atmosphere described in step (4) refers at least one of nitrogen or argon atmosphere.
5. the preparation method of the carbon aerogels with superelevation linear sensitivity according to claim 1, it is characterised in that: step
(2) nano micro crystal cellulose described in is to be obtained using cellulose as raw material by sour water solution or oxidative degradation.
6. the preparation method of the carbon aerogels with superelevation linear sensitivity according to claim 1, it is characterised in that: step
(4) rate of heating described in is 0.1~50 DEG C/min.
7. a kind of carbon aerogels with superelevation linear sensitivity obtained by any one of claim 1~6 preparation method.
8. the application of the carbon aerogels with superelevation linear sensitivity in the sensor according to claim 7.
9. application according to claim 8, it is characterised in that: the sensor is strain gauge.
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| CN112911920A (en) * | 2021-02-08 | 2021-06-04 | 西安理工大学 | Preparation method of MXene-carbon aerogel/TPU composite material |
| 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 |
| CN113101877A (en) * | 2021-04-06 | 2021-07-13 | 南京林业大学 | Preparation method of MXene-based composite aerogel |
| CN113645820A (en) * | 2021-07-12 | 2021-11-12 | 西安理工大学 | Preparation method of MXene-CNT/carbon aerogel composite material |
| CN113645820B (en) * | 2021-07-12 | 2023-12-26 | 西安理工大学 | Preparation method of MXene-CNT/carbon aerogel composite material |
| CN114620706A (en) * | 2022-02-10 | 2022-06-14 | 深圳市丽德宝纸品有限公司 | Wood-based carbon sponge with efficient electromagnetic shielding performance and preparation method and application 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 |
| CN114849599A (en) * | 2022-03-18 | 2022-08-05 | 山东大学 | Nano-cellulose composite carbon aerogel ball and preparation method and application thereof |
| CN114653393A (en) * | 2022-03-29 | 2022-06-24 | 天津科技大学 | High-efficiency photocatalyst, preparation method and application |
| CN115014597A (en) * | 2022-04-29 | 2022-09-06 | 深圳大学 | Flexible pressure sensor based on porous structure composite material and preparation method thereof |
| CN115014597B (en) * | 2022-04-29 | 2023-09-22 | 深圳大学 | Flexible pressure sensor based on porous structure composite material and preparation method thereof |
| CN115347251A (en) * | 2022-10-20 | 2022-11-15 | 安徽大学 | Preparation method of piezoelectric flexible self-powered sensor battery |
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