CN105353015B - A kind of preparation method and application of poly- dioxyethylene thiophene composite membrane - Google Patents
A kind of preparation method and application of poly- dioxyethylene thiophene composite membrane Download PDFInfo
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Abstract
A kind of preparation method and application of poly- dioxyethylene thiophene composite membrane, is related to electrochemical sensor.The preparation method of poly- dioxyethylene thiophene composite membrane: (1) dioxyethylene thiophene EDOT solution and BSA solution are respectively prepared；(2) the dioxyethylene thiophene EDOT solution that step (1) is prepared is mixed with the BSA solution that step (1) is prepared, obtains mixed liquor；(3) using Pt electrode as working electrode and to electrode, Ag/AgCl is auxiliary electrode, and using CHI621B electrochemical workstation, Electrochemical Scanning is carried out in the mixed liquor of step (2), obtain poly- dioxyethylene thiophene composite membrane, i.e. PEDOT (BSA) composite membrane.Prepared poly- dioxyethylene thiophene composite membrane, that is, PEDOT (BSA) composite membrane can be applied in preparing electrode material, and the electrode material includes but is not limited to platinum electrode, carbon paper electrode, Au electrode etc..
Description
Technical field
The present invention relates to electrochemical sensors, enhance poly- dioxyethylene thiophene more particularly, to bovine serum albumin (BSA)
(PEDOT) preparation method and application of a kind of poly- dioxyethylene thiophene composite membrane of membrane stability.
Background technique
PEDOT molecular structure is simple, energy gap is small, conductivity is high, is suitable as the polymeric membrane modification of electrochemical sensor
On electrode substrate (such as Pt, Au).Since Pt is hydrophily, and PEDOT is hydrophobicity, so that being aggregated in the surface Pt
PEDOT film compatibility is not good enough, and in use process, PEDOT film is easy to even fall off from Pt sur-face peeling, influences working electrode
Stability is unfavorable for the progress of experiment, it is therefore necessary to a kind of method for finding simplicity, for enhancing the stability of PEDOT film,
The good electric conductivity of PEDOT film is maintained simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of cheap dopant BSA and for improving PEDOT membrane stability, improve
PEDOT (BSA) composite membrane afterwards can be used tens of times, can be used for a kind of poly- bis oxyethylene thiophene that target product detects in system
The preparation method and application of pheno composite membrane.
A kind of preparation method of the poly- dioxyethylene thiophene composite membrane, comprising the following steps:
(1) dioxyethylene thiophene (EDOT) solution and BSA solution are prepared respectively；
(2) dioxyethylene thiophene (EDOT) solution that step (1) is prepared is mixed with the BSA solution that step (1) is prepared, is obtained
Mixed liquor；
(3) using Pt electrode as working electrode and to electrode, Ag/AgCl is auxiliary electrode, uses CHI621B electrochemical operation
It stands, carries out Electrochemical Scanning in the mixed liquor that step (2) obtains, obtain poly- dioxyethylene thiophene composite membrane, i.e. PEDOT
(BSA) composite membrane, obtained electrode designations are PEDOT (BSA)/Pt.
In step (1), described dioxyethylene thiophene (EDOT) solution of preparing can prepare the dioxy that molar concentration is 0.01M
Vinylthiophene (EDOT) solution, the lithium perchlorate for being 0.1M containing molar concentration in dioxyethylene thiophene (EDOT) solution
(LiClO4)；Dioxyethylene thiophene (EDOT) the solution room temperature is kept in dark place, lasting to stir；The preparation BSA solution can match
Mass ratio processed is the BSA solution of 7.0mg/ml, and 4 DEG C of refrigerators save.
In step (2), the volume ratio of dioxyethylene thiophene (EDOT) solution and BSA solution can be 6: 1, described mixed
The mass concentration for closing the final BSA of liquid can be 1.0mg/ml.
In step (3), the specification of the Pt electrode can be φ 0.6mm × 15mm, and Ag/ can be used in the auxiliary electrode
AgCl (3M NaCl) is auxiliary electrode；The scanning current potential of the Electrochemical Scanning can be 0~1V, and sweep speed can be 0.01V/
S, scanning circle number can be 5 circles, and operation temperature can be 25 DEG C, and it can be 1cm that length is polymerize on working electrode.
Prepared poly- dioxyethylene thiophene composite membrane, that is, PEDOT (BSA) composite membrane can be applied in preparing electrode material,
The electrode material includes but is not limited to platinum electrode, carbon paper electrode, Au electrode etc..
During being tested using PEDOT/Pt electrode, it is found that the PEDOT film for being aggregated in the surface Pt often has chap
The phenomenon that splitting or even falling off, this may be because adhesion condition of the PEDOT film on Pt is bad, cause PEDOT with the time and
Scan action slowly falls off from Pt.
In standard biologic mensuration program, BSA is usually utilized to pass through non-specific binding ability as a kind of retarding agent
To occupy the gap of fixation surface.In order to enhance stability of the PEDOT film on Pt electrode, the present invention polymerize with electrochemical process
When PEDOT film, the bovine serum albumin (BSA) of 1.0mg/ml is added into EDOT monomer solution, observation BSA stablizes PEDOT film
The influence of property.
Detailed description of the invention
Fig. 1 be PEDOT/Pt with PEDOT (BSA)/Pt electrode in potassium ferricyanide solution compared with electrical conductivity.In Fig. 1,
Curve (a) is PEDOT/Pt, and curve (b) is PEDOT (BSA)/Pt.
PEDOT film is compared with PEDOT (BSA) membrane stability on Fig. 2 platinum electrode.In Fig. 2, (a) is PEDOT film, (b) is
PEDOT (BSA) film.
The infrared spectrogram of Fig. 3 BSA powder and platinum sheet surface PEDOT, PEDOT (BSA) film.In Fig. 3, curve (a)
For BSA, curve (b) is PEDOT, and curve (c) is PEDOT (BSA).
PEDOT film is compared with PEDOT (BSA) membrane stability on Fig. 4 carbon paper.In Fig. 4, (a) is PEDOT film, (b) is
PEDOT (BSA) film.
Specific embodiment
In order to illustrate more clearly of the present invention, following embodiment will be described in detail the present invention in conjunction with attached drawing.
Embodiment 1
1) it by the Pt piece of 0.5cm × 1.0cm, is immersed in BSA solution and is taken out after 5min.
2) in Y type cell, the 0.1M PB (pH6.2) and 200 μ l Bio-Rad Protein of 800 μ l is added
Assay covers colorimetric notch using sealed membrane and mixes.
3) the Pt piece of taking-up is immersed in prepared Bio-Rad Protein Assay solution, is stood at 25 DEG C
5min, and be compared with blank sample.
The result shows that solution colour obviously becomes blue, illustrate that BSA has good compatibility in Pt electrode surface, it can be with
As improve PEDOT Pt surface affinity additive.
Embodiment 2
1) the EDOT solution 6ml for taking 0.01M, is sufficiently mixed with the BSA solution of the 7mg/ml of 1ml, so that final BSA's is dense
Degree is 1.0mg/ml, and mixed liquor is labeled as A；
2) the EDOT solution 6ml for taking 0.01M, is sufficiently mixed with the deionized water of 1ml so that in mixed liquor EDOT concentration with
Identical in step 1), mixed liquor is labeled as B；
3) respectively using PEDOT/Pt and PEDOT (BSA)/Pt as working electrode, Pt is to electrode, Ag/AgCl (3M
It NaCl is) auxiliary electrode, with the K of 0.01M3[Fe(CN)6] solution detects the response current size of Different electrodes, and makes comparisons.
The electrical conductivity of PEDOT film affects the size of electrochemical sensor response current, it is therefore necessary to probe into adding for BSA
Add the influence to PEDOT film electrical conductivity.From figure 1 it appears that after bovine serum albumin addition, with leading for PEDOT/Pt electrode
Electric degree is compared, and PEDOT (BSA)/Pt electrode electrical conductivity slightly reduces, but still very high.
Embodiment 3
1) step and method acquisition PEDOT/Pt and PEDOT (BSA)/electrode of Pt two in embodiment 1 are utilized；
2) using PEDOT/Pt as working electrode, Pt is to electrode, and Ag/AgCl (3M NaCl) is auxiliary electrode, to 1.0mM
Hydrogenperoxide steam generator be scanned, scanning circle number 10 enclose, scanning voltage -0.2~0.8V, scanning speed 50mV；It is repeatedly scanned with 5
It is secondary；
3) again using PEDOT (BSA)/Pt as working electrode, Pt is to electrode, and Ag/AgCl (3M NaCl) is auxiliary electrode,
The hydrogenperoxide steam generator of 1.0mM is scanned, scanning circle number 10 encloses, scanning voltage -0.2~0.8V, scanning speed 50mV；Instead
Multiple scanning 20 times；
4) by step 2) with 3) in used electrode sufficiently rinsed with deionized water, be subsequently placed in deoxygenation in drying box and protect
It deposits, keeps it sufficiently dry；
5) two electrodes in step 4) are observed under the amplification factor of X100 with SEM, obtains electrode surface form.
It is as shown in Figure 2 to obtain result.
Since Pt electrode surface is than more hydrophilic, and the oligomer of EDOT and PEDOT be then in aqueous solution it is fairly hydrophobic, this
So that PEDOT film can not be stably adhered to Pt electrode surface.Therefore it is desirable that the addition of BSA can change the surface Pt
Hydrophilic and hydrophobic, thus enable PEDOT it is more compact be attached to the surface Pt.
PEDOT/Pt electrode and PEDOT (BSA)/Pt electrode can be respectively seen after using certain number by Fig. 2
SEM image (amplification factor X100), in which: figure (a) is image of the PEDOT/Pt electrode after using for several times, and film surface is bright
The many crackles of explict occurrence；And scheming (b) is that PEDOT (BSA)/Pt electrode uses the image after 20 times or more, it can be seen that PEDOT
(BSA) film surface is still flat and smooth, shows good stability.
Embodiment 4
In order to understand influence of the addition of BSA to PEDOT membrane structure, to BSA powder and PEDOT/Pt, PEDOT
(BSA)/Pt electrode carries out FTIR analysis.
Preparation of samples process:
(1) substrate of the Pt plate of 0.5cm × 1.0cm as polymeric membrane is selected, surface area is increased.
(2) by three-electrode system, using Pt plate as working electrode, Pt is, to electrode, Ag/AgCl (3M NaCl) are ginseng
Than electrode, it polymerize PEDOT and PEDOT (BSA) with the method for CV scanning.Scanning current potential is 0.0~1.0V, and sweep speed is
0.01V/s, scanning circle number are 40 circles, and temperature is 25 DEG C, and polymerized area is 0.5cm × 0.5cm.PEDOT film one is made respectively,
PEDOT (BSA) film one.
(3) sample test is carried out with reflective FTIR.
During the test, each sample need to be 4 times in different location repeated measurement, to ensure data accuracy.
The characteristic peak positions of PEDOT film are compared it can be found that PEDOT (BSA) composite membrane not only has the feature of PEDOT film
Wave crest, while there is the feature wave crest of BSA；And the addition of BSA increases all PEDOT characteristic peak positions all, to doing
Offset；In view of the electrochemistry formated mode of the electrode, it can learn that the addition of BSA becomes the overall structure of PEDOT
Change, that is to say, that have between chemical bond between BSA and PEDOT and interacts, not just simple contact.
The infrared spectrogram of BSA powder and platinum sheet surface PEDOT, PEDOT (BSA) film is referring to Fig. 3.
Embodiment 5
1) the EDOT solution 6ml for taking 0.01M, is sufficiently mixed with the BSA solution of the 7mg/ml of 1ml, so that final BSA's is dense
Degree is 1.0mg/ml, and mixed liquor is labeled as A；
2) the EDOT solution 6ml for taking 0.01M, is sufficiently mixed with the deionized water of 1ml so that in mixed liquor EDOT concentration with
Identical in step 1), mixed liquor is labeled as B；
3) with carbon paper (CP, specification are) for working electrode, Pt is to electrode (specification is φ 0.6mm × 15mm), Ag/AgCl
(3M NaCl) carries out Electrochemical Scanning using CHI621B electrochemical workstation for auxiliary electrode in solution A.Scan current potential
For 0.0~1.0V, sweep speed 0.01V/s, scanning circle number 5 is enclosed, and operation temperature is 25 DEG C, and length is polymerize on working electrode and is
1cm.Then, electrochemical polymerization is carried out in solution B with same method.Working electrode after two polymerizations is respectively labeled as
PEDOT/CP and PEDOT (BSA)/CP.
4) using PEDOT/CP as working electrode, Pt is to electrode, and Ag/AgCl (3M NaCl) is auxiliary electrode, to 1.0mM
Hydrogenperoxide steam generator be scanned, scanning circle number 10 enclose, scanning voltage -0.2~0.8V, scanning speed 50mV；It is repeatedly scanned with 5
It is secondary；
5) again using PEDOT (BSA)/CP as working electrode, Pt is to electrode, and Ag/AgCl (3M NaCl) is auxiliary electrode,
The hydrogenperoxide steam generator of 1.0mM is scanned, scanning circle number 10 encloses, scanning voltage -0.2~0.8V, scanning speed 50mV；Instead
Multiple scanning 20 times；
6) by step 4) with 5) in used electrode sufficiently rinsed with deionized water, be subsequently placed in deoxygenation in drying box and protect
It deposits, keeps it sufficiently dry；
7) two electrodes in step 6) are observed under the amplification factor of X100 with SEM, obtains electrode surface form.
Result is obtained as shown in figure 4, (a) is image of the PEDOT/CP electrode after using for several times, film in Fig. 4
Obviously there are many crackles in surface；It and is (b) that PEDOT (BSA)/CP electrode uses the image after 20 times or more, it can be seen that
PEDOT (BSA) film surface is still flat and smooth, shows good stability.
This carbon paper Jing Guo PEDOT (BSA) film modified mistake can be used as the electricity of the work in microbiological fuel cell (MFC)
Pole, test are adsorbed on the electricity production situation of electrode surface bacterium.
Claims (5)
1. a kind of preparation method of poly- dioxyethylene thiophene composite membrane, it is characterised in that the following steps are included:
(1) dioxyethylene thiophene solution and BSA solution are prepared respectively；The preparation dioxyethylene thiophene solution is to prepare 0.01M
Dioxyethylene thiophene solution, the lithium perchlorate for being 0.1M containing molar concentration in the dioxyethylene thiophene solution；It is described to match
BSA solution processed is to prepare the BSA solution that mass ratio is 7.0mg/mL；
(2) the dioxyethylene thiophene solution that step (1) is prepared is mixed with the BSA solution that step (1) is prepared, obtains mixed liquor；Institute
The volume ratio for stating dioxyethylene thiophene solution and BSA solution is 6: 1, and the mass concentration of the final BSA of the mixed liquor is
1.0mg/mL；
(3) using Pt electrode as working electrode and to electrode, Ag/AgCl is auxiliary electrode, using CHI621B electrochemical workstation,
Electrochemical Scanning is carried out in the mixed liquor of step (2), obtains poly- dioxyethylene thiophene composite membrane, i.e. PEDOT (BSA) is compound
Film, obtained electrode designations are PEDOT (BSA)/Pt.
2. a kind of preparation method of poly- dioxyethylene thiophene composite membrane as described in claim 1, it is characterised in that in step (3)
In, the specification of the Pt electrode is
3. a kind of preparation method of poly- dioxyethylene thiophene composite membrane as described in claim 1, it is characterised in that in step (3)
In, the auxiliary electrode uses Ag/AgCl for auxiliary electrode.
4. a kind of preparation method of poly- dioxyethylene thiophene composite membrane as described in claim 1, it is characterised in that in step (3)
In, the scanning current potential of the Electrochemical Scanning is 0~1V, sweep speed 0.01V/s, and scanning circle number is 5 circles, and operation temperature is
25 DEG C, it is 1cm that length is polymerize on working electrode.
5. as a kind of poly- dioxyethylene thiophene composite membrane of any one of Claims 1 to 4 the method preparation is preparing electrode
It is applied in material；The electrode material includes platinum electrode, carbon paper electrode, Au electrode.
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| US6987164B2 (en) * | 2002-03-09 | 2006-01-17 | Samsung Electronics Co., Ltd. | Electrically conductive polymer, sensor using the same, and method for detecting target molecule using the sensor |
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| Enhancing the sensitivity and stability of HRP/PANI/Pt electrode by implanted bovine serum albumin;Chien-Chung Chen等;《Biosensors and Bioelectronics》;20070823;第765-770页 |
| 杨欢.微米级高导向PEDOT膜与PEDOT/α-ZrP复合膜的制备与应用.《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2015, |
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