CN108918506A - A kind of preparation method of ZnTPP flower-shape aggregation and its composite material - Google Patents
A kind of preparation method of ZnTPP flower-shape aggregation and its composite material Download PDFInfo
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- CN108918506A CN108918506A CN201810481293.8A CN201810481293A CN108918506A CN 108918506 A CN108918506 A CN 108918506A CN 201810481293 A CN201810481293 A CN 201810481293A CN 108918506 A CN108918506 A CN 108918506A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
Abstract
The invention discloses a kind of preparation method of ZnTPP flower-shape aggregation, this method includes：Tetraphenyl zinc protoporphyrin is self-assembled into ZnTPP flower-shape aggregation in the in the mixed solvent of chloroform and methanol.The aggregation of ZnTPP flower-shape prepared by the method for the present invention physical efficiency is obviously improved the electrochemical luminescence performance of ZnTPP, after the ZnTPP flower-shape aggregation and redox graphene are compound, the electrochemical luminescence performance of material can be further promoted, which can be used for preparing electrochemical luminescence device.
Description
Technical field
The invention belongs to electrochemical luminescence Material Fields, and in particular to a kind of ZnTPP flower-shape aggregation and its composite material
Preparation method.
Background technique
Currently, electrochemical luminescence (also referred to as electrochemical luminescence, abbreviation ECL) has become a powerful analysis tool, by
It is easy to operate in its advantage, such as high sensitivity, have many advantages, such as that good time and space control to light emitting, very
It is multi-field to be widely used.ECL is the electron transfer reaction that high-energy occurs for the electronics that species generate on the electrode, shape
At luminous excitation state.In other words, ECL refers to the chemiluminescence triggered by electrochemical method.It represents a kind of valuable
The electrochemistry of value and chemiluminescent combination.ECL reaction usually requires illuminator, also referred to as electrochemical luminescence reagent.Several allusion quotations
The ECL luminescent substance such as luminol of type, quantum dot, porphyrin is by wide coverage and research.
Summary of the invention
It is an object of the invention to the statuses according to above-mentioned background technique, provide a kind of system of ZnTPP flower-shape aggregation
The composite material of Preparation Method and the ZnTPP flower-shape aggregation and redox graphene.
In order to solve the above-mentioned technical problems, the present invention provides the following technical solutions：
A kind of preparation method of ZnTPP flower-shape aggregation, including：Mixing of the tetraphenyl zinc protoporphyrin in chloroform and methanol
ZnTPP flower-shape aggregation is self-assembled into solvent.
Preferably, the volume ratio of chloroform and methanol is 1:1.
Preferably, tetraphenyl zinc protoporphyrin is 5~15mmol/L in the concentration of in the mixed solvent.
Preferably, tetraphenyl zinc protoporphyrin is first dissolved with chloroform, adds methanol.
A kind of ZnTPP flower-shape aggregation prepared according to any of the above-described method.
A kind of ZnTPP flower-shape aggregation/redox graphene composite material, including redox graphene and attached
ZnTPP flower-shape aggregation as described above on redox graphene.
A method of above-mentioned ZnTPP flower-shape aggregation/redox graphene composite material is prepared, including：By electrode
It immerses in graphene oxide dispersion, by electrochemical reduction, obtains redox graphene film in electrode surface, then will
ZnTPP flower-shape aggregation drop coating on the electrode to get arrive ZnTPP flower-shape aggregation/redox graphene composite material.
Above-mentioned ZnTPP flower-shape aggregation is preparing the application in electrochemical luminescence device.
Above-mentioned ZnTPP flower-shape aggregation/redox graphene composite material is preparing answering in electrochemical luminescence device
With.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the scanning electron microscope diagram of SA-ZnTPP of the invention.
Fig. 2 is the uv absorption spectra of ZnTPP, SA-ZnTPP of the invention.
Fig. 3 is the electrochemical luminescence signals comparison diagram of ZnTPP, SA-ZnTPP of the invention.
The explanatory diagram that the electrochemical luminescence signals that Fig. 4 is SA-ZnTPP/RGO of the invention increase.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
It weighs 0.0068g ZnTPP (tetraphenyl zinc protoporphyrin) to be dissolved in 0.5mL chloroform, forming concentration is 20mM's
Uniform porphyrin solution, is then added 0.5mL methanol, at this time in mixed solvent (V (CHCl in this solution3:CH3OH)=1:1)
Under the conditions of, the concentration of porphyrin solution is 10mM (just formation saturated solution), and the flower-shape aggregation for foring ZnTPP at this time is denoted as
Self-assembled ZnTPP(SA-ZnTPP)。
The above-mentioned SA-ZnTPP drop coating of 2.5 μ L is taken on the electrode, in 0.1M PBS (0.1M KH2PO4-K2HPO4；pH 7.4；
Supporting electrolyte is KCl) its electrochemical luminescence signals is scanned in buffer solution.
By electrode immerse concentration be 0.72mg/mL graphene oxide aqueous dispersions in, by electrochemical reduction (-
In the voltage range of 1.5-0.6V, 10 circle of scanning under the parameter of speed is swept with 0.025V/s), oxygen reduction fossil is obtained in electrode surface
Black alkene film, then take the above-mentioned SA-ZnTPP drop coating of 2.5 μ L on the electrode to get to ZnTPP flower-shape aggregation/redox graphene
Composite material.In 0.1M PBS (0.1M KH2PO4-K2HPO4, pH 7.4；Supporting electrolyte is KCl) it is scanned in buffer solution
Electrochemical luminescence signals.
Embodiment 2
It weighs 0.0034g ZnTPP to be dissolved in 0.5mL chloroform, it is molten to form the uniform porphyrin that concentration is 10mM
Then 0.5mL methanol is added, at this time in mixed solvent (V (CHCl in liquid in this solution3:CH3OH)=1:1) under the conditions of, porphyrin
The concentration of solution is 5mM (for unsaturated solution), and the flower-shape aggregation for foring ZnTPP at this time is denoted as Self-assembled
ZnTPP(SA-ZnTPP)。
The above-mentioned SA-ZnTPP drop coating of 2.5 μ L is taken on the electrode, in 0.1M PBS (0.1M KH2PO4-K2HPO4；pH 7.4；
Supporting electrolyte is KCl) its electrochemical luminescence signals is scanned in buffer solution.
By electrode immerse concentration be 0.72mg/mL graphene oxide aqueous dispersions in, by electrochemical reduction (-
In the voltage range of 1.5-0.6V, 10 circle of scanning under the parameter of speed is swept with 0.025V/s), oxygen reduction fossil is obtained in electrode surface
Black alkene film, then take the above-mentioned SA-ZnTPP drop coating of 2.5 μ L on the electrode to get to ZnTPP flower-shape aggregation/redox graphene
Composite material.
Embodiment 3
It weighs 0.01017g ZnTPP to be dissolved in 0.5mL chloroform, it is molten to form the uniform porphyrin that concentration is 30mM
Then 0.5mL methanol is added, at this time in mixed solvent (V (CHCl in liquid in this solution3:CH3OH)=1:1) under the conditions of, porphyrin
The concentration of solution is 15mM (for supersaturated solution), and the flower-shape aggregation for foring ZnTPP at this time is denoted as Self-assembled
ZnTPP(SA-ZnTPP)。
The above-mentioned SA-ZnTPP drop coating of 2.5 μ L is taken on the electrode, in 0.1M PBS (0.1M KH2PO4-K2HPO4；pH 7.4；
Supporting electrolyte is KCl) its electrochemical luminescence signals is scanned in buffer solution.
By electrode immerse concentration be 0.72mg/mL graphene oxide aqueous dispersions in, by electrochemical reduction (-
In the voltage range of 1.5-0.6V, 10 circle of scanning under the parameter of speed is swept with 0.025V/s), oxygen reduction fossil is obtained in electrode surface
Black alkene film, then take the above-mentioned SA-ZnTPP drop coating of 2.5 μ L on the electrode to get to ZnTPP flower-shape aggregation/redox graphene
Composite material.
Graphene oxide can be used commercial product or prepare with reference to existing literature.
Redox graphene film can be indicated with RGO.
Fig. 3 is the electrochemical luminescence signals comparison diagram of ZnTPP, SA-ZnTPP of the invention, as seen from the figure, ZnTPP
After being self-assembled into flower-shape aggregation, electrochemical luminescence luminous intensity increases significantly.
The explanatory diagram that the electrochemical luminescence signals that Fig. 4 is SA-ZnTPP/RGO of the invention increase, it is compound with RGO, it can be into
The electrochemical luminescence performance of one step promotion SA-ZnTPP.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (9)
1. a kind of preparation method of ZnTPP flower-shape aggregation, including：Tetraphenyl zinc protoporphyrin is molten in the mixing of chloroform and methanol
ZnTPP flower-shape aggregation is self-assembled into agent.
2. preparation method according to claim 1, it is characterised in that：The volume ratio of chloroform and methanol is 1:1.
3. preparation method according to claim 1, it is characterised in that：Tetraphenyl zinc protoporphyrin is in the concentration of in the mixed solvent
5~15mmol/L.
4. preparation method according to claim 1, it is characterised in that：Tetraphenyl zinc protoporphyrin is first dissolved with chloroform, then
Methanol is added.
5. a kind of ZnTPP flower-shape aggregation according to any the method preparation of Claims 1 to 4.
6. a kind of ZnTPP flower-shape aggregation/redox graphene composite material, including redox graphene, and be attached to
ZnTPP flower-shape aggregation as claimed in claim 5 on redox graphene.
7. ZnTPP flower-shape aggregation/redox graphene composite material method described in claim 6 is prepared a kind of, including：
Electrode is immersed in graphene oxide dispersion, by electrochemical reduction, obtains redox graphene film in electrode surface, then
By ZnTPP flower-shape aggregation drop coating on the electrode to get arrive ZnTPP flower-shape aggregation/redox graphene composite material.
8. the application of ZnTPP flower-shape aggregation described in claim 5, the ZnTPP flower-shape aggregation are preparing electrochemical luminescence
Application in device.
9. ZnTPP flower-shape aggregation/redox graphene composite material application described in claim 6, the ZnTPP flower-shape
Aggregation/redox graphene composite material is preparing the application in electrochemical luminescence device.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114047156A (en) * | 2021-10-09 | 2022-02-15 | 中南民族大学 | Identification method for dendrobium huoshanense cultivation mode and age limit |
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| CN114047156B (en) * | 2021-10-09 | 2022-10-18 | 中南民族大学 | Identification method for dendrobium huoshanense cultivation mode and age limit |
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