CN109179365A - Highly sensitive chitosan-based sensing material of one kind and its preparation method and application - Google Patents
Highly sensitive chitosan-based sensing material of one kind and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to the technical fields of sensing material, disclose highly sensitive chitosan-based sensing material of one kind and its preparation method and application.Method: iron chloride or ferric chloride hexahydrate are dissolved in cellulose nano microcrystalline suspension, and chitosan dissolution is then added, obtains FeCl3/ Chitosan/Cellulose nano microcrystalline suspension；Liquid nitrogen frozen, and then be freeze-dried, gained aeroge is carbonized obtains sensing material in an inert atmosphere.The advantage of present invention combination chitosan and cellulose nano microcrystalline, support and carbon connection function using cellulose nano microcrystalline are prepared for high compression, high rebound, the sensing material that the characteristics such as excellent, highly sensitive, the wide sensing detection range of performance are recycled by freezing, freeze-drying and carbonization.The sensing material can be realized the sensitive detection to slight pressure and strain, can be applied to various pressure sensing electronic devices.
Description
Technical field
The invention belongs to the technical fields of sensing material, and in particular to a kind of with highly sensitive, wide sensing detection range
Chitosan-based sensing material and its preparation method and application.
Background technique
Sensing material can be elastic carbon material.Elastic carbon material is pressed in the important function of wearable sensors part depending on it
Contracting performance, sensitivity and fatigue resistance.The compressible carbon material of tradition graphene and its spreads out mostly by nano-carbon material such as carbon nanotube
The building such as biology and nano carbon composite material.
Carbon nanotube is to construct elastic airsetting due to its high aspect ratio, flexibility, mechanical robustness and satisfactory electrical conductivity
The good raw material of glue, main preparation methods are chemical vapour deposition techniques.As Han Wang et al. (Wang H, Lu W, Di J,
et al.Ultra‐Lightweight and Highly Adaptive All‐Carbon Elastic Conductors
with Stable Electrical Resistance[J].Advanced Functional Materials,2017,27
(13): 1606220.) having manufactured ultralight compressible carbon nanotube foam using CVD method.Graphene and its derivative conduct
The representative materials of two-dimensional nano-carbon material, have high conductivity and certain flexibility, and planar structure makes it in ultrathin electrodes, soft
Property material and lightweight basis material design there is unique advantage, be equally concerned in terms of preparing elastic carbon material.Mesh
Before, it can be divided mainly into vapour deposition process, solvent-thermal method and freezing in the method for the standby elastic carbon material such as graphene, graphene oxide
Casting.Such as Hui Bi et al. (Bi H, Chen I, Lin T, et al.A New Tubular Graphene Form of a
Tetrahedrally Connected Cellular Structure[J].Advanced Materials,2015,27(39):
The three-dimensional tubulose graphene gas of superelevation porosity 5943-5949.) is prepared for using aerosil as template using CVD method
Gel.Yingpeng Wu et al. (Wu Y, Yi N, Huang L, et al.Three-dimensionally bonded
spongy graphene material with super compressive elasticity and near-zero
Poisson ' s ratio [J] .Nature Communications, 2015,6:6141.) graphene sheet passed through into solvent heat
With the graphene-based elastic sponge of carbonisation self assembly.H Sun et al. (Sun H, Xu Z, Gao
C.Multifunctional,ultra-flyweight,synergistically assembled carbon aerogels.
[J] .Advanced Materials, 2013,25 (18): 2554-2560.) pass through freezing casting carbon nanotube and graphite oxide
Alkene (GGO) aqueous solution is prepared for high resiliency aeroge, can be used as hydrophobic thin oil material.But these nano-carbon material multi-sources in
The problems such as non-renewable fossil resources, face environmental pollution, unsustainable, and preparation method is complicated, it is with high costs.These bullets
Property carbon material is still to be improved when as sensing material.
Biomass is to prepare low cost, sustainable carbon material as rich reserves in nature, the carbon source of cheap reproducible
Desirable feedstock.But the biomass resource currently used for manufacturing compressible carbon material is very limited, predominantly bacteria cellulose and
Cellulose nano microcrystalline.Such as X Yang et al. (Yang X, Shi K, Zhit omirsky I, et al.Cellulose
Nanocrystal Aerogels as Universal 3D Lightweight Substrates for
Supercapacitor Materials. [J] .Advanced Materials, 2015,27 (40): 6104-6109.) by cold
The cellulose nano microcrystalline suspension for freezing casting and rear carbonization aldehyde and hydrazides modification, constructs the elastic carbon aerogels of hydrazone crosslinking.
Due to the difficulty that structure is designed and controlled, the mechanical performance of this kind of material is poor, it is difficult to industrial application.Therefore, building has
The biomass-based compressible carbon aerogels of super-elasticity, excellent fatigue resistance are still very challenging.Elasticity current simultaneously
Carbon material is not possible to realize the highly sensitive linear sensitivity with wide scope.
Therefore, preparation has high resiliency, excellent fatigue resistance, high sensitivity, wide sensing detection range linear sensitivity
Biomass-based sensing material is of great significance in terms of wearable sensors part.
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 the chitosan-based sensing material of highly sensitive, wide sensing detection range.
There is the inspection of highly sensitive, wide sensing by what the above method was prepared another object of the present invention is to provide a kind of
Survey the chitosan-based sensing material of range.
A further object of the present invention is to provide above-mentioned chitosan-based sensing material answering in pressure sensing electronic device
With.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of highly sensitive chitosan-based sensing material, includes the following steps:
(1) cellulose nano microcrystalline is dispersed in water, obtains cellulose nano microcrystalline suspension；
(2) by FeCl3·6H2O or FeCl3It is dissolved in cellulose nano microcrystalline suspension, obtains FeCl3/ cellulose is received
Rice microcrystalline suspension；
(3) FeCl is dissolved the chitosan in3In/cellulose nano microcrystalline suspension, FeCl is obtained3/ Chitosan/Cellulose
Nano microcrystalline suspension；
(4) by FeCl obtained by step (3)3/ Chitosan/Cellulose nano microcrystalline suspension carries out liquid nitrogen frozen and then freezes
It is dry, obtain FeCl3/ Chitosan/Cellulose nano microcrystalline composite aerogel；
(5) by the composite aerogel that step (4) obtains be warming up in an inert atmosphere 500~1200 DEG C and keep the temperature 0~
12h obtains elastic carbon aerogels i.e. sensing material.
Preferably, cellulose nano microcrystalline described in step (1) is to pass through sour water solution or oxidation by raw material of cellulose
Degradation obtains；It is highly preferred that the cellulose nano microcrystalline is obtained by 65% sulphuric acid hydrolysis cellulose.
Preferably, the additional amount of cellulose nano microcrystalline described in step (1) is 0.001%~5%；It is highly preferred that fine
The additional amount for tieing up plain nano microcrystalline is 0.5%.
Preferably, FeCl described in step (2)3The FeCl of/cellulose nano microcrystalline suspension3Concentration be 0.0005~
0.1mol/L；Preferred FeCl3Solution concentration is 0.004mol/L.
Preferably, FeCl is dissolved the chitosan in described in step (3)3Concentration in/cellulose nano microcrystalline suspension
It is 0.02%~2%；The concentration more preferably dissolved the chitosan in suspension is 0.5%.
Preferably, inert atmosphere described in step (4) refers at least one of nitrogen or argon gas.
The rate of heating described in step (4) is 0.1~50 DEG C/min, preferably 3~5 DEG C/min；More preferably with 3~5
DEG C/rate of min is warming up to 800 DEG C and keeps the temperature 2h.
A kind of sensing material with highly sensitive wide scope linear sensing, is prepared by the above method.
Application of the sensing material in senser element.
The principle of the present invention are as follows: by FeCl3Chitosan is dissolved in solution and obtains chitosan solution, and fine by being added
It ties up plain nano microcrystalline and forms support force, promote the mechanical property of materials.Cellulose nano microcrystalline is provided from reproducible cellulose
Source, with high-specific surface area, lightweight, surface group abundant, excellent mechanical strength, low cost, renewable, environment is friendly
Well, the advantages that dispersion performance and suspendability are excellent in water.This preparation method and the method for preparing elastic carbon material at present have
It is very different place: first is that selecting biomass chitosan is raw material, avoiding using preparation process such as carbon nanotube, graphenes
Nano-carbon material complicated, with high costs makes material have environmental-friendly renewable, the cheap, advantages such as preparation is simple；Two
It is that cellulose nano microcrystalline has excellent suspension, dispersion performance in water, and not will increase the viscosity of solution, is being freeze-dried
When play backing material structure function, prevent material volume substantially shrinkage；Third is that chitosan is changed into carbonisation
Wave sheet carbon skeleton, cellulose nano microcrystalline is transformed into the connection of nano-sized carbon reinforcing sheet interlayer, and then prevents structure collapses, makes
Obtaining carbon aerogels has good resilience performance.The advantage of present invention combination chitosan and cellulose nano microcrystalline, utilizes fiber
Support and carbon connection function of the plain nano microcrystalline to chitosan chain are prepared for high pressure by guiding freezing, freeze-drying and carbonization
Contracting, high rebound, the carbon aerogels that the characteristics such as excellent, highly sensitive, the wide scope linear sensing of performance are recycled.And the architectural characteristic
Make gained carbon aerogels that can realize highly sensitive and wide scope linear sensing, can be applied to various pressure sensing electronic devices.
Preparation method and gained sensing material of the invention have the following advantages that and the utility model has the advantages that
(1) preparation process is simple, at low cost；
(2) sensing material (carbon aerogels) prepared has high-compressibility, high resiliency and cyclical stability；
(3) sensing material (carbon aerogels) prepared has stable electric conductivity；
(4) sensing material (carbon aerogels) prepared is not only with the sensitivity of superelevation, and induction range is wide, stable circulation
Property is excellent, can be widely applied to sensory field.
Detailed description of the invention
Sensing material prepared by Fig. 1 embodiment 1 (carbon aerogels) recycles ten circle of compression under different compression strains
Height-change chart；
Sensing material prepared by Fig. 2 embodiment 1 (carbon aerogels) is when compression strain is 50% by 50000 circle circulations
The stress-strain diagram of compression；
Sensing material prepared by Fig. 3 embodiment 1 (carbon aerogels) the 1st, 100,300 circles when compression strain is 70%
The stress-strain diagram (right side) of 10 circles before when stress-strain diagram (left side) and compression strain are 90%；
Fig. 4 is sensing material (carbon aerogels) prepared by embodiment 1 in the 1st, 10,10000,30000 second compression
Current stability (right side) figure of normalized resistance (left side) and 1-1000 second compression under 50% strain；
Fig. 5 is sensing material (carbon aerogels) (0-18kPa) under wide detection range prepared by embodiment 1, is shown
High sensitivity (27.2kPa-1)；
Fig. 6 is induction result figure (left side) of the sensing material (carbon aerogels) prepared by embodiment 1 to minimal stress (1Pa)
With the induction result figure (right side) to small strain (being equivalent to the 0.05% of material height)；
Fig. 7 is sensing material prepared by embodiment 2 (carbon aerogels) when compression strain is 60% the 1st, 10,100,
300 stress-strain curves.
Fig. 8 is sensing material prepared by embodiment 3 (carbon aerogels) when compression strain is 60% the 1st, 10,100,
300 stress-strain curves.
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) cellulose nano microcrystalline is added to the water, mechanical stirring obtains the cellulose nanometer that dispersion concentration is 0.5%
Microcrystalline suspension；
(2) by FeCl3·6H2O is dissolved in above-mentioned cellulose nano microcrystalline suspension, and concentration 0.004mol/L is obtained
FeCl3/ cellulose nano microcrystalline suspension；
(3) at high-speed stirred (revolving speed 800rpm), to above-mentioned gained FeCl3In/cellulose nano microcrystalline suspension
It is slowly added to the chitosan that gross mass is 0.5%, high-speed stirred obtains FeCl to dissolving3/ Chitosan/Cellulose nano microcrystalline
Suspension；
(4) by above-mentioned FeCl3/ Chitosan/Cellulose nano microcrystalline suspension is placed in plastic casing, and box is lain in metal
Box outer wall pours into liquid nitrogen in metal box and is freezed (freezing freezes), freezed after having freezed completely to solution
Dry (- 58 DEG C, vacuum degree 0.22mbar, the time is 16 hours), are made FeCl3/ Chitosan/Cellulose nano microcrystalline suspension
Composite aerogel；
(5) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels i.e. sensing material.
The compression performance and compression-resistance of gained elasticity carbon aerogels (sensing material), compression-electric current induction behavior exist
It is carried out on electronic universal tester, uses the sensor of 100N；Resistance when using the record material compression of high-precision multimeter；
Curent change when compressing is noted down using electrochemical workstation.
Fig. 1 is that sensing material (elastic carbon aerogels) prepared by the present embodiment recycles compression under different compression strains
The height-change chart of ten circles.When compression strain is less than 70%, material height in ten circle circulation compressions does not change substantially,
Show that material has excellent elasticity and structural stability.Fig. 2 is sensing material (Elastic Carbon airsetting prepared by the present embodiment
Glue) stress-strain diagram for recycling compression is enclosed by 50000 when compression strain is 50%, the stress reservation of material reaches 70%.
Fig. 3 is sensing material prepared by the present embodiment (elastic carbon aerogels) 300 circle of process when compression strain is 70%, and pressure
Cyclic compressive stress-strain figures of 10 circle of process when shrinkage strain is 90%.Answered under strain big in this way Retention still compared with
Height shows that material has the compressibility of height.Fig. 4 is sensing material (elastic carbon aerogels) prepared by the present embodiment the
1, the current stability on normalized resistance (left side) and 1-1000 second compression under differently strained when 10,10000,30000 second compression
(right side) figure, normalized resistance are almost unchanged in 1,10,10000,30000 second compression；And stablize by 1000 second compression electric currents
Property it is excellent, show material have good structural stability and conductive stability.Fig. 5 is sensing material prepared by the present embodiment
(elastic carbon aerogels) under wide detection range (0-18kPa), the high sensitivity (27.2kPa shown-1).Fig. 6 is this implementation
The sensing material (elastic carbon aerogels) of example preparation to 1Pa minimal stress carry out sensitive induction result figure (left side) with to being equivalent to
0.05% small strain of material height incudes result figure (right side).The carbon material tested in micro-stress test device is clipped in
Between two panels nickel is thin, by obtaining corresponding electric signal to upper surface drop of dripping, calculating is often dripped corresponding pressure (stress), in turn
Sensitivity data is calculated.Gained carbon aerogels can sensitively incude slight pressure and deformation, show that material has
The sensitivity of superelevation.
Fig. 1-3 is the height or stress variation under material circulation compression, illustrates that material can bear big strain, and 50,000
After secondary circulation compression, preferable height and stress are still kept, illustrates the excellent fatigue resistance of material.Material is following in Fig. 4
The stability of electrochemical data under ring compression illustrates material circulation excellent in stability.Fig. 5 illustrates that the induction range of material is wide,
The pressure range of detectable 0-18kPa.It is detected in conjunction with the small pressure of Fig. 6, small strain, can illustrate the high sensitivity and wide sense of material
Answer range.
Embodiment 2
(1) cellulose nano microcrystalline is added in ultrapure water, mechanical stirring obtains the cellulose that dispersion concentration is 0.5%
Nano microcrystalline suspension；
(2) by FeCl3·6H2O is dissolved in above-mentioned cellulose nano microcrystalline suspension, and concentration 0.008mol/L is obtained
FeCl3/ cellulose nano microcrystalline suspension；
(3) to above-mentioned gained FeCl at high-speed stirred (revolving speed 800rpm)3Delay in/cellulose nano microcrystalline suspension
The slow chitosan that gross mass is added and is 0.5%, high-speed stirred obtain FeCl to dissolving3/ Chitosan/Cellulose nano microcrystalline is outstanding
Supernatant liquid；
(4) by above-mentioned FeCl3/ Chitosan/Cellulose nano microcrystalline suspension is placed in plastic casing, and box is lain in metal
Box outer wall pours into liquid nitrogen in metal box and is freezed (freezing freezes), freezed after having freezed completely to solution
Dry (- 58 DEG C, vacuum degree 0.22mbar, the time is 16 hours), are made FeCl3/ Chitosan/Cellulose nano microcrystalline suspension
Composite aerogel；
(5) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The the 1st, 10,100,300 stress-when compression strain is 60% of elastic carbon aerogels prepared by the present embodiment
Strain curve figure is as shown in Figure 7.Show that material has excellent compressibility, resilience.
Embodiment 3
(1) cellulose nano microcrystalline is added in ultrapure water, mechanical stirring obtains the cellulose that dispersion concentration is 0.4%
Nano microcrystalline suspension；
(2) by FeCl3·6H2O is dissolved in above-mentioned cellulose nano microcrystalline suspension, and concentration 0.004mol/L is obtained
FeCl3/ cellulose nano microcrystalline suspension；
(3) to above-mentioned gained FeCl at high-speed stirred (revolving speed 800rpm)3Delay in/cellulose nano microcrystalline suspension
The slow chitosan that gross mass is added and is 0.6%, high-speed stirred obtain FeCl to dissolving3/ Chitosan/Cellulose nano microcrystalline is outstanding
It is floating；
(4) by above-mentioned FeCl3/ Chitosan/Cellulose nano microcrystalline suspension is placed in plastic casing, and box is lain in metal
Box outer wall pours into liquid nitrogen in metal box and is freezed (freezing freezes), freezed after having freezed completely to solution
Dry (- 58 DEG C, vacuum degree 0.22mbar, the time is 16 hours), are made FeCl3/ Chitosan/Cellulose nano microcrystalline suspension
Composite aerogel；
(5) obtained composite aerogel is placed in tube furnace, is warming up in nitrogen atmosphere with the rate of 3 DEG C/min
800 DEG C and 2h is kept the temperature, obtains elastic carbon aerogels.
The the 1st, 10,100,300 stress-when compression strain is 60% of elastic carbon aerogels prepared by the present embodiment
Strain curve figure is as shown in Figure 8.Show that material has excellent 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 (9)
1. a kind of preparation method of highly sensitive chitosan-based sensing material, characterized by the following steps:
(1) cellulose nano microcrystalline is dispersed in water, obtains cellulose nano microcrystalline suspension；
(2) by FeCl3·6H2O or FeCl3It is dissolved in cellulose nano microcrystalline suspension, obtains FeCl3/ cellulose nanometer is micro-
Crystalline suspension liquid；
(3) FeCl is dissolved the chitosan in3In/cellulose nano microcrystalline suspension, FeCl is obtained3/ Chitosan/Cellulose nanometer
Microcrystalline suspension；
(4) by FeCl obtained by step (3)3/ Chitosan/Cellulose nano microcrystalline suspension carries out liquid nitrogen frozen and is then freeze-dried,
Obtain FeCl3/ Chitosan/Cellulose nano microcrystalline composite aerogel；
(5) composite aerogel that step (4) obtains is warming up to 500~1200 DEG C in an inert atmosphere and keeps the temperature 0~12h, is obtained
To sensing material.
2. the preparation method of highly sensitive chitosan-based sensing material according to claim 1, it is characterised in that: in step (2)
The FeCl3The FeCl of/cellulose nano microcrystalline suspension3Concentration is 0.0005~0.1mol/L；
Step dissolves the chitosan in FeCl described in (3)3Concentration in/cellulose nano microcrystalline suspension is 0.02%~
2%.
3. the preparation method of highly sensitive chitosan-based sensing material according to claim 1, it is characterised in that: in step (1)
The additional amount of the cellulose nano microcrystalline is 0.001%~5%.
4. the preparation method of highly sensitive chitosan-based sensing material according to claim 1, it is characterised in that:
Cellulose nano microcrystalline described in step (1) is to be obtained using cellulose as raw material by sour water solution or oxidative degradation.
5. the preparation method of highly sensitive chitosan-based sensing material according to claim 1, it is characterised in that: in step (4)
The inert atmosphere refers at least one of nitrogen or argon gas.
6. the preparation method of highly sensitive chitosan-based sensing material according to claim 1, it is characterised in that: in step (4)
The rate of the heating is 0.1~50 DEG C/min.
7. the preparation method of highly sensitive chitosan-based sensing material according to claim 6, it is characterised in that: the heating
Rate is 3~5 DEG C/min.
8. a kind of highly sensitive chitosan-based sensing material obtained by any one of claim 1~7 preparation method.
9. application of the highly sensitive chitosan-based sensing material in senser element according to claim 1.
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Cited By (2)
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| CN109851313A (en) * | 2019-01-22 | 2019-06-07 | 华南理工大学 | A kind of highly sensitive, the wide line sensing scope compressible compound carbon aerogels and its preparation and application |
| CN114180556A (en) * | 2021-12-30 | 2022-03-15 | 重庆大学 | Three-dimensional porous modified carbon nanotube and preparation method and application thereof |
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| CN108212185A (en) * | 2017-12-29 | 2018-06-29 | 中国林业科学研究院木材工业研究所 | A kind of electrocatalysis material in relation to compound carbon aerogels and preparation method thereof |
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| CN104743541A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of carbon aerogel |
| CN107134373A (en) * | 2017-04-25 | 2017-09-05 | 武汉大学 | A kind of carbon aerogels/metal oxide composite and preparation method and application |
| CN108212185A (en) * | 2017-12-29 | 2018-06-29 | 中国林业科学研究院木材工业研究所 | A kind of electrocatalysis material in relation to compound carbon aerogels and preparation method thereof |
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| CN114180556A (en) * | 2021-12-30 | 2022-03-15 | 重庆大学 | Three-dimensional porous modified carbon nanotube and preparation method and application thereof |
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