CN107973283A - A kind of elasticity carbon aerogels and its preparation method and application - Google Patents
A kind of elasticity carbon aerogels and its preparation method and application Download PDFInfo
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- CN107973283A CN107973283A CN201711057227.XA CN201711057227A CN107973283A CN 107973283 A CN107973283 A CN 107973283A CN 201711057227 A CN201711057227 A CN 201711057227A CN 107973283 A CN107973283 A CN 107973283A
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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 Elastic Carbon Material Field, discloses a kind of elastic carbon aerogels and its preparation method and application.Graphene oxide is dispersed in water, stirring, ultrasonic disperse are uniform, then carry out liquid nitrogen frozen, defrosting and supersound process successively, obtain graphene oxide suspension；Nano micro crystal cellulose is added, small molecule carbon source or nitrogen source is added after supersound process, obtains graphene oxide/nano micro crystal cellulose suspension；Liquid nitrogen frozen, is then freeze-dried, and is then warming up to 500~850 DEG C in an inert atmosphere and keeps the temperature 0~12h, obtains elastic carbon aerogels.The present invention combines the advantage of graphene oxide and nano micro crystal cellulose, using nano micro crystal cellulose to the scattered of graphene oxide, support and carbon connection function, and further combined with the carbon connection function of small molecule carbon source or nitrogen source, gained carbon aerogels have the characteristics such as low-density, high compression, height are sprung back, recycling performance is excellent.
Description
Technical field
The invention belongs to Elastic Carbon Material Field, and in particular to a kind of elasticity carbon aerogels and its preparation method and application.
Background technology
Elastic carbon material can the important function of deformable element depend on its compression performance, elasticity and fatigue resistance.Two
The planar structure of dimension nano-carbon material makes its design in ultrathin electrodes, flexible material and lightweight basis material with the excellent of uniqueness
Gesture.Graphene oxide, as the representative materials in two-dimensional nano-carbon material, has high conductivity and necessarily soft with graphene
Property, big size can be realized in the case of ultra-thin, therefore, is closed extensively in terms of preparing with favorable elasticity carbon material
Note.At present, the method for elastic carbon material being prepared with graphene or graphene oxide can be divided into sol-gel process and freezing casting
Method.Such as Hu et al. (Hu, H, et al.Ultralight and Highly Compressible Graphene
Aerogels.Advanced Materials,2013,25:2219-23) by being crosslinked ethylenediamine and graphene oxide, use is molten
Glue-gel, drying, carbonization method prepare the compound carbon aerogels of elastomeric graphene.Li et al. people (Li, Y, et al.Highly
Compressible Macroporous Graphene Monoliths via an Improved Hydrothermal
Process.Advanced Materials,2014,26:Sol-gel process 4789-93) is improved, passes through drying, carbonization side
Method has successfully prepared the graphene aerogel with macroporous structure.Sun et al. (Sun, H, et al.Multifunctional,
Ultra-Flyweight,Synergistically Assembled Carbon Aerogels.Advanced Materials,
2013,25:2554-60) it is prepared for by freezing casting, freeze-drying, carbonization with the preferably stone of elasticity and anti-fatigue performance
The black compound carbon aerogels of alkene.A kind of (the graphene elastic composite with layer structure of patent of invention 201510030224.1
Preparation method) stannic oxide/graphene nano piece is added in water-soluble polymer solution, by be orientated freezing, deice it is dry,
The mode of carbonization is prepared for the elastic composite with layer structure.But macromolecule is added in the above method can increase oxygen
The viscosity of graphite alkene dispersion liquid so that graphene oxide is difficult to fine dispersion in aqueous, the carbon material because obtained from
Density is high, compression degree and flexibility are inadequate, limits the high-compressibility of carbon material and the sensitive sensing to slight pressure and strain.
Therefore, prepare low-density, high compression, elastomeric graphene oxide, the key of graphene carbon material are how to prevent oxidation stone
Black alkene, graphene in scattered, carbonisation stacking and form connection certain between graphene oxide, graphene layer.
The content of the invention
For more than in place of shortcoming and defect existing in the prior art, primary and foremost purpose of the invention is to provide a kind of elasticity
The preparation method of carbon aerogels.
Another object of the present invention is to provide a kind of elastic carbon aerogels being prepared by the above method.
It is still another object of the present invention to provide application of the above-mentioned elastic carbon aerogels in pressure sensing electronic device.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of elasticity carbon aerogels, including following preparation process：
(1) graphene oxide is dispersed in water, stirring, ultrasonic disperse are uniform, then carry out gained dispersion liquid successively
Liquid nitrogen frozen, defrosting and supersound process, obtain graphene oxide suspension；
(2) nano micro crystal cellulose is added in graphene oxide suspension obtained by step (1), is added after supersound process
Small molecule carbon source or nitrogen source, obtain graphene oxide/nano micro crystal cellulose suspension；
(3) graphene oxide obtained by step (2)/nano micro crystal cellulose suspension is subjected to liquid nitrogen frozen, then freezed
It is dry, obtain graphene oxide/nano micro crystal cellulose composite aerogel；
(4) composite aerogel that step (3) obtains is warming up to 500~850 DEG C in an inert atmosphere and keeps the temperature 0~12h,
Obtain elastic carbon aerogels.
Preferably, the concentration being dispersed in water graphene oxide described in step (1) is 0.005%~0.5%；It is described
The time of stirring is 1~48h, and the time of ultrasonic disperse is 1~24h.The concentration that more preferably graphene oxide is dispersed in water
For 0.1%；The time of stirring is 12h, and the time of ultrasonic disperse is 2h.
Preferably, nano micro crystal cellulose is to pass through sour water solution or oxidation by raw material of cellulose described in step (2)
Degraded obtains；It is highly preferred that the nano micro crystal cellulose is obtained by 65% sulphuric acid hydrolysis cellulose.
Preferably, the addition of nano micro crystal cellulose described in step (2) is graphene oxide quality in step (1)
1~10 times.
Preferably, small molecule carbon source described in step (2) or nitrogen source are at least one in glucose, urea, melamine
Kind；0.5~8 times of the addition of small molecule carbon source or nitrogen source equivalent to graphene oxide quality.
Preferably, the inert atmosphere described in step (4) refers to nitrogen or argon gas atmosphere.
Preferably, the speed to heat up described in step (4) is 0.5~10 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 elasticity carbon aerogels, are prepared by the above method.
Application of the above-mentioned elasticity carbon aerogels in senser element.
The principle of the present invention is：By adding nano micro crystal cellulose in graphene oxide dispersion, nano microcrystalline is fine
Dimension usually comes from reproducible resource, has high-specific surface area, lightweight, abundant surface group, excellent mechanical strength, low
Cost, it is renewable, environmental-friendly, dispersion performance and suspendability are excellent in water the advantages that.With at present prepare graphene oxide,
Graphene elasticity carbon material adds high molecular method difference, and the addition of nano micro crystal cellulose plays the effect of uniqueness：When
Nano micro crystal cellulose has excellent suspension, dispersion performance in water, and will not increase the viscosity of solution, in graphene oxide
In scattered process be inserted into graphene oxide interlayer play the role of space obstacle, prevent graphene oxide layer in the solution, it is cold
During jelly and carbonisation stacking；Second, play support graphene oxide when freeze-drying and prevent structure collapses
Effect, advantageously form the aeroge of low-density；Third, it is transformed into nano-sized carbon in carbonisation to connect reduced graphene
Layer so that carbon aerogels have good resilience performance.Therefore, there is reproducible nano micro crystal cellulose macromolecule not had
Unique effect, be to prepare the ideal material with high-performance elastic carbon material.The present invention combines graphene oxide and nanometer is micro-
The advantage of crystalline cellulose, using nano micro crystal cellulose to the scattered of graphene oxide, support and carbon connection function, and further
With reference to the carbon connection function of small molecule carbon source or nitrogen source, by freeze, be freeze-dried and carbonization be prepared for low-density, high compression,
The carbon aerogels for the characteristics such as height is sprung back, recycling performance is excellent.Due to above-mentioned architectural characteristic, obtained carbon aerogels
The sensitive detection to slight pressure and strain can be achieved, can be applied to various pressure sensing electronic devices.
The present invention preparation method and gained elasticity carbon aerogels have the following advantages that and beneficial effect：
(1) preparation process graphene oxide keeps the scattered of height, prevents from stacking；
(2) carbon aerogels prepared have low density；
(3) carbon aerogels prepared have high-compressibility, high resiliency and cyclical stability；
(4) carbon aerogels prepared have stable electric conductivity；
(5) carbon aerogels prepared not only have miniature deformation the sensitivity of superelevation, and induction range is wide, stable circulation
Property is excellent, can be widely applied to sensory field.
Brief description of the drawings
The height and stress-strain curve before and after the compression of elastic carbon aerogels prepared by Fig. 1 embodiments 1.
Elastic carbon aerogels prepared by Fig. 2 embodiments 1 stress-should of the 1st, 10,100 time when compression strain is 99%
Varied curve figure.
Returning under elastic carbon aerogels prepared by Fig. 3 embodiments 1 are differently strained in the 10th, 1000,10000 second compression
One changes current stability (right side) figure of resistance (left side) and 1-10000 second compressions.
The sensing result figure of elastic carbon aerogels prepared by Fig. 4 embodiments 1 to 1 μm of miniature deformation.
Elastic carbon aerogels prepared by Fig. 5 embodiments 1 are to the small weight of 10mg (equivalent to 0.25Pa slight pressures)
Sense result figure.
Elastic carbon aerogels prepared by Fig. 6 embodiments 2 are when compression strain is 70% the 1st, 10,1000,10000 time
Stress-strain curve.
Elastic carbon aerogels prepared by Fig. 7 embodiments 3 are when compression strain is 70% the 1st, 10,1000,10000 time
Stress-strain curve.
Embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) graphene oxide is dispersed in a certain amount of water, concentration 0.1%, when stirring 12 is small, then carries out ultrasound
It is scattered 2 it is small when；When ultrasound 0.5 is small again after progress liquid nitrogen frozen, processing of thawing；Circulating frozen, defrosting, ultrasound 2 times, obtain
Graphene oxide suspension.
(2) nano micro crystal cellulose that will be equivalent to 4 times of graphene oxide quality is added to graphite oxide obtained by step (1)
In alkene suspension, when ultrasound 0.5 is small again；Glucose of 2 times equivalent to graphene oxide quality is added, obtains graphite oxide
Alkene/nano micro crystal cellulose suspension.
(3) above-mentioned graphene oxide/nano micro crystal cellulose suspension is placed in plastic casing, box is lain in into can
Sub- outer wall, in metal box pouring into liquid nitrogen is freezed.Treat that solution is freeze-dried after having freezed completely, graphite is made
Alkene/nano micro crystal cellulose composite aerogel.
(4) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the speed of 5 DEG C/min
700 DEG C and 2h is kept the temperature, obtain elastic carbon aerogels.
The compression performance and compression-resistance of gained elasticity carbon aerogels, compression-electric current sensing behavior are tried in electronic universal
Test on machine and carry out, use the sensor of 100N；Resistance during using the record material compression of high-precision universal meter；Using electrochemistry
Curent change during work station record compression.
Elastic carbon aerogels have ultralow density made from the present embodiment, are 2.92mg/cm3.Fig. 1 is the present embodiment institute
(a) before the elastic carbon aerogels circulation compression of preparation, compression 1000 times (b) and compress the height after 10000 times (c) and stress-
Strain curve (d) figure.It is no after 1000 circulation compressions that obvious plastic deformation occurs, after 10000 circulation compressions,
Carbon aerogels remain to keep the 91.8% of elemental height, show that material has excellent elasticity and structural stability.Fig. 2 is this reality
Elastic carbon aerogels prepared by example are applied when compression strain is 99% stress-strain curve of the 1st, 10,100 time, several
Recycled 100 times in the case of compression (strain is 99%) completely, show that material has the compressibility of height.Fig. 3 is
Normalized resistance under elastic carbon aerogels prepared by the present embodiment are differently strained in the 10th, 1000,10000 second compression
Current stability (right side) figure of (left side) and 1-10000 second compressions, normalized resistance in the 10th, 1000,10000 second compression almost
It is constant；And it is excellent by 10000 second compression current stabilities, show that material has good structural stability and conductive stable
Property.Fig. 4 is that the elastic carbon aerogels prepared by the present embodiment carry out 1 μm of miniature deformation sensitive sensing result figure.Fig. 5 is this
The sensing result figure of elastic carbon aerogels prepared by embodiment to the small weight of 10mg (equivalent to 0.25Pa slight pressures).By
Fig. 4 and Fig. 5 results, which can be seen that gained carbon aerogels, sensitively to sense miniature deformation and pressure, show that material has
There is the sensitivity of superelevation.
Embodiment 2
(1) graphene oxide is dispersed in a certain amount of water, concentration 0.1%, when stirring 24 is small, then carries out ultrasound
It is scattered 1 it is small when；When ultrasound 1 is small again after progress liquid nitrogen frozen, processing of thawing；Circulating frozen, defrosting, ultrasound 3 times, obtain oxygen
Graphite alkene suspension.
(2) nano micro crystal cellulose that will be equivalent to 4 times of graphene oxide quality is added to graphite oxide obtained by step (1)
In alkene suspension, when ultrasound 0.5 is small again；Glucose of 5 times equivalent to graphene oxide quality is added, obtains graphite oxide
Alkene/nano micro crystal cellulose suspension.
(3) above-mentioned graphene oxide/nano micro crystal cellulose suspension is placed in plastic casing, box is lain in into can
Sub- outer wall, in metal box pouring into liquid nitrogen is freezed.Treat that solution is freeze-dried after having freezed completely, graphite is made
Alkene/nano micro crystal cellulose composite aerogel.
(4) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the speed of 3 DEG C/min
700 DEG C and 2h is kept the temperature, obtain elastic carbon aerogels.
Elastic carbon aerogels have ultralow density obtained by the present embodiment, are 3.98mg/cm3.Prepared Elastic Carbon gas
Gel compression strain be 70% when the 1st, 10,1000,10000 time stress-strain curve it is as shown in Figure 6.Show material
With excellent compressibility, resilience.
Embodiment 3
(1) graphene oxide is dispersed in a certain amount of water, concentration 0.1%, when stirring 12 is small, then carries out ultrasound
It is scattered 2 it is small when；When ultrasound 0.5 is small again after progress liquid nitrogen frozen, processing of thawing；Circulating frozen, defrosting, ultrasound 2 times, obtain
Graphene oxide suspension.
(2) nano micro crystal cellulose that will be equivalent to 4 times of graphene oxide quality is added to graphite oxide obtained by step (1)
In alkene suspension, when ultrasound 0.5 is small again；Add urea of 2 times equivalent to graphene oxide quality, obtain graphene oxide/
Nano micro crystal cellulose suspension.
(3) above-mentioned graphene oxide/nano micro crystal cellulose suspension is placed in plastic casing, box is lain in into can
Sub- outer wall, in metal box pouring into liquid nitrogen is freezed.Treat that solution is freeze-dried after having freezed completely, graphite is made
Alkene/nano micro crystal cellulose composite aerogel.
(4) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the speed of 5 DEG C/min
700 DEG C and 2h is kept the temperature, obtain elastic carbon aerogels.
Elastic carbon aerogels have ultralow density obtained by the present embodiment, are 2.60mg/cm3.Prepared Elastic Carbon gas
Gel compression strain be 70% when the 1st, 10,1000,10000 time stress-strain curve it is as shown in Figure 7.Show material
With excellent compressibility, resilience.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of elasticity carbon aerogels, it is characterised in that including following preparation process：
(1) graphene oxide is dispersed in water, stirring, ultrasonic disperse are uniform, and gained dispersion liquid is then carried out liquid nitrogen successively
Freezing, thaw and be ultrasonically treated, and obtains graphene oxide suspension；
(2) nano micro crystal cellulose is added in graphene oxide suspension obtained by step (1), small point is added after supersound process
Sub- carbon source or nitrogen source, obtain graphene oxide/nano micro crystal cellulose suspension；
(3) graphene oxide obtained by step (2)/nano micro crystal cellulose suspension is subjected to liquid nitrogen frozen, is then freeze-dried,
Obtain graphene oxide/nano micro crystal cellulose composite aerogel；
(4) composite aerogel that step (3) obtains is warming up to 500~850 DEG C in an inert atmosphere and keeps the temperature 0~12h, obtained
Elastic carbon aerogels.
A kind of 2. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (1)
The concentration that graphene oxide is dispersed in water is 0.005%~0.5%；The time of the stirring is 1~48h, ultrasonic disperse
Time be 1~24h.
A kind of 3. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (2)
Nano micro crystal cellulose is to be obtained using cellulose as raw material by sour water solution or oxidative degradation.
A kind of 4. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (2)
The addition of nano micro crystal cellulose is 1~10 times of graphene oxide quality in step (1).
A kind of 5. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (2)
Small molecule carbon source or nitrogen source are at least one of glucose, urea, melamine；The addition of small molecule carbon source or nitrogen source is suitable
In 0.5~8 times of graphene oxide quality.
A kind of 6. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (4)
Inert atmosphere refer to nitrogen or argon gas atmosphere.
A kind of 7. preparation method of elastic carbon aerogels according to claim 1, it is characterised in that：Described in step (4)
The speed of heating is 0.5~10 DEG C/min.
A kind of 8. elasticity carbon aerogels, it is characterised in that：It is prepared by claim 1~7 any one of them method.
A kind of 9. application of elastic carbon aerogels in senser element described in claim 8.
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| CN108751178A (en) * | 2018-07-09 | 2018-11-06 | 合肥艾飞新材料有限公司 | A kind of carbonized graphite alkene and preparation method thereof |
| CN109019597A (en) * | 2018-07-17 | 2018-12-18 | 华南理工大学 | A kind of preparation method and applications of cellulose/graphene oxide carbon aerogels |
| CN109095449A (en) * | 2018-08-24 | 2018-12-28 | 华南理工大学 | A kind of carbon aerogels and its preparation and application in the sensor with superelevation linear sensitivity |
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| CN114195122A (en) * | 2021-12-22 | 2022-03-18 | 北京理工大学 | Composite porous carbon aerogel material and preparation method and application thereof |
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