CN106745187B - The preparation and the application in terms of biosensor of a kind of zinc oxide nano popped rice - Google Patents
The preparation and the application in terms of biosensor of a kind of zinc oxide nano popped rice Download PDFInfo
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- CN106745187B CN106745187B CN201611014931.2A CN201611014931A CN106745187B CN 106745187 B CN106745187 B CN 106745187B CN 201611014931 A CN201611014931 A CN 201611014931A CN 106745187 B CN106745187 B CN 106745187B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
A kind of preparation the present invention relates to zinc oxide nano popped rice and the application in terms of biosensor, belong to new function material and biosensor detection technique field.The present invention is to solve current materials to detect the problem of levodopa sensitivity is relatively low in biological sensor.Preparation method of the present invention is as follows：First, hydrothermal synthesis method；2nd, automatic spraying process.The zinc oxide nano popped rice prepared has the characteristics that large specific surface area, good conductivity and is accumulated with solution contact surface big.Present invention is mainly used for prepare a kind of preparation and its application of zinc oxide nano popped rice.
Description
Technical field
The present invention relates to a kind of preparation method and applications of zinc-oxide nano floral material.
Background technology
Zinc oxide is a kind of Group II-VI semiconductor material, that zinc oxide nanowire has a morphology controllable and be easily-synthesized excellent
Point has excellent bio-compatibility, outside chemical stability, can be provided when biosensor detects biomolecule straight
It connects, quick electron channel.And the porosity and the specific surface area of bigger for having the zinc oxide nano popped rice of three-dimensional structure big make it
With the contact area bigger of solution.The method of common synthesizing zinc oxide nano flower is hydrothermal synthesis method, and this method has cost
It is low, the simple advantage of building-up process.
Parkinson's disease is a kind of common nervous system degeneration disease, and most important pathological change is substantia nigra of midbrain dopamine
The denaturation of serotonergic neuron is dead, thus DOPAMINE CONTENT IN RABBIT is caused to substantially reduce and cause a disease.Levodopa（L-dopa）It is also known as left more
Bar, it is a kind of antiparkinsonian drug, is mainly used to treat Parkinson disease.Levodopa is by blood cerebral disorders and in aromatic amine
Dopamine is generated under the action of base acid decarboxylase, to make up the deficiency of brain dopamine, but levodopa content mistake in human body
Toxic side effect can mostly be generated.So accurately detection levodopa has very important significance in the in vivo content of people.
The content of the invention
The purpose of the present invention is prepare zinc oxide nano popped rice by hydro-thermal method and prepare oxidation using automatic spraying process
Zinc nano flower/ITO electrode, and by the electrode for the detection of levodopa.
A kind of preparation method of zinc oxide nano popped rice/ITO electrode provided by the invention is to carry out according to the following steps：
First, hydrothermal synthesis method：
1）By the use of distilled water as the solvent zinc nitrate solution that compound concentration is 0.03mol/L~0.07mol/L respectively,
The hexa solution of 0.03mol/L~0.07mol/L, the ammonia spirit of 0mol/L~0.07mol/L and 0mmol/L~
The polyetherimide solution of 7mmol/L, and by four kinds of solution after mixing with the rotating speed magnetic force of 450r/min~550r/min
Stirring 3min~5min obtains hydro-thermal reaction solution；
2）By step 1）Obtained hydro-thermal reaction solution is poured into reaction kettle, covers reaction kettle lid, 90 DEG C~120
DEG C temperature conditionss under reaction 11 ~ 13 it is small when, then take out cooled to room temperature in air, obtain zinc oxide nano popped rice,
It opens reaction kettle distilled water material clean is clean, and the zinc oxide nano popped rice after filtering is transferred in culture dish, be put into
Zinc oxide nano popped rice is obtained when drying 1 ~ 3 is small at 70 DEG C~90 DEG C in drying box；
2nd, automatic spraying process
1）The deionized water of the zinc oxide nano popped rice of 0.01g ~ 0.03g and 20mL is mixed to get zinc oxide suspension；
2）After ITO electro-conductive glass is cleaned by ultrasonic 20min in acetone soln, ethanol solution and deionized water respectively, in room
The lower natural cooling drying of temperature.Six pieces of ITO electro-conductive glass are fixed in spraying equipment heating plate, it is with adhesive tape that ITO is conductive
Glass clamp electrode wires one side covers, and ensures that electrode wires are contacted directly with ITO electro-conductive glass；
3）Finely dispersed burnett's solution is prepared into zinc oxide nano popped rice/ITO electricity in spray gun using automatic spraying process
Pole, entire spraying process carry out under 10 psi air inlet pressures, and the distance of nozzle to ITO electro-conductive glass is 15cm, heating dish temperature
For 160 DEG C, burnett's solution is stirred continuously with mini-sized blender in spraying process；
4）The ITO electrode for being coated with zinc oxide nano popped rice is placed in quartz tube furnace, under air, with 10 DEG C
min-1Heating rate to 450 DEG C heat preservation 1h, then furnace cooling to room temperature；
5）0.1% Nafion solution of the μ L of 5 μ L~20 is added dropwise on ITO electro-conductive glass after the cooling period, finally obtains oxidation
Zinc nano flower/ITO electrode.
Advantages of the present invention：
1）For the present invention using hydrothermal synthesis method, this method, which has, synthesizes at low cost, the simple advantage of building-up process, Ran Houyong
Automatic spraying process constructs zinc oxide nano popped rice/ITO electrode in the case where Seed Layer is not required；
2）The zinc-oxide nano floral material that the present invention prepares maintain the excellent biocompatibility of original zinc oxide and
Directly, outside quick electron channel, the specific surface area of zinc oxide is increased, the contact area of itself and solution is made to become larger, improves material
Expect chemical property, the sensitivity that may be such that Electrochemical Detection levodopa is 0.1 μ A μM-1。
Description of the drawings：
Fig. 1 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment two is prepared amplifies 10000 times；
Fig. 2 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment three is prepared amplifies 10000 times；
Fig. 3 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment four is prepared amplifies 10000 times；
Fig. 4 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment one is prepared amplifies 10000 times；
Fig. 5 is the X ray diffracting spectrum of zinc oxide nano popped rice prepared by experiment；
Fig. 6 is the Linear Fit Chart of the levodopa concentration that detection obtains and oxidation peak current.
Specific embodiment
Specific embodiment one：A kind of preparation method of zinc-oxide nano floral material in present embodiment, specifically press with
What lower step carried out：
First, hydrothermal synthesis method：
1）By the use of distilled water as the six of the solvent zinc nitrate solution that compound concentration is 0.05mol/L respectively and 0.05mol/L
Methenamine solution, and by both solution after mixing with the rotating speed magnetic agitation of 450r/min~550r/min
3min~5min obtains hydro-thermal reaction solution；
2）By step 1）Obtained hydro-thermal reaction solution is poured into reaction kettle, covers reaction kettle lid, 90 DEG C~120
DEG C temperature conditionss under reaction 11 ~ 13 it is small when, then take out cooled to room temperature in air, obtain zinc oxide nano popped rice,
It opens reaction kettle distilled water material clean is clean, and the zinc oxide nano popped rice after filtering is transferred in culture dish, be put into
Zinc oxide nano popped rice is obtained when drying 1 ~ 3 is small at 70 DEG C~90 DEG C in drying box；
2nd, automatic spraying process
1）The deionized water of the zinc oxide nano popped rice of 0.01g ~ 0.03g and 20mL is mixed to get zinc oxide suspension；
2）After ITO electro-conductive glass is cleaned by ultrasonic 20min in acetone soln, ethanol solution and deionized water respectively, in room
The lower natural cooling drying of temperature.Six pieces of ITO electro-conductive glass are fixed in spraying equipment heating plate, it is with adhesive tape that ITO is conductive
Glass clamp electrode wires one side covers, and ensures that electrode wires are contacted directly with ITO electro-conductive glass；
3）Finely dispersed burnett's solution is prepared into zinc oxide nano popped rice/ITO electricity in spray gun using automatic spraying process
Pole, entire spraying process carry out under 10 psi air inlet pressures, and the distance of nozzle to ITO electro-conductive glass is 15cm, heating dish temperature
For 160 DEG C, burnett's solution is stirred continuously with mini-sized blender in spraying process；
4）The ITO electrode for being coated with zinc oxide nano popped rice is placed in quartz tube furnace, under air, with 10 DEG C
min-1Heating rate to 450 DEG C heat preservation 1h, then furnace cooling to room temperature；
5）The 0.1%Nafion solution of the μ L of 5 μ L~20 is added dropwise on ITO electro-conductive glass after the cooling period, finally obtains zinc oxide
Nano flower/ITO electrode.
Specific embodiment two：The present embodiment is different from the first embodiment in that：Step 11）Made with distilled water
For the solvent zinc nitrate solution that compound concentration is 0.05mol/L respectively, 0.05mol/L hexa solution and
The ammonia spirit of 0.05mol/L, and by three kinds of solution after mixing with the rotating speed magnetic agitation 3 of 450r/min ~ 550r/min
~ 5min obtains hydro-thermal reaction solution；It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that：Step 11）With distillation
Water as solvent difference compound concentration be the zinc nitrate solution of 0.05mol/L, 0.05mol/L hexa solution,
The ammonia spirit of 0.05 mol/L and the polyetherimide solution of 2mmol/L, and by these four solution after mixing with 450r/
3 ~ 5min of rotating speed magnetic agitation of min ~ 550r/min obtains hydro-thermal reaction solution；Other and specific embodiment one or two-phase
Together.
Specific embodiment four：Present embodiment is unlike specific embodiment one to three：Step 11）With distillation
Water as solvent difference compound concentration be the zinc nitrate solution of 0.05mol/L, 0.05mol/L hexa solution,
0.05mol/L ammonium hydroxide and 5mmol/L polyetherimide solutions, and by these four solution after mixing with 450r/min ~ 550r/
3 ~ 5min of rotating speed magnetic agitation of min obtains hydro-thermal reaction solution；It is other identical with one of specific embodiment one to three.
Specific embodiment five：Present embodiment is unlike specific embodiment one to four：Step by 0.03g ~
The zinc oxide nano popped rice of 0.05g and the deionized water of 20mL are mixed to get zinc oxide suspension, other and specific embodiment one
It is identical to one of four.
Specific embodiment six：Present embodiment is unlike specific embodiment one to five:Step 25）At middle heat
After reason, the 0.1%Nafion solution of the μ L of 20 μ L~40 is added dropwise on the ITO electro-conductive glass of cooling, finally obtains zinc-oxide nano
Flower/ITO electrode is other identical with one of specific embodiment one to five.
Present embodiment is that a kind of zinc oxide nano popped rice/ITO is used as working electrode, is tested by Pulse Voltammetry method
Corresponding current value of the material to various concentration levodopa is obtained, so as to play the role of detecting levodopa.
Using following verification experimental verifications effect of the present invention：
Experiment one：A kind of preparation method of zinc-oxide nano floral material of this experiment is realized by the following method：
First, hydrothermal synthesis method：
1）By the use of distilled water as the solvent zinc nitrate solution that compound concentration is 0.05mol/L respectively, 0.05mol/L it is six sub-
The polyetherimide solution of tetramine solution, the ammonia spirit of 0.05 mol/L and 5mmol/L, and four kinds of solution are mixed
Hydro-thermal reaction solution is obtained with the rotating speed magnetic agitation 5min of 500 r/min after even；
2）By step 1）Obtained hydro-thermal reaction solution is poured into reaction kettle, covers reaction kettle lid, in 100 DEG C of temperature
12h is reacted under the conditions of degree, then takes out cooled to room temperature in air, obtains zinc oxide nano popped rice, reaction kettle is opened and uses
Distilled water is clean by material clean, and the zinc oxide nano popped rice after filtering is transferred in culture dish, is put into drying box 80
When drying 2 is small at DEG C；
2nd, automatic spraying process
1）The deionized water of the zinc oxide nano popped rice of 0.01 g and 20mL is mixed to get zinc oxide suspension；
2）After ITO electro-conductive glass is cleaned by ultrasonic 20min in acetone soln, ethanol solution and deionized water respectively, in room
The lower natural cooling drying of temperature.Six pieces of ITO electro-conductive glass are fixed in spraying equipment heating plate, it is with adhesive tape that ITO is conductive
Glass clamp electrode wires one side covers, and ensures that electrode wires are contacted directly with ITO electro-conductive glass；
3）Finely dispersed burnett's solution is prepared into zinc oxide nano popped rice/ITO electricity in spray gun using automatic spraying process
Pole, entire spraying process carry out under 10psi air inlet pressures, and the distance of nozzle to ITO electro-conductive glass is 15cm, and heating dish temperature is
160 DEG C, burnett's solution is stirred continuously with mini-sized blender in spraying process；
4）The ITO electrode for being coated with zinc oxide nano popped rice is placed in quartz tube furnace, under air, with 10 DEG C
min-1Heating rate to 450 DEG C heat preservation 1h, then furnace cooling to room temperature；
5）5 μ L0.1% Nafion solutions are added dropwise on ITO electro-conductive glass after the cooling period respectively, finally obtain zinc oxide nano
Popped rice/ITO electrode.
Fig. 1 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment two is prepared amplifies 10000 times；From figure
In it can be seen that zinc oxide nano popped rice limb it is also coarseer, for quantity also than sparse, nanometer rods are hexa-prism, and length is
1.5 ~ 2 μm, diameter is about 500nm.
Fig. 2 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment three is prepared amplifies 10000 times；From figure
In it can be seen that zinc oxide in nanometer rods be sheet, length be 1.5 ~ 2 μm, diameter is about 300nm.
Fig. 3 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment four is prepared amplifies 10000 times；From figure
In it can be seen that the limb of zinc oxide nano popped rice becomes more fine uniform, but not dense enough, nanometer rods are needle-shaped, and length is
1.5 ~ 2 μm, diameter is about 200nm.
Fig. 4 is the stereoscan photograph that the zinc oxide nano popped rice that specific embodiment one is prepared amplifies 10000 times；From figure
In it can be seen that the limb fine uniform of nano flower, aligned orderly, and denser, nanometer rods are needle-shaped, length is 3 μm,
Diameter is about 100nm.
Fig. 5 is the diffracting spectrum of synthesizing zinc oxide nanometer floral material, and peak value therein corresponds to the spy of zinc oxide nano popped rice
Peak is levied, the substance for thus proving synthesis is zinc oxide nano popped rice.
Experiment two：Zinc oxide nano popped rice/ITO is tested as the detection of working electrode, and concrete operations are as follows：
Using zinc oxide nano popped rice together with ITO electro-conductive glass as working electrode, effective material area is 0.7cm2, silver/
Silver chlorate is used as to electrode, is tested using traditional three-electrode system by pulse voltammetry as reference electrode, platinum filament, and current potential increases
Add 50mV, pulse height 4mV, sweep speed 8mV/s, so as to obtain corresponding electric current of the material to various concentration levodopa
Value；The zinc oxide nano popped rice is prepared by experiment one.
It is detected using traditional three-electrode system by pulse voltammetry test, obtains levodopa concentration and current line
Property fitting figure, Fig. 6 is the Linear Fit Chart for testing two obtained levodopas and electric current, by Fig. 6 test concentration model
In enclosing, levodopa concentration variation and the linear relationship straight line of electric current, scope of the levodopa concentration at 0 ~ 40 μM can be obtained
When interior, the ITO electrode of zinc-oxide nano floral material modification is 0.1 μ A μM to the sensitivity of levodopa-1。
Claims (1)
- A kind of 1. preparation method of zinc oxide nano popped rice/ITO electrode, it is characterised in that the preparation of zinc oxide nano popped rice/ITO electrode Method carries out according to the following steps：First, hydrothermal synthesis method1）By the use of distilled water as the solvent zinc nitrate solution that compound concentration is 0.03mol/L~0.07mol/L respectively, 0.03mol/ The hexa solution of L~0.07mol/L, the ammonia spirit of 0mol/L~0.07mol/L and 0mmol/L~7mmol/L Polyetherimide solution, and by four kinds of solution after mixing with the rotating speed magnetic agitation of 450r/min~550r/min 3min~5min obtains hydro-thermal reaction solution；2）Obtained hydro-thermal reaction solution is poured into reaction kettle, covers reaction kettle lid, in 90 DEG C~120 DEG C of temperature strip 12h is reacted under part, then takes out cooled to room temperature in air, obtains zinc oxide nano popped rice, opens reaction kettle distillation Water is clean by material clean, and the zinc oxide nano popped rice after filtering is transferred in culture dish, be put into drying box 70 DEG C~ Zinc oxide nano popped rice is obtained when drying 1 ~ 3 is small at 90 DEG C；2nd, automatic spraying process1）The deionized water of the zinc oxide nano popped rice of 0.01g ~ 0.03g and 20mL is mixed to get zinc oxide suspension；2）After ITO electro-conductive glass is cleaned by ultrasonic 20min in acetone soln, ethanol solution and deionized water respectively, at room temperature Natural cooling is dried, and six pieces of ITO electro-conductive glass are fixed in spraying equipment heating plate, with adhesive tape by ITO electro-conductive glass The covering of electrode wires one side is pressed from both sides, ensures that electrode wires are contacted directly with ITO electro-conductive glass；3）Finely dispersed burnett's solution is prepared into zinc oxide nano popped rice/ITO electrode in spray gun using automatic spraying process, it is whole A spraying process carries out under 10psi air inlet pressures, and the distance of nozzle to ITO electro-conductive glass is 15cm, and heating dish temperature is 160 DEG C, burnett's solution is stirred continuously with mini-sized blender in spraying process；4）The ITO electrode for being coated with zinc oxide nano popped rice is placed in quartz tube furnace, under air, with 10 DEG C of min-1Liter Warm speed keeps the temperature 1h, then furnace cooling to room temperature to 450 DEG C；5）The 0.1%Nafion solution of the μ L of 5 μ L~20 is added dropwise on ITO electro-conductive glass after the cooling period, finally obtains zinc-oxide nano Flower/ITO electrode.
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| CN107315045A (en) * | 2017-07-05 | 2017-11-03 | 哈尔滨理工大学 | The preparation and application of a kind of graphene/zinc oxide nano popped rice/ITO electrode |
| CN109239154B (en) * | 2018-08-23 | 2020-11-06 | 哈尔滨理工大学 | Preparation and application of zinc oxide nano-flower-graphene composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776639A (en) * | 2010-01-15 | 2010-07-14 | 长春理工大学 | ZnO nanowire biosensor and preparation method thereof |
| CN104445363A (en) * | 2013-09-14 | 2015-03-25 | 金秀华 | Preparation method for nano-zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101776639A (en) * | 2010-01-15 | 2010-07-14 | 长春理工大学 | ZnO nanowire biosensor and preparation method thereof |
| CN104445363A (en) * | 2013-09-14 | 2015-03-25 | 金秀华 | Preparation method for nano-zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| ZnO Nanowire Arrays on 3D Hierachical Graphene Foam: Biomarker Detection of Parkinson"s Disease;Hong Yan Yue等;《ACS NANO》;20140109;第8卷(第2期);摘要 * |
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