CN109851313A - A kind of highly sensitive, the wide line sensing scope compressible compound carbon aerogels and its preparation and application - Google Patents
A kind of highly sensitive, the wide line sensing scope compressible compound carbon aerogels and its preparation and application Download PDFInfo
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- CN109851313A CN109851313A CN201910059048.2A CN201910059048A CN109851313A CN 109851313 A CN109851313 A CN 109851313A CN 201910059048 A CN201910059048 A CN 201910059048A CN 109851313 A CN109851313 A CN 109851313A
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Abstract
The invention belongs to Elastic Carbon Material Fields, disclose highly sensitive, the wide line sensing scope the compressible compound carbon aerogels of one kind and its preparation and application.MXene nanometer sheet: 1) being dispersed in water by the method, obtains MXene suspension；2) water-soluble trivalent ferric salt, acid, MXene suspension are uniformly mixed with chitosan, freezing processing, it is dry, obtain composite aerogel；3) composite aerogel is heat-treated in an inert atmosphere, obtains compound carbon aerogels；Heat treatment, which refers to, to be warming up to 500~1200 DEG C and keeps the temperature 0~12h.Method of the invention is simple, environmental-friendly；Prepared carbon aerogels have high-compressibility, high resilience and excellent cyclical stability；Prepared carbon aerogels also have the sensitivity of superelevation simultaneously, and wide scope linear sensing is applied to senser element.
Description
Technical field
The invention belongs to Elastic Carbon Material Fields, and in particular to a kind of to press with highly sensitive, the wide line sensing scope
Contract compound carbon aerogels and its preparation method and application.
Background technique
External pressure or strain can be converted to current signal in compression process due to it by compressible elastomeric carbon aerogels
Performance, can be assembled into piezoresistive transducer applied to fields such as human-computer interaction, biomedical monitoring and motion detections.Tradition can
Carbon material is compressed mostly by nano-carbon material such as carbon nanotube, graphene and its building such as derivative and nano carbon composite material.But
That these nano-carbon material multi-sources face environmental pollution in non-renewable fossil resources, it is unsustainable the problems such as, and prepare
Method is complicated, with high costs.
MXene has unique physicochemical properties as a kind of emerging two-dimensional material, including high charge carrier moves
Shifting rate, metallic conductivity, very good mechanical properties etc. are widely used in the fields such as energy storage, electromagnetic shielding, seperation film.For MXene
Sensing capabilities and its correlative study of sensor field also there is document to be related to.There is document report with reticular structure
MXene/rGO aeroge (3D Synergistical MXene/Reduced Graphene Oxide Aerogel for a
Piezoresistive Sensor.Acs Nano2018), the aeroge is compressible.But the maximum compressibility of the aeroge is only
60%, High Linear sensitivity can not be obtained in wide pressure or range of strain, the scope of application is limited, and service life is difficult to be protected
Card；And lower (the 22.56kPa of sensitivity-1), application is also limited.In addition, using graphene oxide but also the cost of the material
It is high, it is difficult to realize practical application.Biomass is low for constructing as rich reserves in nature, the carbon source of cheap reproducible
The desirable feedstock of cost, sustainable carbon material.But the difficulty that single creature matter raw material is designed due to its structure, in carbonisation
Substantially shrinkage and its derived carbon brittleness, the mechanical performance of this kind of material is often poor, it is difficult to industrial application.Therefore, it makes
The standby carbon material with high resiliency, excellent fatigue resistance, high sensitivity, wide scope linear sensing is in terms of wearable sensors part
It is of great significance.
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
Excellent fatigue resistance, high sensitivity, compressible compound carbon aerogels of the wide line sensing scope and preparation method thereof.Of the invention
Compressible compound carbon aerogels have the characteristics that excellent antifatigue, highly sensitive, the wide line sensing scope.
Another object of the present invention is to provide application of the above-mentioned compressible compound carbon aerogels in senser element, especially
It is the application in pressure sensing electronic device.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of highly sensitive, the wide line sensing scope compressible compound carbon aerogels, includes the following steps:
1) MXene nanometer sheet is dispersed in water, obtains MXene suspension；
2) water-soluble trivalent ferric salt, acid, MXene suspension are uniformly mixed with chitosan, freezing processing, it is dry, it obtains
Composite aerogel；
3) composite aerogel is heat-treated in an inert atmosphere, obtains compound carbon aerogels；The heat treatment refers to
It is warming up to 500-1200 DEG C and keeps the temperature 0~12h.
The temperature of the heat treatment is preferably 600~900 DEG C, and more preferably 700~900 DEG C；The time of heat treatment is preferred
For 1~3h.
MXene nanometer sheet described in step 1) is Ti3C2.The concentration of MXene suspension described in step 1) be 0.5~
10mg/mL, preferably 1~5mg/mL.
Water-soluble trivalent ferric salt described in step 2) is ferric trichloride, ferric nitrate, the sulphur containing the crystallization water or without the crystallization water
More than one in sour iron；Preferably ferric trichloride.
Acid described in step 2) is glacial acetic acid, dilute hydrochloric acid, dilute sulfuric acid, preferably glacial acetic acid；
The temperature of freezing processing described in step 2) is -200~-160 DEG C.The drying is freeze-drying, temperature >=-60
℃。
The molal volume ratio of water-soluble iron salts described in step 2) and MXene suspension is (0.0005~0.1) mol:1L,
Preferably (0.001~0.005) mol/L.
The volume ratio of acid described in step 2) and MXene suspension is (0.1~2): 100.
The mass volume ratio of chitosan described in step 2) and MXene suspension is (0.02~2) g:100mL, preferably
0.1~1g:100mL, more preferably 0.5g:100mL.
Composite aerogel described in step 2) is prepared especially by following methods:
A) water-soluble trivalent ferric salt and acid are mixed with MXene suspension, obtains acidity MXene suspension；
B) it dissolves the chitosan in acid MXene suspension, is ultrasonically treated, freezing processing, it is dry, obtain compound airsetting
Glue.
Inert atmosphere described in step 3) refers at least one of nitrogen or argon gas.
When being heat-treated in step 3), the rate of heating is 0.1~50 DEG C/min；More preferably with 3~5 DEG C/min.
Highly sensitive, the wide line sensing scope the compressible compound carbon aerogels, are prepared by the above method.
Application of above-mentioned highly sensitive, the wide line sensing scope the compressible compound carbon aerogels in senser element, especially
It is the application in pressure sensing electronic device.
The principle of the present invention are as follows: (1) presence of chitosan macromolecular avoid MXene nanometer sheet directly again stack, and
Adjacent MXene nanometer sheet is connected by combining or bridging, to form continuous layer structure；(2) protonation chitosan and
Ionic interaction between negatively charged MXene nanometer sheet, and a large amount of hydrogen bond connects so that MXene nanometer sheet is by shell
Glycan is wrapped up and is connected, and the aeroge of three-dimensional structure is welded as in carbonisation；(3) undaform shape layer structure guarantees material tool
There is excellent elastic deformation performance, and stable electricity can be exported from small pressure or strain by contact area between change lamella
Flow response signal.
Preparation method of the invention and the method for preparing elastic carbon material at present have in place of a great difference: giving birth to first is that selecting
Substance chitosan is raw material, avoids the complicated, nano carbon material with high costs using preparation process such as carbon nanotube, graphenes
Material makes material have environmental-friendly renewable, the cheap, advantages such as preparation is simple；Second is that in carbonisation, by with shell
Glycan derived carbon extension welds MXene nanometer sheet to enhance the bond strength between MXene nanometer sheet；Third is that in refrigerating process
The presence of MXene nanometer sheet contributes to form lamellar structure, and the shrinkage phenomenological structure of chitosan is changed into wave in carbonisation
Sheet carbon skeleton.Furthermore MXene also can be used as a nanometer backing material effectively prevent material volume in carbonisation substantially
Shrinkage.The two synergistic effect prevents structure collapses, so that carbon aerogels have good resilience performance.Present invention combination chitosan
With the advantage of MXene two-dimensional nano piece, using MXene to the supporting role of chitosan chain and chitosan derivative carbon to the company of structure
Effect is connect, is prepared for high compression by being oriented to freezing, freeze-drying and carbonization, height is sprung back, recycling performance is excellent, Gao Ling
The carbon aerogels of the characteristics such as quick, wide scope linear sensing.And the architectural characteristic make gained carbon aerogels can realize it is highly sensitive and wide
The linear sensing of range 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 is simple, environmental-friendly；
(2) carbon aerogels prepared have high-compressibility, high resiliency and excellent cyclical stability；
(3) carbon aerogels prepared have stable electric conductivity；
(4) carbon aerogels prepared not only have the sensitivity of superelevation, and induction range is wide, cyclical stability is excellent, can
It is widely used in sensory field.
Detailed description of the invention
Fig. 1 is the stress-that elastic carbon aerogels prepared by embodiment 1 recycle ten circle of compression under different compression strains
Strain curve figure；Photo in figure before the figure compression of top, after 99% compression and rebound；
Fig. 2 is that elastic carbon aerogels prepared by embodiment 1 are pressed when compression strain is 50% by 150 000 circle circulations
The stress-strain diagram (a) and maximum stress and height retention (b) of contracting；The figure of top is the photo of compression front and back in a；
Fig. 3 is (0~70% strain of corresponding material height in 0~5kPa of elastic carbon aerogels prepared by embodiment 1
Amount) sensitivity；
Fig. 4 is elastic carbon aerogels prepared by embodiment 1 to the induction result figure (a) of minimal stress (1Pa) and right
The induction result figure (b) of small strain (being equivalent to the 0.05% of material height)；
Fig. 5 is elastic carbon aerogels prepared by embodiment 1 to curved response results figure；Test at normal temperatures and pressures into
It goes, 30,60,90 equal numerical value indicate the bending angle applied to gained aeroge in figure；The figure in the lower right corner is curved carbon airsetting
The photo of glue；
Fig. 6 is elastic carbon aerogels prepared by embodiment 2 when compression strain is 70% the 1st, 100,300,500 times
Stress-strain curve；The figure in upper right side is the photo of the carbon aerogels of 500 circulation compression front and backs；
Fig. 7 is elastic carbon aerogels prepared by embodiment 3 when compression strain is 70% the 1st, 10,100,300,500
Secondary stress-strain curve；The figure in upper right side is the photo of the carbon aerogels of 500 circulation compression front and backs.
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) it is placed in water carry out ultrasonic disperse, it obtains the MXene that 50ml concentration is 1mg/mL and suspends
Liquid；
(2) by 0.05g FeCl3·6H2O and 500 μ l glacial acetic acid are dissolved in above-mentioned MXene suspension, obtain acid MXene
Suspension；
(3) at high-speed stirred (500r/min), it is slowly added to 0.25g chitosan into suspension, high-speed stirred is to molten
Solution, ultrasonic 20 minutes (300 hertz or more), obtains MXene/ chitosan suspension；
(4) by MXene/ chitosan suspension liquid nitrogen frozen, (- 196 DEG C, processing generally needs until complete freezing is ice
Want 20min or so), (- 58 DEG C, 0.22mbar, until being completely dried) are freeze-dried after having freezed completely to solution,
Composite aerogel is made；
(5) obtained composite aerogel is placed in tube furnace, is warming up in argon atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The compression performance and compression-resistance of gained elasticity carbon aerogels, compression-electric current induction behavior are tried in electronic universal
It tests on machine and carries out, use the sensor of 100N；Resistance when using the record material compression of high-precision multimeter；Using electrochemistry
Curent change when work station record compression.
Fig. 1 is that elastic carbon aerogels prepared by the present embodiment recycle answering for ten circle of compression under different compression strains
Force-strain curve figure.Material can bear 99% decrement and height is kept not change substantially, and it is excellent to show that material has
Elasticity.Fig. 2 is that elastic carbon aerogels prepared by the present embodiment are pressed when compression strain is 50% by 150 000 circle circulations
The stress-strain diagram (a) and maximum stress and height retention (b) of contracting.The height retention of material is in 150 000 circle circulation pressures
It is up to 91.6% after contracting, shows the excellent structural stability of material.Fig. 3 is elastic carbon aerogels prepared by the present embodiment 0
In~5kPa 0~70% dependent variable of material height (corresponding) to the induction result figure of larger pressure (i.e. elastic carbon aerogels 0~
Sensitivity in 5kPa).Material has the linear detection range of 5kPa, and such stress respective material is up to 70% strain
Amount and material can still keep stable linear signal to export in the case where significantly compressing.Fig. 4 is Elastic Carbon prepared by the present embodiment
Aeroge is to the induction result figure (a) of minimal stress (1Pa), and to small strain (being equivalent to the 0.05% of material height)
Incude result figure (b).Gained carbon aerogels can sensitively incude slight pressure and deformation, in conjunction with upper figure, show material
Sensitivity and wide use scope with superelevation.Fig. 5 is that elastic carbon aerogels prepared by the present embodiment tie curved response
Fruit figure；Test carries out at normal temperatures and pressures, and 30,60,90 wait numerical value to indicate the bending angle applied to gained aeroge in figure.Material
Material can export different signal values to differently curved angle, show potential application of the material in bending angle detection.
Embodiment 2
(1) MXene is placed in water carry out ultrasonic disperse, and then obtains the MXene suspension that 50ml concentration is 3mg/mL；
(2) by 0.03g FeCl3·6H2O and 300 μ l glacial acetic acid (anhydrous acetic acid) are dissolved in above-mentioned MXene suspension,
Obtain acid MXene suspension；
(3) under high velocity agitation, 0.15g chitosan is slowly added into above-mentioned gained suspension, high-speed stirred extremely dissolves,
Ultrasound 20 minutes, obtains MXene/ chitosan suspension；
(4) it by above-mentioned MXene/ chitosan suspension liquid nitrogen frozen, is freeze-dried after having been freezed completely to solution
Composite aerogel is made in (- 58 DEG C, 0.22mbar, until being completely dried)；
(5) obtained composite aerogel is placed in tube furnace, is warming up in argon atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The 1st, 100,300, the 500 circle circulation pressure when compression strain is 70% of elastic carbon aerogels prepared by the present embodiment
Stress-strain curve under contracting is as shown in Figure 6.Show that material has excellent compressibility, resilience.
Embodiment 3
(1) MXene is placed in water carry out ultrasonic disperse, obtains the MXene suspension that 50ml concentration is 5mg/mL；
(2) by 0.05g FeCl3·6H2O and 500 μ l glacial acetic acid are dissolved in above-mentioned MXene suspension, obtain acid MXene
Suspension；
(3) under high velocity agitation, 0.25g chitosan is slowly added into above-mentioned gained suspension, high-speed stirred extremely dissolves,
Ultrasound 20 minutes, obtains MXene/ chitosan suspension；
(4) by above-mentioned MXene/ chitosan liquid nitrogen frozen, be freeze-dried after having been freezed completely to solution (- 58 DEG C,
0.22mbar, until being completely dried), composite aerogel is made；
(5) obtained composite aerogel is placed in tube furnace, is warming up in argon atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The 1st, 10,100,300,500 circles when compression strain is 70% of elastic carbon aerogels prepared by the present embodiment follow
Stress-strain curve under ring compression is as shown in Figure 7.Show that material has excellent compressibility, resilience.
Embodiment 4
(1) by MXene (Ti3C2) it is placed in water carry out ultrasonic disperse, it obtains the MXene that 50ml concentration is 1mg/mL and suspends
Liquid；
(2) by 0.05g FeCl3·6H2O and 500 μ l glacial acetic acid are dissolved in above-mentioned MXene suspension, obtain acid MXene
Suspension；
(3) at high-speed stirred (500r/min), 0.25g chitosan is slowly added into above-mentioned gained suspension, high speed
To dissolving, ultrasonic 20 minutes (300 hertz) obtain MXene/ chitosan suspension for stirring；
(4) it by above-mentioned MXene/ chitosan suspension liquid nitrogen frozen, is freeze-dried after having been freezed completely to solution
Composite aerogel is made in (- 58 DEG C, 0.22mbar, until being completely dried)；
(5) obtained composite aerogel is placed in tube furnace, is warming up in argon atmosphere with the rate of 3 DEG C/min
700 DEG C and 4h is kept the temperature, obtains elastic carbon aerogels.
Elastic carbon aerogels prepared by the present embodiment can bear 80% decrement and height is kept not become substantially
Change, does not change substantially when compression strain is 50% by 1000 circle circulation compression heights.It is excellent to show that material has
Compressibility, resilience.
Embodiment 5
(1) MXene is placed in water carry out ultrasonic disperse, obtains the MXene suspension that 50ml concentration is 5mg/mL；
(2) by 0.05g FeCl3·6H2O and 500 μ l glacial acetic acid are dissolved in above-mentioned MXene suspension, obtain acid MXene
Suspension；
(3) 0.25g chitosan is slowly added into above-mentioned gained suspension under high velocity agitation, high-speed stirred extremely dissolves,
Ultrasound 20 minutes, obtains MXene/ chitosan suspension；
(4) by above-mentioned MXene/ chitosan liquid nitrogen frozen, be freeze-dried after having been freezed completely to solution (- 58 DEG C,
0.22mbar, until being completely dried), composite aerogel is made；
(5) obtained composite aerogel is placed in tube furnace, is warming up in argon atmosphere with the rate of 5 DEG C/min
900 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
Elastic carbon aerogels prepared by the present embodiment can bear 90% decrement and height is kept not become substantially
Change, does not change substantially when compression strain is 50% by 5000 circle circulation compression heights.It is excellent to show that material has
Compressibility, resilience.
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 (10)
1. a kind of preparation method of highly sensitive, the wide line sensing scope compressible compound carbon aerogels, it is characterised in that: including
Following steps:
1) MXene nanometer sheet is dispersed in water, obtains MXene suspension；
2) water-soluble trivalent ferric salt, acid, MXene suspension are uniformly mixed with chitosan, freezing processing, it is dry, it obtains compound
Aeroge；
3) composite aerogel is heat-treated in an inert atmosphere, obtains compound carbon aerogels；The heat treatment refers to heating
To 500~1200 DEG C and keep the temperature 0~12h.
2. the preparation method of highly sensitive according to claim 1, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: the temperature of heat treatment described in step 3) is 600~900 DEG C；
The concentration of MXene suspension described in step 1) is 0.5~10mg/mL；
The molal volume ratio of water-soluble trivalent ferric salt described in step 2) and MXene suspension is (0.0005~0.1) mol:1L；
The mass volume ratio of chitosan described in step 2) and MXene suspension is (0.02~2) g:100mL.
3. the preparation method of highly sensitive according to claim 2, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: the concentration of the MXene suspension is 1~5mg/mL；The temperature of heat treatment described in step 3) is 700~900
℃。
4. the preparation method of highly sensitive according to claim 1, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: the volume ratio of acid described in step 2) and MXene suspension is (0.1~2): 100；
The time being heat-treated in step 3) is 1~3h.
5. the preparation method of highly sensitive according to claim 1, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: MXene nanometer sheet described in step 1) is Ti3C2；
Water-soluble trivalent ferric salt described in step 2) is ferric trichloride, ferric nitrate, the ferric sulfate containing the crystallization water or without the crystallization water
In more than one；
Acid described in step 2) is glacial acetic acid, dilute hydrochloric acid, dilute sulfuric acid.
6. the preparation method of highly sensitive according to claim 5, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: it is rapid 2) described in water-soluble trivalent ferric salt be containing the crystallization water or without the ferric trichloride of the crystallization water；
Acid described in step 2) is glacial acetic acid.
7. the preparation method of highly sensitive according to claim 1, the wide line sensing scope compressible compound carbon aerogels,
Be characterized in that: the temperature of freezing processing described in step 2) is -200~-160 DEG C；
It is dry for freeze-drying, temperature >=-60 DEG C described in step 2)；
Inert atmosphere described in step 3) refers at least one of nitrogen or argon gas；
When being heat-treated in step 3), the rate of heating is 0.1~50 DEG C/min.
8. it is a kind of obtained by any one of claim 1~7 preparation method it is highly sensitive, the wide line sensing scope compressible
Compound carbon aerogels.
9. highly sensitive according to claim 8, the wide line sensing scope compressible compound carbon aerogels are in senser element
Application.
10. application according to claim 9, it is characterised in that: the senser element is pressure sensing electronic device.
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| 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 |
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