CN110128695A - A kind of conduction composite sponge and conductive composite sponge sensor and its application - Google Patents
A kind of conduction composite sponge and conductive composite sponge sensor and its application Download PDFInfo
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- 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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Abstract
The invention discloses a kind of conductive composite sponge and conductive composite sponge sensor and its applications.The material is first using hydroxyethyl cellulose, soybean protein as primary raw material, it is crosslinked and is freeze-dried through epoxychloropropane and form hydroxyethyl cellulose/soybean protein sponge, hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge is obtained using the mode of in-situ polymerization aniline, is finally assembled into conductive composite sponge sensor.Animal pattern rat nerve injury repairing effect is assessed using the application sensor, anesthesia or surgical injury can not be carried out to animal, and directly dynamic monitoring rat nerve repairs degree, its evaluation effect is suitable with conventional electro physiology evaluation effect, but avoids anesthesia to animal, operation equivalent damage.This method not only obtains a kind of sensor of compression resistance formula, also provides a kind of new evaluating apparatus and evaluation method to evaluate the reparation of peripheral nerve injury.
Description
Technical field
The invention belongs to biomedical materials fields, also belong to polymeric material field.It is compound more particularly to a kind of conduction
Sponge, using the conduction composite sponge as sensor made of material and its in the application of evaluation model animal Peripheral nerve repair.
Background technique
Flexible, sensitive pressure sensor human motion monitoring, man-machine interface, speech recognition, personalized health monitoring,
Robot artificial limb, electronic skin, portable health patient monitor, even rehabilitation real-time measurement have be widely applied.In recent years, people
Explore many for high-compressibility, the new materials of highly sensitive pressure sensor, they are used as monitoring human health and work
Dynamic pressure sensor causes people and greatly pays close attention to.The transformation mechanism of various pressure sensors can be divided into compression resistance formula,
Condenser type, piezoelectric type and friction electric-type.Wherein, ambient pressure is converted to resistance signal by compression resistance formula sensor, has system
Make the advantages that simple, at low cost, signal acquisition facilitates.In this sensor, electrically conductive elastic composite material or sponge are being pressed
More conductive paths are formed under the effect of contracting power, sensor resistance is caused to reduce, this transmission mechanism is referred to as negativity pressure drag effect
It answers.Good mechanical elasticity, high-compressibility and good electric conductivity are the basic demands of piezoresistance sensor material.In recent years, perhaps
More flexible, spongy and conductive materials be used to prepare the three-dimensional conductive sponge of pressure sensor.Three-dimensional conductive sponge is according to it
Structure and composition can be divided into four seed types: (1) simple conductive sponge；(2) composite material conductive sponge；(3) infused elastomer
Conductive sponge；(4) conductive sponge of conductive material is coated.The characteristics of every kind of conductive sponge material has oneself and disadvantage: single
Pure conductive sponge refers to the three-dimensional porous sponge structure only assembled by conductive material.Carbon material (carbon nanotube, graphite
Alkene, graphene oxide) it is the most common material for constructing high conductivity, extremely-low density three-dimensional conductive sponge.Although this
Conductive sponge has extremely-low density, high conductivity, good thermal stability and chemical stability, but just due to its intrinsic machinery
Property and brittleness, these materials may have limited sensibility and compression strain range.Composite conducting sponge is in conductive material
Polymeric binder is added in assembling process, or conductive material is mixed with polymers compositions, then passes through the methods of foaming, freeze-drying
It is prepared, the uneven dispersion of conductive material and polymer is one of composite conducting sponge material intractable during the preparation process
Problem.Elastomer dipping conductive sponge refer to regular conductive sponge is impregnated/coat elastomeric polymer, to enhance the steady of sponge
Qualitative and compressibility.The shortcomings that polymer impregnated conductive sponge is that conductivity is substantially reduced, and density increases.Conductive material coating sea
Silk floss refer to the methods of sputtering, dip-coating, in-situ polymerization by conductive material be coated in non-conductive polymer sponge on made of lead
Electric sponge.Non-conductive polymer sponge in the solution or can also be dispersed in carbon and metal by direct impregnation and be converted into conduction
Material, and it is used as carbon nanotube, graphene, silver of conductive coating etc. expensive the shortcomings that such conductive sponge, and prepare
Complex process.
In above-mentioned four kinds of conductive sponge materials, conductive material, which coats sponge, has preferable practicability and stability.And
In the research of early period, we be prepared for it is a kind of have shape memory function i.e. elasticity and the good hydroxyethyl cellulose of recovery/
Soybean protein sponge (patent No.: 201710370099.8, a kind of hydroxyethyl cellulose of water sensitive shape memory function/big
Legumin matter composite sponge and preparation method thereof), find it with good biocompatibility, degradability and regeneration function
Energy.Can by the sponge be applied to conductive material coat sponge, prepare it is cheap, environmentally protective, led with favorable elasticity
Electric sponge material needs further to study.
In neural tissue engineering basic research, often using animals such as rat, rabbit or dogs as model, week is caused by operation
Neurologic defect is enclosed, then is bridged with various nerve tracheas, neurologic defect is repaired, and it is evaluated by serial of methods
Repairing effect.Currently, carrying out surgical exposure nerve usually after certain repair time, under narcosis carries out electro physiology detection mind
Repaired situation.Or after animal is put to death, further commented with the methods of HE slice, immunofluorescence slice and transmission electron microscope slice
Valence repairing effect and research repair mechanisms.If there is the pressure sensor of real-time tracking is connected with the position or acra being repaired
It connects, perhaps it can directly evaluate repairing effect without anesthesia, operation and put to death animal, can at least reduce the wound to animal
Evil realizes dynamic observation, provides a more effective way to evaluate neural restoration.
Summary of the invention
In order to solve defect and deficiency of the existing technology, the object of the present invention is to provide a kind of conductive composite sponge,
The shape memory function that has of the preparation of the technical solution disclosed in ZL 201710370099.8 is elasticity and the good hydroxyl of recovery
On the basis of ethyl cellulose/soybean protein sponge, hydroxyethyl cellulose/big can get using the mode of in-situ polymerization aniline
Legumin matter/polyaniline composite conducting sponge material.And the sponge not only has original hydroxyethyl cellulose/soybean protein sea
Continuous elasticity and recoverability, while electric conductivity is also imparted, and its resistance is related with the pressure of application, it is a kind of good
Pressure-sensitive conductive material.
The second object of the present invention is to provide a kind of conductive composite sponge sensor, is compound in conduction provided by the invention
Sponge opposite side even spread conductive silver oil simultaneously connects copper wire, compound at new type of compression resistance-type conduction with digital sourcemeter assembled end
Sponge sensor device.Sensitivity, response time and the stability of the sensor reach higher level, to evaluate nerve fiber work
The reparation of the peripheral nerve injury of animal model in journey basic research provides a kind of new evaluating apparatus and evaluation method.
Third object of the present invention is to provide conductive composite sponge sensors on preparation evaluation neural tissue engineering basis
Application in the device of the reparation of the peripheral nerve injury of animal model in research, conductive compound sensor and rat ischium mind
The connection of underwent operative limb is applied to the degree of evaluation rat sciatic nerve reparation, and whole process avoids the operations damage such as anaesthetizing and perform the operation
Animal, evaluation effect are suitable with electro physiology evaluation effect.
To achieve the goals above, the invention adopts the following technical scheme:
In a first aspect, a kind of hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge is provided, by following step
Suddenly it prepares:
(1) hydroxyethyl cellulose/soybean protein sponge preparation: hydroxyethyl cellulose and soybean protein are first distinguished
It is dissolved in deionized water and 4~5wt% sodium hydrate aqueous solution, is then blended in proportion, hydroxyethyl cellulose and soybean egg
The mass ratio of white matter is 90:10~30:70, stirs to get uniform blended liquid, and it is fine that ethoxy is added in Xiang Shangshu blend solution
The epoxychloropropane or ethylene glycol diglycidylether of dimension element and the 10-50% of soybean protein gross mass stir and evenly mix at room temperature
Cross-linking reaction is carried out, is placed at -20 DEG C through centrifugation degassing and places 12h, then be transferred at -80 DEG C and place for 24 hours afterwards through being freeze-dried,
Then being neutralized to pH with spirit of vinegar is 7, and clear water rinses up to composite sponge；
(2) hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge preparation: aniline monomer is dissolved in
In 0.5~2M hydrochloric acid solution, final concentration of 0.1~1M of aniline is quickly mixed, and the hydroxyethyl cellulose that step (1) is obtained/
Soybean protein sponge, which is put into solution, to stir, and 1 gram of hydroxyethyl cellulose/soybean protein is added in every 1L hydrochloric acid/aniline solution
0.1~1M the ammonium persulfate solution isometric with hydrochloric acid/aniline solution is slowly dropped into aniline/hydrochloric acid solution by sponge, is induced
Aniline polymerization reaction, flowing water rinses after the completion of polymerization, is freeze-dried to get hydroxyethyl cellulose/soybean protein/polyaniline is arrived
Conductive composite sponge.
The application hydroxyethyl cellulose/soybean protein sponge preparation method refer to " patent No.:
201710370099.8 hydroxyethyl cellulose/the soy protein composite sponge and its system of a kind of water sensitive shape memory function
Technical solution disclosed in Preparation Method ".
Second aspect provides a kind of conductive composite sponge sensor, is prepared by the following steps acquisition: will be made from the application
Hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge opposite side even spread conductive silver oil simultaneously connects copper wire, with number
Word source table assembled end obtains conductive composite sponge sensor at sensor device.
The third aspect provides above-mentioned conductive composite sponge sensor in preparation evaluation neural tissue engineering basic research
Application in the device of the reparation of the peripheral nerve injury of animal model, this application be specially by conductive composite sponge sensor with
The sole of the operation limb of the injury of sciatic nerve of animal pattern rat is wanted to contact, and during rat acts on one's own, completes to collect
Signal from sensor, for evaluating its restoration effect.
Compared with prior art, of the invention to have the prominent advantages that:
(1) make full use of abundance, cheap, environmentally protective and hydroxyethyl cellulose with degradation property and
Soybean protein raw material, and compound sponges material includes polyaniline, has biocompatibility.
(2) using hydroxyethyl cellulose/soybean protein sponge as sponge elastomer, polyaniline is led as conductive sponge
Electric material, prepared compound sponges material had both remained hydroxyethyl cellulose/soybean protein biomaterial favorable elasticity,
Pressure current waveform is consistent, and the time needed for electric current becomes initial value from maximum value is 0.14s, card in conventional pressing for conductive sponge
Bright this sponge sensor can be used for general motor function detection.Polyaniline biomaterial elasticity is compensated for simultaneously not
Foot.
(3) hydroxyethyl cellulose/soybean protein/polyaniline sponge sensor is carrying out pressing 100 of 10% deformation
After circulation, there is no substantially changeing for current waveform, it was demonstrated that such sponge has good repeatability and stability.
It (4) is control, hydroxyethyl cellulose/soybean protein/polyaniline sponge prepared by the present invention with electro physiology experiment
Sensor is used to evaluate the method and electro physiology Comparison between detecting methods of neural restoration, has without anaesthetizing and putting to death animal, nothing
The significant advantages such as damage and dynamic monitoring, and its evaluation effect is suitable with electro physiology evaluation effect.To the base of neural tissue engineering
Plinth research is of great significance.
Detailed description of the invention
Fig. 1 is hydroxyethyl cellulose/soybean protein sponge (left side) for obtaining and hydroxyethyl cellulose in embodiment 1/greatly
Legumin matter/polyaniline sponge (right side) light microscopic figure.
The hydroxyethyl cellulose obtained in Fig. 2 embodiment 1/soybean protein sponge (upper left, lower-left) and hydroxy ethyl fiber
Element/soybean protein/polyaniline sponge (upper right, bottom right) SEM electron microscope.
Hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive sponge resistance-strain the system obtained in Fig. 3 embodiment 1
Number.
Hydroxyethyl cellulose/the soybean protein obtained in Fig. 4 embodiment 1/layer/polyaniline conductive sponge reaction time.
Hydroxyethyl cellulose/the soybean protein obtained in Fig. 5 embodiment 1/layer/polyaniline conductive sponge recycles compression performance.
Hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive the sponge obtained in Fig. 6 embodiment 1 and example 2 is detected
The schematic diagram of situation detection is repaired after sciatic nerve autotransplantation operation.
Hydroxyethyl cellulose/the soybean protein obtained in Fig. 7 embodiment 5/polyaniline composite conducting sponge is detected
The postoperative testing result of sciatic nerve autotransplantation (right side) and electro physiology testing result (left side) compare.
Specific embodiment
By following detailed description combination attached drawing it will be further appreciated that the features and advantages of the invention.Provided implementation
Example is only the explanation to the method for the present invention, remaining content without limiting the invention in any way announcement.
[embodiment 1]
2g hydroxyethyl cellulose is dissolved in 98g deionized water obtained 2% hydroxyethyl cellulose solution, 1g soybean protein
It is dissolved in 5% sodium hydroxide solution of 6g deionized water and 3g and 10% soy bean proteinous soln is made, with the dry ratio of 3:7 by hydroxyl
Ethyl cellulose and soy bean proteinous soln are mixed, and are added with 20% hydroxyethyl cellulose and soybean protein dry ratio
Epichlorohydrin crosslinker carries out cross-linking reaction 40 minutes, and 2000rpm is centrifuged bubble in 15 minutes removing composite solutions, will be compound
Solution pours into 10 × 10cm2In mold and it is put into -20 degree freezing 12 hours, vacuum freeze drying 48 hours fine up to ethoxy
Tie up element/soy protein composite sponge.Aniline monomer is dissolved in 1M hydrochloric acid solution, the final concentration of 0.2M of aniline, aniline with
The molar concentration rate of hydrochloric acid is 1:5, is mixed using magnetic stirring apparatus, hydroxyethyl cellulose/soybean protein sponge is put
Entering and continues stirring 30 minutes in solution, 1 gram of hydroxyethyl cellulose/soybean protein sponge is added in every 1L hydrochloric acid/aniline solution, with
Hydrochloric acid/aniline solution same volume ammonium persulfate solution (0.2M) is slowly dropped into aniline/hydrochloric acid solution, and induction aniline polymerization is anti-
It answers.Flowing water rinses 24 hours after polymerization 2 hours, is freeze-dried to get novel hydroxyethyl cellulose/soybean protein/polyphenyl is arrived
Amine composite conducting sponge.
Fig. 1 and Fig. 2 is hydroxyethyl cellulose/soybean protein/polyaniline composite conducting sponge obtained in embodiment 1
Light microscopic figure and scanning electron microscope (SEM) photograph.As shown in Figure 1, hydroxyethyl cellulose/soybean protein is white, polymerization aniline 2 hours it
After become black.As shown in Fig. 2, hydroxyethyl cellulose/soybean protein sponge and hydroxyethyl cellulose/soybean protein/poly-
Aniline sponge all has porous structure, but hydroxyethyl cellulose/soybean protein/polyaniline composite sponge and pure hydroxy ethyl fiber
Element/soybean protein sponge is compared, and surface increases polyaniline particles and distribution is more uniform.
[embodiment 2]
By hydroxyethyl cellulose/soybean protein/polyaniline sponge two sides even spread conductive silver oil and copper wire is connected, is made
It is made sponge sensor.After being connect with digital sourcemeter, causes sponge that different degrees of deformation occurs by applying pressure, detect
The resistance of sponge corresponding deformation obtains responsive parameter-resistor-strain coefficient of sponge.Resistor-strain coefficient (GF)=((R-
R0)/R0)/strain,R0It is the initial resistance of sponge, R is the resistance that corresponding deformation occurs for sponge, and strain is the shape of sponge
Become.
Fig. 3 is the coefficient of strain of composite sponge obtained in embodiment 1 and embodiment 2.As shown, hydroxy ethyl fiber
Element/soybean protein/polyaniline sponge passes through different deformation, collects its resistance data in digital sourcemeter and makees Fig. 3, resistance is answered
Variable coefficient (GF)=- 0.29.
[embodiment 3]
Hydroxyethyl cellulose/the soybean protein of [embodiment 2]/polyaniline sponge sensor is subjected to normal press, with
After digital sourcemeter connection, the electric current of sponge corresponding deformation is detected, another important parameter --- the reaction time of sponge is obtained.Its
Middle I0It is the initial current under 3V voltage of sponge, I is the electric current that corresponding deformation occurs under 3V voltage for sponge.
Fig. 4 is current curve figure obtained in embodiment 1 and embodiment 3.As shown, conductive sponge is in routine
By pressure current waveform it is consistent, in enlarged drawing wherein it can be seen that electric current initial value is become from maximum value needed for the time
For 0.14s, prove that this sponge sensor can be used for general motor function detection.
[embodiment 4]
[embodiment 2] hydroxyethyl cellulose/soybean protein/polyaniline sponge sensor is subjected to pressing for 10% deformation
Pressure after connecting with digital sourcemeter, detects the curent change of sponge corresponding deformation, detects the stability of sponge.
Fig. 5 is current curve figure obtained obtained in embodiment 1 and embodiment 4.As shown, ethoxy is fine
Element/soybean protein/polyaniline sponge sensor is tieed up after carrying out pressing 100 circulations of 10% deformation, current waveform does not have
It substantially change, it was demonstrated that such sponge has good repeatability and stability.
[embodiment 5]
By hydroxyethyl cellulose/soybean protein obtained/polyaniline composite conducting sponge opposite side even spread conductive silver
Oil simultaneously connects copper wire, with digital sourcemeter assembled end at sensor device, by conductive sponge sensor and rat sciatic nerve into
It is (as shown in Figure 6) for evaluating rat nerve repairing effect degree after the postoperative operation limb connection of row nerve autograft.
Fig. 7 (a)-(f) is by electro physiology method and sensor side in the case of the acquisition different time points neural restoration of embodiment 5
Method result compares.As seen from the figure, electro physiology result is after carrying out nerve autograft operation, with the increase of repair time, electricity
Physiological compound muscle action potential (CMAPs) peak value increases, but still has compared with normal neuronal after repairing 12 weeks certain
Gap.As repair time increases, the current signal being collected by sensor, method is in change intensity and signal frequency
On have certain increase, it is same repair 12 weeks after also certain difference compared with the current signal caused by the normal side hind leg
It is different.The compound muscle action potential of electro physiology and sensor, which detect resulting current signal, has similar enhancing trend, and two kinds
The neural restoration evaluation effect of method is suitable, but electro physiology needs to anaesthetize animal and performed the operation, need profession anesthesia and
Surgical skills could be completed, and deal with easy anesthesia improperly and excessively even result in animal dead.And we are carried out using this sensor
Detection is not needed to be anaesthetized and be performed the operation, and not damaging can survey at any time, continuous dynamic observation can be also carried out, especially to same
Animal can be observed for a long time, and repairing effect is compared in front and back.The Normal representative of Fig. 7 g, h are normal rats, that is, are not had
The electro physiology experimental result of mouse by surgical procedure and sensor detection as a result, the not no difference at time point, only complete
Result caused by full normal rat.The device is expected to lack as a kind of new evaluation method for animal pattern peripheral nerve
The repairing effect of damage is evaluated.
Claims (3)
1. a kind of hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge, which is characterized in that by following steps system
It is standby to obtain:
(1) hydroxyethyl cellulose/soybean protein sponge preparation: hydroxyethyl cellulose and soybean protein are first dissolved respectively
It in deionized water and 4 ~ 5wt% sodium hydrate aqueous solution, is then blended in proportion, hydroxyethyl cellulose and soy proteinaceous
Mass ratio is 90:10~30:70, stirs to get uniform blended liquid, be added in Xiang Shangshu blend solution hydroxyethyl cellulose and
The epoxychloropropane or ethylene glycol diglycidylether of the 10-50 % of soybean protein gross mass stirs and evenly mixs handed at room temperature
Connection reaction is placed at -20 DEG C through centrifugation degassing and places 12 h, then be transferred at -80 DEG C place 24 h after through being freeze-dried, then
Being neutralized to pH with spirit of vinegar is 7, and clear water rinses up to composite sponge；
(2) aniline monomer hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge preparation: is dissolved in 0.5 ~ 2
In M hydrochloric acid solution, the final concentration of 0.1 ~ 1M of aniline is quickly mixed, hydroxyethyl cellulose/soybean protein that step (1) is obtained
Matter sponge, which is put into solution, to stir, and 1 gram of hydroxyethyl cellulose/soybean protein sponge is added in every 1L hydrochloric acid/aniline solution, will be with
0.1 ~ 1 isometric M ammonium persulfate solution of hydrochloric acid/aniline is slowly dropped into aniline/hydrochloric acid solution, induction aniline polymerization reaction,
Flowing water rinses after the completion of polymerization, is freeze-dried to get hydroxyethyl cellulose/soybean protein/layer/polyaniline conductive composite sponge is arrived.
2. a kind of conduction composite sponge sensor, which is characterized in that be prepared by the following steps acquisition: by the ethoxy of claim
Cellulose/soybean protein/layer/polyaniline conductive composite sponge opposite side even spread conductive silver oil simultaneously connects copper wire, with digital sourcemeter
Assembled end obtains conductive composite sponge sensor at sensor device.
3. animal of the conduction composite sponge sensor as claimed in claim 2 in preparation evaluation neural tissue engineering basic research
Application in the device of the reparation of the peripheral nerve injury of model, which is characterized in that the application is specially by conductive composite sponge
Sensor is wanted to contact with the sole of the operation limb of the injury of sciatic nerve of animal pattern rat, during rat acts on one's own,
It completes to collect the signal from sensor, for evaluating its restoration effect.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114221573A (en) * | 2022-01-11 | 2022-03-22 | 四川大学 | Cellulose-based nano friction generator with high output performance and preparation method thereof |
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| CN101251506A (en) * | 2008-03-15 | 2008-08-27 | 西北师范大学 | Method for manufacturing conductive polyaniline/cellulose composite biosensor |
| CN102212210A (en) * | 2011-04-29 | 2011-10-12 | 南京理工大学 | Method for preparing polyaniline-coated bacteria cellulose nano conductive composite by in-situ polymerization |
| CN108665686A (en) * | 2018-05-15 | 2018-10-16 | 武汉大学 | Intelligent urine wetting monitoring device based on soybean protein isolate/hydroxyethyl cellulose/polypyrrole composite sponge |
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| CN114221573A (en) * | 2022-01-11 | 2022-03-22 | 四川大学 | Cellulose-based nano friction generator with high output performance and preparation method thereof |
| CN114221573B (en) * | 2022-01-11 | 2024-01-30 | 四川大学 | Cellulose-based nano friction generator with high output performance and preparation method thereof |
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