CN110057887A - The preparation method and applications of conductive polymer-intercalated metal oxide mixed gel - Google Patents
The preparation method and applications of conductive polymer-intercalated metal oxide mixed gel Download PDFInfo
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- CN110057887A CN110057887A CN201910394591.8A CN201910394591A CN110057887A CN 110057887 A CN110057887 A CN 110057887A CN 201910394591 A CN201910394591 A CN 201910394591A CN 110057887 A CN110057887 A CN 110057887A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
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Abstract
The invention discloses a kind of preparation methods of conductive polymer-intercalated metal oxide mixed gel, comprising the following steps: S1, is dispersed in water two-dimensional layer metal oxide powder, under stirring conditions, with H2O2Solution reaction；S2, the reaction solution for obtaining step S1 carry out hydro-thermal reaction, obtain metal oxide gel；S3, it disperses the obtained metal oxide gel of step S2 in solvent, EDOT is added, intercalation occurs for oscillation mixing to get the metal oxide/PEDOT mixed gel is arrived.The present invention also provides the conductive polymer-intercalated metal oxide mixed gels prepared by the method, and the flexible biosensor being prepared by it.Mixed gel prepared by the present invention has printing and electric conductivity, can direct printed electrode on a flexible substrate, and it is to H2O2Detection have good selectivity.
Description
Technical field
The present invention relates to gel rubber material technical fields, and in particular to a kind of conductive polymer-intercalated metal oxide mixing
The preparation method of gel and its application in flexible biosensor.
Background technique
With the development of the applications such as medical diagnosis on disease and individual health care, flexible biosensor part has been widely used in detecting
Different types of biological indicator such as cell, biomolecule, pH value.Compared to traditional biosensor, it can monitor and measure
It is emerging that the flexible biosensor for the electronically or chemically signal that change is generated by specific microenvironment has attracted scientific research personnel greatly to study
Interest.Flexible wearable biosensor be by be connected to tissue surface realize it is continuous it is close to physiology biomarker and
The biochemical signals etc. of human body are monitored, and have light weight, portable, conformability, Noninvasive and implantable etc. main excellent
Point presents huge application potential in personal medical treatment and medical diagnosis on disease.
In recent years, the fast development of electrically conductive ink and printing technology has expedited the emergence of flexible, compressible and stretchable electronics device
Part.However for these flexible electronic devices, how by ultra-thin patterned print electrode or active material and flexible base board phase
In conjunction with, promote device with the complex-curved holding of human body or tissue is good contacts, and guarantee device in compression or tensional state
Under stability, be the technical difficult points that flexible wearable biosensing device is faced at present.Therefore, it is necessary to design one kind
Novel method is used to develop the detection device of original position, flexible wearable formula, for realize the clinical diagnosis of disease early stage, treatment and
Health monitoring provides new development opportunity.
The development of nano material technology facilitates the solution of above-mentioned difficult point, with structure controllability nano material by
Exploitation flexible biosensor is widely used in the past ten years, although the design of advanced nano material, device and nanometer add
Work technology accelerates the development of flexible biosensor part, but by nano material and flexible substrates carry out effective integration to
Building flexible biosensor part still has many challenges.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of conductive polymer-intercalated metal oxide mixed gels
Preparation method has printing and electric conductivity by the mixed gel of this method preparation, can directly print electricity on a flexible substrate
Pole, and it is to H2O2Detection have good selectivity.
In order to solve the above-mentioned technical problems, the present invention provides a kind of conductive polymer-intercalated metal oxide mixing is solidifying
The preparation method of glue, comprising the following steps:
S1, two-dimensional layer metal oxide powder is dispersed in water, under stirring conditions, with H2O2Solution reaction；
S2, the reaction solution for obtaining step S1 carry out hydro-thermal reaction, obtain metal oxide gel；
S3, it disperses the obtained metal oxide gel of step S2 in solvent, 3,4-rthylene dioxythiophene is added
(EDOT), intercalation occurs for oscillation mixing to get the metal oxide/PEDOT mixed gel is arrived.
Further, in step S1, the metal oxide is V2O5Or MnO2。
Further, in step S1, metal oxide powder is dispersed in water, being made into concentration is 10~15mg/mL's
Aqueous solution.
Further, in step S1, the metal oxide and H2O2The mass volume ratio of solution is 50~80:1 (mg/
mL)。
Further, in step S2, the temperature of hydro-thermal reaction is 150~200 DEG C, and the reaction time is 12~18h.
Further, in step S3, the metal oxide gel further includes being centrifuged to it before being scattered in solvent
The step of processing removal supernatant.
Further, in step S3, the solvent is acetonitrile, n,N-Dimethylformamide, alcohols or dimethyl sulfoxide.
Further, in step S3, the volume ratio of metal oxide gel and solvent is 1:0.5~1.5.
Further, in step S3, the volume ratio of metal oxide gel dispersion liquid and EDOT are 15~30:1.
Another aspect of the present invention additionally provides the conductive polymer-intercalated metal oxide being prepared by the method
Mixed gel.
It the present invention also provides a kind of flexible biosensor, is prepared by the mixed gel, the flexibility
Biosensor can be used for clinical diagnosis, treatment and health monitoring of disease early stage etc..
Further, the flexible biosensor can be prepared by following methods:
1. electrode shape needed for designing senser element, sealed membrane is attached on flexible mylar (PET) and is passed through
Cutting machine obtains patterned electrode on sealed membrane；
2. taking a certain amount of mixed gel, it is added dropwise on patterned sealed membrane and carries out electrode print, room temperature is dried；
3. removing sealed membrane template after it is dried and obtaining the PET film for being printed on mixed gel electrode, further on its surface
Attaching one layer, there are the films of well, and flexible biosensor part is made.
Beneficial effects of the present invention:
The present invention is based on metal oxide powders, make its elder generation and H with solution agitating2O2It reacts, then passes through water
Metal oxide hydrogel is made in thermal response；Intercalation further is carried out to metal oxide hydrogel by conducting polymer PEDOT
The conductive polymer-intercalated metal oxide mixed gel of two dimension is made in reaction.The mixed gel has printing and electric conductivity can
With directly on a flexible substrate printed electrode and its to H2O2Detection have good selectivity, the furthermore cost of the mixed gel
Low, preparation is simply；In addition, this prints electrode, the printing process compared with traditional print electrode is more directly simple and stability
It is good；These advantages make it with huge industrialization prospect.
Detailed description of the invention
Fig. 1 is V2O5The transmission electron microscope picture of/PEDOT；
Fig. 2 is by V2O5The different pattern of/PEDOT mixed gel printing；
Fig. 3 is V2O5The electric conductivity test result of/PEDOT mixed gel；
Fig. 4 is by V2O5The flexible sensing device of/PEDOT mixed gel preparation is to H2O2The anti-interference detection figure of detection.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
1. conductive polymer-intercalated vanadic anhydride mixed gel the preparation method is as follows:
By 0.36g vanadic anhydride (V2O5) powder ultrasonic dispersing and dissolving is in the deionized water of 30mL, then in stirring bar
By hydrogenperoxide steam generator (30%, the H of 5mL under part2O2) it is slowly added into V2O5In aqueous solution and continue to stir a few hours.When mixed
It closes object and becomes to put it into hydrothermal reaction kettle hydro-thermal reaction 15 hours at 190 DEG C when rufous clear solution, obtain V2O5Water
Gel.Then, by V2O5Hydrogel carries out centrifugal treating and removes supernatant.Finally, by V2O5Hydrogel is dispersed in acetonitrile (body
Product is than being 1:1), (volume ratio 20:1) is then mixed by oscillation with a certain amount of 3,4-rthylene dioxythiophene (EDOT), is sent out
Raw intercalation, obtains V2O5/ PEDOT mixed gel.
2. the preparation of flexible biosensor part
(1) electrode shape needed for designing senser element, sealed membrane is attached on flexible mylar (PET) and is passed through
Cutting machine obtains patterned electrode on sealed membrane.
(2) a certain amount of V is taken2O5The progress electrode print on patterned sealed membrane is added dropwise in/PEDOT mixed gel
Brush, room temperature are dried.
(3) after it is dried, remove sealed membrane template, obtain being printed on V2O5The PET film of/PEDOT electrode, further at it
Surface attaches one layer, and there are the films of well, obtain flexible biosensor part.
3.V2O5The test of/PEDOT mixed gel physicochemical property
Fig. 1 is V2O5The morphology characterization of/PEDOT mixed gel, from figure 1 it appears that the mixed gel is tied in the form of sheets
Structure.
Fig. 2 is by V2O5Different pattern made of the printing of/PEDOT mixed gel, it is fine to show that the mixed gel has
Printing.
Fig. 3 is V2O5The conducting performance test result figure of/PEDOT mixed gel, as shown in figure 3, the U-shaped figure printed by it
Case can successfully be used as conducting wire lightening LED lamp, illustrate that the electric conductivity of the mixed gel is very good.
4. the Electrochemical Properties of flexible biosensor part
Using chronoamperometry (i-t) to by V2O5The electrode of/PEDOT mixed gel printing is to H2O2That detects is anti-interference
Ability is tested, the chaff interferent of selection be in actual sample often and H2O2The some substances coexisted, such as: ascorbic acid
(AA), dopamine (DA), uric acid (UA) glucose (Glucose), K+、Na+Deng.Can significantly it see from Fig. 4, when respectively
Sequentially add the H of same concentrations2O2After other interfering substances, the sensor is to H2O2Show apparent current-responsive, and it is right
Other interfering substances are almost without response.This shows the sensor to H2O2There is good selectivity, its anti-interference ability is very
By force.
In conclusion V2O5/ PEDOT mixed gel can be obtained by above-mentioned preparation method, which has fine
Two-dimensional structure and its with good impressionability and electric conductivity；Furthermore by V2O5/ PEDOT mixed gel is in flexible PET base
The electrode of upper printing is to H2O2There are good catalytic effect and strong antijamming capability, the flexible sensing device of mixed gel preparation
It is simpler, economical, portable, stability is good, the holding time is long compared with traditional sensor, it is examined in the clinic of disease early stage
There is better industrialization prospect in terms of disconnected, treatment and health monitoring.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of preparation method of conductive polymer-intercalated metal oxide mixed gel, which is characterized in that including following step
It is rapid:
S1, two-dimensional layer metal oxide powder is dispersed in water, under stirring conditions, with H2O2Solution reaction；
S2, the reaction solution for obtaining step S1 carry out hydro-thermal reaction, obtain metal oxide gel；
S3, it disperses the obtained metal oxide gel of step S2 in solvent, EDOT is added, it is anti-that intercalation occurs for oscillation mixing
Should to get arrive the metal oxide/PEDOT mixed gel.
2. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S1, the metal oxide is V2O5Or MnO2。
3. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In, in step S1, the metal oxide and H2O2The mass volume ratio of solution is 50~80:1 (mg/mL).
4. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S2, the temperature of hydro-thermal reaction is 150~200 DEG C, and the reaction time is 12~18h.
5. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S3, the metal oxide gel further includes carrying out centrifugal treating removal supernatant to it before being scattered in solvent
The step of.
6. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S3, the solvent is acetonitrile, n,N-Dimethylformamide, alcohols or dimethyl sulfoxide.
7. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S3, the volume ratio of metal oxide gel and solvent is 1:0.5~1.5.
8. the preparation method of conductive polymer-intercalated metal oxide mixed gel as described in claim 1, feature exist
In in step S3, the volume ratio of metal oxide gel dispersion liquid and EDOT are 15~30:1.
9. the conductive polymer-intercalated metal oxide mixing that method according to claim 1-8 is prepared
Gel.
10. a kind of flexible biosensor, which is characterized in that be prepared by mixed gel as claimed in claim 9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112993217A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of organic-inorganic hybrid material based on vanadium pentoxide and application of organic-inorganic hybrid material in zinc ion battery |
| CN115266870A (en) * | 2021-04-30 | 2022-11-01 | 苏州科技大学 | Preparation method of wearable micro-fluidic quasi-solid biochip based on gel, product and application thereof |
| CN115403744A (en) * | 2022-08-18 | 2022-11-29 | 苏州科技大学 | Two-dimensional ultrathin porous PEDOT, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112993217A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Preparation method of organic-inorganic hybrid material based on vanadium pentoxide and application of organic-inorganic hybrid material in zinc ion battery |
| CN115266870A (en) * | 2021-04-30 | 2022-11-01 | 苏州科技大学 | Preparation method of wearable micro-fluidic quasi-solid biochip based on gel, product and application thereof |
| CN115403744A (en) * | 2022-08-18 | 2022-11-29 | 苏州科技大学 | Two-dimensional ultrathin porous PEDOT, and preparation method and application thereof |
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