CN1727884A - PVP/CdS quantum point modified electrode, and preparation method - Google Patents
PVP/CdS quantum point modified electrode, and preparation method Download PDFInfo
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- CN1727884A CN1727884A CN 200510027143 CN200510027143A CN1727884A CN 1727884 A CN1727884 A CN 1727884A CN 200510027143 CN200510027143 CN 200510027143 CN 200510027143 A CN200510027143 A CN 200510027143A CN 1727884 A CN1727884 A CN 1727884A
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Abstract
A PVP / CdS quantum point modification electrode is composed of vitreous carbon electrode and PVP / CdS quantum point composite material film as well as Nafion film on said electrode. Its preparing method includes preparing PVP / CdS quantum point composite material with raw materials of PVP. Na2S. 9 H2O; and 2 CdCI2. 5 H2O; making it to modify solution and dropping as well as coating solution on said electrode surface for forming a layer of PVP / CdS film, then dropping and coating Nation methanol solution on said film for forming a layer of Nation film.
Description
Technical field
The present invention relates to a kind of PVP/CdS quanta dot modified electrode and preparation method thereof, belong to the technical field of nano-modified electrode and preparation thereof.PVP is a polyvinylpyrrolidone.
Background technology
Protein is a kind of informational macromolecule, all play a crucial role in all life processes, thereby the research galvanochemistry of protein and electronic transfer process is for disclosing the essential significant of life process.Simultaneously, quantitative analysis of protein is also quite important, because the amount of protein often is used as the important references value of other compound mensurations or even the important basis for estimation of various clinical medical diagnosis on disease (as anaemia, miocardial infarction etc.) in the body fluid.But because the huge three-D space structure of protein causes its electric activity center to be embedded in the polypeptied chain, and it is in conventional electrodes, cause the passivation of electrode surface as the absorption sex change meeting on the surface of glass-carbon electrode, so the electron transfer speed of protein on general electrode is very slow, can not get effective current-responsive, its Direct Electrochemistry research is very restricted.
(quantum dot is the semiconductor nanocrystal that shows quantum size effect QD) to quantum dot, and its size is less than the mutually semi-conductive bohr diameter of its corresponding body, usually at 2～20nm.Quantum dot is along with crystalline size reduces, and the semiconductor energy level more and more separates, and effectively band gap increases, and can obtain unique optics and electrical properties.The electrical properties of this uniqueness helps being used for realizing to protein, as Direct Electrochemistry researchs on electrode such as haemoglobin, myoglobins, cytochrome cs.But, be applied to chemically modified electrode and realize the research report is not seen in the Direct Electrochemistry detection of biomolecule as yet for its unique electrical properties.
Summary of the invention
First technical matters that the present invention will solve is to release a kind of PVP/CdS quanta dot modified electrode 1.The advantage of kind electrode is that the preparation method is easy, with low cost, the dressing agent particle size is little, significant quantum size effect is arranged, the Electrochemical Detection that is used for protein as the working electrode of electrochemical detector, can be implemented in the protein electrochemical response that can't obtain on the glass-carbon electrode 10, highly sensitive, response speed is fast, good stability can be realized the direct mensuration to protein concentration in the solution.
The technical scheme that the present invention solves the problems of the technologies described above employing is: described quanta dot modified electrode has following structure, with existing glass-carbon electrode 10 is base electrode, one deck PVP/CdS quantum dot composite material film 3 is arranged on the surface 2 of glass-carbon electrode, one deck Nafion film 4 is arranged on PVP/CdS quantum dot composite material film 3.
Principle of work:
As shown in Figure 2, in electrolytic cell, be working electrode with PVP/CdS quanta dot modified electrode 1, Pt electrode 5 is to electrode, and saturated calomel electrode 6 is a contrast electrode, sets up three-electrode system, electrolytic solution 8 is phosphate buffer solution in the electrolytic cell 7, this solution letting nitrogen in and deoxidizing before experiment.Electrochemical gaging is finished under nitrogen atmosphere.With the CHI832 electrochemical workstation three-electrode system is carried out the Data Control transmission, adopt cyclic voltammetry that electrochemical behavior is investigated.PVP/CdS quanta dot modified electrode 1 does not have feature redox peak in the phosphate buffer solution of blank, substrate current obviously reduces than glass-carbon electrode 10, and this is because due to the characteristic of semiconductor of quantum dot.When quanta dot modified electrode carries out cyclic voltammetry scan in containing the phosphate buffer solution of protein, sensitive reduction peak has appearred near-0.2V, and along with the increase of protein concentration, peak current increases linearly, can carry out quantitative measurement to protein concentration according to its peak current size.
Producing the reason of this electrochemical behavior, is that these surface atoms have very high activity because greatly reducing of CdS quantum point grain diameter makes most of atom be positioned at the surface of quantum dot on the one hand; The specific surface area of quantum dot increases along with reducing of particle diameter in addition, has greatly increased with the direct surface of protein molecule to contact, and has improved the efficient of electron transport; On the other hand, PVP has good bio-compatibility, it is a kind of good dispersant, the CdS quantum dot that makes is evenly distributed in the PVP film form a space lattice, simultaneously, because the cubic three-D space structure of CdS quantum dot can promote electronics to transmit quickly and efficiently well, making observation be difficult to observed protein electrochemical response originally on glass-carbon electrode 10 becomes possibility.
Second technical matters that the present invention will solve is to release a kind of method of the PVP/CdS of preparation quanta dot modified electrode 1.
It is with polyvinylpyrrolidone, Na that the present invention solves the problems of the technologies described above the technical scheme that is adopted
2S9H
2O and 2CdCl
25H
2O is a raw material, preparation PVP/CdS quantum dot composite material, then the PVP/CdS quantum dot composite material is made decorating liquid, drip and to be coated on the surface 2 of glass-carbon electrode, dry formation one deck PVP/CdS quantum dot composite material film 3 naturally, on PVP/CdS quantum dot composite material film 3, drip again and be coated with the Nafion methanol solution, naturally dry, form one deck Nafion film 4, make PVP/CdS quanta dot modified electrode 1.
Now describe the technical scheme that the present invention prepares electrode in detail.A kind of method for preparing PVP/CdS quanta dot modified electrode 1 is a base electrode with existing glass-carbon electrode 10, it is characterized in that the concrete operations step:
The preparation of first step PVP/CdS quantum dot composite material
CdCl with 0.05～0.2mol/L concentration
2Solution injects 5%～20% polyvinylpyrrolidonesolution solution, feeds N
2, stir 30～45min in the ice-water bath, under agitation, with Na
2S solution splashes into CdCl
2In the mixed solution of polyvinylpyrrolidone, Na
2S and CdCl
2Mol ratio be 1: 2, stirring reaction 30～60min in the ice-water bath, it is centrifugal to add acetone again in solution, get the precipitation nature and dry, the PVP/CdS quantum dot composite material;
The preparation of the second step decorating liquid
PVP/CdS quantum dot composite material with the first step makes adds redistilled water, and the mass ratio of PVP/CdS quantum dot composite material and distilled water 1: 10～200 is ultrasonic even, gets decorating liquid;
Glass-carbon electrode 10 pre-service of the 3rd step
With the method for the grinding and buffing of routine grinding and buffing is carried out on the surface 2 of glass-carbon electrode and handle, use 1mol/L NaOH solution, 1mol/L HNO successively
3Solution, acetone and redistilled water supersound washing;
The preparation of the 4th step PVP/CdS quanta dot modified electrode 1
The modification drop that second step was made is coated on the surface 2 of the 3rd step pretreated glassy carbon electrode, and dripping the amount of being coated with is 0.7 μ L/mm
2, leave standstill, dry naturally, form one deck PVP/CdS quantum dot composite material film 3, on PVP/CdS quantum dot composite material film 3, drip and be coated with the Nafion methanol solution, form one deck Nafion film 4, the volume ratio of Nafion and methyl alcohol is 1: 200～500, and dripping the amount of being coated with is 0.7 μ L/mm
2, get PVP/CdS quanta dot modified electrode 1.
The technical scheme that the present invention prepares electrode is further characterized in that, in the first step, and Na
2S and CdCl
2Mol ratio be 1: 1.
The technical scheme that the present invention prepares electrode is further characterized in that, in the first step, and Na
2S and CdCl
2Mol ratio be 2: 1.
Compare with existing glass-carbon electrode 10, the present invention has the following advantages:
1, PVP/CdS quanta dot modified electrode 1 of the present invention can be implemented in the protein Direct Electrochemistry response that can't realize on the glass-carbon electrode 10.Its reason is to have modified the PVP/CdS quantum dot composite material on the surface 2 of glass-carbon electrode, its particle size is 2～5nm, because reducing greatly of particle diameter obtained high specific surface area, greatly increased with the direct surface of protein and contacted, improved the efficient of electron transport; Simultaneously because the cubic three-D space structure of CdS quantum dot has promoted transmitting efficiently rapidly of electronics well.
2, PVP/CdS quanta dot modified electrode 1 of the present invention has good stable performance and sensitive electrocatalysis characteristic.PVP is a kind of non-ionic macromolecule compound of excellent performance, chemical property is stable, it is prepared the PVP/CdS quantum dot as coating material, make the quantum dot favorable dispersibility that makes, be difficult for reuniting, particle diameter is littler, and size distribution is more even, has guaranteed the good stable performance and the sensitive electrocatalysis characteristic of electrode of the present invention.
3, PVP/CdS quanta dot modified electrode 1 of the present invention, wide to the electrochemical gaging range of linearity of protein, detectability is low.The range of linearity can reach 3 more than the order of magnitude, and detectability is reduced to 10
-8The mol/L order of magnitude can directly detect the solution that contains micro-haemoglobin, myoglobins, cytochrome c etc., for example human whole blood sample etc.
4, PVP/CdS quanta dot modified electrode 1 of the present invention has good bio-compatibility, and protein is improved in the shortcoming of the surface of glass-carbon electrode 2 changeablenesies, and be improved the serviceable life of electrode.
Technology was simple, easy to operate when 5, method of the present invention prepared PVP/CdS quantum dot composite material film 3 and Nafion film 4, low cost of manufacture.
Description of drawings
The structural representation of Fig. 1 PVP/CdS quanta dot modified electrode 1 of the present invention.
Wherein: 1 is the PVP/CdS quanta dot modified electrode in the macrograph, 2 is the surface of glass-carbon electrode in the microgram, 3 is PVP/CdS quantum dot composite material film, and 4 is the Nafion film, and microgram is the structural representation at the electrode end surface place of PVP/CdS quanta dot modified electrode 1 in the macrograph.
Fig. 2 PVP/CdS quanta dot modified electrode 1 of the present invention is used for the synoptic diagram of three-electrode cell.
Wherein: 5 is the Pt electrode, and 6 is saturated calomel electrode, and 7 is electrolytic cell, and 8 is electrolytic solution, and 9 is electrode suppor.
The TEM phenogram of Fig. 3 PVP/CdS quantum dot of the present invention decorating liquid.
The XRD phenogram of Fig. 4 PVP/CdS quantum dot of the present invention decorating liquid.
The structural representation of the existing glass-carbon electrode 10 of Fig. 5.
Wherein: 10 is glass-carbon electrode in the macrograph, in the microgram 2 for the surface microscopic figure of glass-carbon electrode be the structural representation at the electrode end surface place of glass-carbon electrode 10 in the macrograph.
Embodiment
One of preparation of embodiment 1 PVP/CdS quanta dot modified electrode 1
CdCl with 0.05mol/L
2Solution 1mL injects the aqueous solution of 40mL5% polyvinylpyrrolidone (PVP), feeds N
2, stir 30min in the ice-water bath.Under agitation, with the Na of the 0.01mol/L of 5mL
2S solution splashes into CdCl
2In the mixed solution of polyvinylpyrrolidone, solution gradually by colourless become faint yellow, reaction 30min.After reaction finished, adding acetone was centrifugal, got the precipitation nature and dried, and got the PVP/CdS quantum dot composite material.Characterized by transmission electron microscope (TEM), see Fig. 3, can find out that the quantum dot of this PVP/CdS quantum dot composite material is a spheric grain, mean grain size is about 3.4nm.The above-mentioned PVP/CdS quantum dot composite material that makes of 10mg is joined in L distilled water of 100 μ, ultrasonic even, get decorating liquid.
The surface 2 of glass-carbon electrode is through the abrasive paper for metallograph polishing and containing the Al that particle size is 0.05 μ m magnitude
2O
3After the polishing, use 1mol/L NaOH solution, 1mol/LHNO successively on the chamois leather of powder
3Solution, acetone and redistilled water supersound washing.Be coated on the surface 2 of pretreated glass-carbon electrode modifying drop, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck PVP/CdS quantum dot composite material film 3, on PVP/CdS quantum dot composite material film 3, drip again and be coated with the 0.2%Nafion methanol solution, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck Nafion film 4, get PVP/CdS quanta dot modified electrode 1.
Two of the preparation of embodiment 2 PVP/CdS quanta dot modified electrodes 1
CdCl with 0.1mol/L
2Solution 2mL injects 80mL 10%PVP aqueous solution, feeds N
2, in ice-water bath, stir 40min.Under agitation, with the Na of the 0.01mol/L of 10mL
2S solution splashes into CdCl
2In the mixed solution of polyvinylpyrrolidone, solution gradually by colourless become faint yellow, reaction 45min.After reaction was finished, adding acetone was centrifugal, got the precipitation nature and dried, and got the PVP/CdS quantum dot composite material.Characterize through XRD, see Fig. 4, the size of the particle of PVP/CdS quantum dot is about 2.7nm.The above-mentioned quantum dot composite material that makes of 10mg is joined in the 1mL redistilled water, ultrasonic even, get decorating liquid.
The surface 2 of glass-carbon electrode is through the abrasive paper for metallograph polishing and containing the Al that particle size is 0.05 μ m magnitude
2O
3After the polishing, use 1mol/L NaOH solution, 1mol/LHNO successively on the chamois leather of powder
3Solution, acetone and redistilled water supersound washing.Be coated on the surface 2 of the good glass-carbon electrode of pre-service modifying drop, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck PVP/CdS quantum dot composite material film 3, on PVP/CdS quantum dot composite material film 3, drip again and be coated with the 0.3%Nafion methanol solution, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck Nafion film 4, get PVP/CdS quanta dot modified electrode 1.
Three of the preparation of embodiment 3 PVP/CdS quanta dot modified electrodes 1
CdCl with 0.2mol/L
2Solution 1mL injects the 40mL20%PVP aqueous solution, feeds N
2, in ice-water bath, stir 45min.Under agitation, with the Na of the 0.02mol/L of 20mL
2S solution splashes into CdCl
2In the mixed solution of polyvinylpyrrolidone, solution gradually by colourless become faint yellow, reaction 60min.After reaction was finished, adding acetone was centrifugal, got the precipitation nature and dried, and got the PVP/CdS quantum dot composite material.The above-mentioned quantum dot composite material that makes of 10mg is joined in the 2mL redistilled water, ultrasonic even, get decorating liquid.
The surface 2 of glass-carbon electrode is through the abrasive paper for metallograph polishing and containing the Al that particle size is 0.05 μ m magnitude
2O
3After the polishing, use 1mol/L NaOH solution, 1mol/LHNO successively on the chamois leather of powder
3Solution, acetone and redistilled water supersound washing.Be coated on the glass-carbon electrode surface of handling well 2 modifying drop, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck PVP/CdS quantum dot composite material film 3, on PVP/CdS quantum dot composite material film 3, drip again and be coated with the 0.5%Nafion methanol solution, dripping the amount of being coated with is 0.7 μ L/mm
2, dry naturally, form one deck Nafion film 4, get PVP/CdS quanta dot modified electrode 1.
1 pair of protein measuring of embodiment 4 PVP/CdS quanta dot modified electrodes
With the PVP/CdS quanta dot modified electrode 1 that makes among the embodiment 3 as working electrode, Pt electrode 5 is to electrode, saturated calomel electrode 6 is a contrast electrode, set up three-electrode system as shown in Figure 2, electrolytic solution 8 is the phosphate buffer solution of 0.1mol/L in the electrolytic cell 7, this solution letting nitrogen in and deoxidizing before experiment.Electrochemical gaging is finished under nitrogen atmosphere.With the CHI832 electrochemical workstation described three-electrode system is carried out the Data Control transmission, adopt cyclic voltammetry that electrochemical behavior is investigated.Prepare 5.0 * 10 respectively
-6The haemoglobin of mol/L, myoglobins and cytochrome c solution, the reduction current response that obtains on PVP/CdS quanta dot modified electrode 1 is respectively 5.44,6.32 and 5.78 μ A.And, on existing glass-carbon electrode 10, can not get the reduction current response with the protein solution of concentration.
Claims (4)
1, a kind of PVP/CdS quanta dot modified electrode (1), with existing glass-carbon electrode (10) is base electrode, it is characterized in that, it has following structure, on the surface (2) of glass-carbon electrode, one deck PVP/CdS quantum dot composite material film (3) is arranged, one deck Nafion film (4) is arranged on PVP/CdS quantum dot composite material film (3).
2, the preparation method of the described PVP/CdS quanta dot modified electrode of claim 1 (1) is a base electrode with existing glass-carbon electrode (10), it is characterized in that the concrete operations step:
The preparation of first step PVP/CdS quantum dot composite material
CdCl with 0.05～0.2mol/L concentration
2Solution injects 5%～20% polyvinylpyrrolidonesolution solution, feeds N
2, stir 30～45min in the ice-water bath, under agitation, with Na
2S solution splashes into CdCl
2In the mixed solution of polyvinylpyrrolidone, Na
2S and CdCl
2Mol ratio be 1: 2, stirring reaction 30～60min in the ice-water bath, it is centrifugal to add acetone again in solution, get the precipitation nature and dry, the PVP/CdS quantum dot composite material;
The preparation of the second step decorating liquid
PVP/CdS quantum dot composite material with the first step makes adds redistilled water, and the mass ratio of PVP/CdS quantum dot composite material and distilled water 1: 10～200 is ultrasonic even, gets decorating liquid;
Glass-carbon electrode (10) pre-service of the 3rd step
With the method for the grinding and buffing of routine grinding and buffing is carried out on the surface (2) of glass-carbon electrode and handle, use 1mol/L NaOH solution, 1mol/L HNO successively
3Solution, acetone and redistilled water supersound washing;
The preparation of the 4th step PVP/CdS quanta dot modified electrode (1)
The modification drop that second step was made is coated on the surface (2) of the 3rd step pretreated glassy carbon electrode, and dripping the amount of being coated with is 0.7 μ L/mm
2, leave standstill, dry naturally, form one deck PVP/CdS quantum dot composite material film (3), be coated with the Nafion methanol solution, form one deck Nafion film (4) last the dripping of PVP/CdS quantum dot composite material film (3), the volume ratio of Nafion and methyl alcohol is 1: 200～500, and dripping the amount of being coated with is 0.7 μ L/mm
2, get PVP/CdS quanta dot modified electrode (1).
3, the preparation method of PVP/CdS quanta dot modified electrode according to claim 2 (1) is characterized in that, in the first step, and Na
2S and CdCl
2Mol ratio be 1: 1.
4, the preparation method of PVP/CdS quanta dot modified electrode according to claim 2 (1) is characterized in that, in the first step, and Na
2S and CdCl
2Mol ratio be 2: 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104391006A (en) * | 2014-11-13 | 2015-03-04 | 无锡信大气象传感网科技有限公司 | Preparation method of gas sensor |
| CN111427111A (en) * | 2020-03-30 | 2020-07-17 | Tcl华星光电技术有限公司 | Quantum dot patterning method, device and system |
| US11377723B2 (en) | 2020-03-30 | 2022-07-05 | Tcl China Star Optoelectronics Technology Co., Ltd. | Method of patterning quantum dots, device using same, and system thereof |
-
2005
- 2005-06-24 CN CN 200510027143 patent/CN1727884A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104391006A (en) * | 2014-11-13 | 2015-03-04 | 无锡信大气象传感网科技有限公司 | Preparation method of gas sensor |
| CN111427111A (en) * | 2020-03-30 | 2020-07-17 | Tcl华星光电技术有限公司 | Quantum dot patterning method, device and system |
| US11377723B2 (en) | 2020-03-30 | 2022-07-05 | Tcl China Star Optoelectronics Technology Co., Ltd. | Method of patterning quantum dots, device using same, and system thereof |
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