CN110231378A - A kind of preparation method of super-hydrophobic gold electrode - Google Patents

A kind of preparation method of super-hydrophobic gold electrode Download PDF

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CN110231378A
CN110231378A CN201910431737.1A CN201910431737A CN110231378A CN 110231378 A CN110231378 A CN 110231378A CN 201910431737 A CN201910431737 A CN 201910431737A CN 110231378 A CN110231378 A CN 110231378A
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electrode
solution
concentration
super
electro
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潘宏程
李向葵
陈雯
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Guilin University of Technology
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Guilin University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02—Investigating surface tension of liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02—Investigating surface tension of liquids
    • G01N2013/0208—Investigating surface tension of liquids by measuring contact angle

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  • Life Sciences & Earth Sciences (AREA)
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  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention discloses a kind of preparation methods of super-hydrophobic gold electrode.Its method and step: first with cyclic voltammetry by PbS/PbSe complex deposits in ITO electrode, electrode is then placed in HAuCl4Solution in, in 40 DEG C of thermostat water baths react 3h after can be obtained surface have superhydrophobic characteristic gold electrode.The method of the present invention preparation process is simple, high-efficient, at low cost, mass production may be implemented, and the fitting in obtained gold electrode has nano-scale, has broad application prospects in field of bioanalysis.

Description

A kind of preparation method of super-hydrophobic gold electrode
Technical field
The invention belongs to nano film material field and electrochemical field, in particular to a kind of preparation of super-hydrophobic gold electrode Method.
Background technique
" super-hydrophobic " is one kind of the special wettability of material surface, and wettability is the core of many bioprocess and industrial technology The heart.Super hydrophobic surface and water drop contact area are small, are able to achieve enrichment and concentration to water droplet, thus super hydrophobic surface can be applied In every field such as automatically cleaning, anticorrosions.
Gold electrode has good bioaffinity and photoelectric respone, is often applied to immunochromatography, gene diagnosis, life The every field concerning human health such as object sensing.However, gold electrode usually has hydrophily, this allows sample drop wet Moisten entire material surface, but sample drop cannot be made to condense, which greatly limits the detection sensitivities of bioanalysis.
Super-hydrophobic gold electrode not only remains the advantages of gold nano-material, moreover it is possible to reduce connecing for sample drop and material surface Contacting surface product, sample drop can be focused on after evaporation in the region of super-hydrophobic gold surface very little, to reach enrichment, concentration sample The effect of product drop can improve the sensitivity of analysis detection efficiently against the limit of diffusion.Therefore, super-hydrophobic gold electrode exists It is had broad application prospects in field of bioanalysis.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of super-hydrophobic gold electrode.
Specific steps are as follows:
(1) the ITO electro-conductive glass cut out in advance is clear with analysis pure acetone, analysis straight alcohol and each ultrasound of secondary water respectively 3min is washed, is placed in 50 DEG C of baking ovens and dries, measures conducting surface with universal meter, it is spare.
(2) Pb (NO that 1mL concentration is 0.2mol/L is successively measured3)2Solution, the EDTA that 1mL concentration is 0.2mol/L are molten Liquid, 1.71mL concentration are the Na of 0.3mol/L2S2O3Solution, the dust technology that 1mL mass fraction is 3%, 1.71mL concentration are The SeO of 0.01mol/L2The Na that solution and 4mL concentration are 1.25mol/L2SO4Solution is placed in 20mL beaker and uniformly mixes, and is formed Orange-yellow electroplating solution.
(3) when being electroplated, electroplating solution obtained in step (2) is placed in 30 DEG C of water-baths, and is built in electroplating solution Vertical three-electrode system, wherein working electrode is electro-conductive glass obtained in step (1), is Pt electrode, Ag/AgCl electricity to electrode Extremely reference electrode carries out electro-deposition with cyclic voltammetry, and electric potential scanning range is -1V~0V, scanning speed 0.05V/s, Scanning number of segment is 60 sections, after electro-deposition, and electrode is taken out and is rinsed well with secondary water, be can be obtained after air drying black Grey PbS/PbSe-ITO electrode.
(4) HAuCl that 100 μ L mass fractions are 1% is successively measured4, it is 5.8 that 300 μ L concentration, which are 0.2mol/L, pH, HAc-NaAc buffer solution, 80 μ L concentration are the hexadecyltrimethylammonium chloride solution and 5mL secondary water of 0.2mol/L, mixing Growth-promoting media is made, after grey black PbS/PbSe-ITO electrode incline obtained in step (3) is put into growth-promoting media, in 40 DEG C of water-baths Isothermal reaction 3h in pot, the i.e. meeting autonomous growth of gold nanoparticle take out electrode after grey black electrode surface, 3h, are rushed with secondary water Wash clean is simultaneously dried, and the super-hydrophobic gold electrode that surface is sepia can be obtained.
ITO electro-conductive glass in the step (1) is the glass electrode of doped indium tin oxide.
The advantages of the method for the present invention, is as follows:
(1) super-hydrophobic gold electrode preparation process made from the method for the present invention is simple, and high-efficient, raw material is cheap and easy to get, is not necessarily to The surface modification of the organic matters such as chain alkyl mercaptan, it is more environmentally friendly.
(2) fitting in super-hydrophobic gold electrode made from the method for the present invention has the size of Nano grade, and surface area is big, can More Adsorption for Biomolecules reduces the dosage of biological reagent.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph (SEM) of the super-hydrophobic gold electrode surfaces of preparation of the embodiment of the present invention.
Fig. 2 is the contact angle schematic diagram in the super-hydrophobic gold electrode face of preparation of the embodiment of the present invention.
Specific embodiment
Embodiment
The present embodiment is used to illustrate the preparation method and its morphology analysis of the super-hydrophobic gold electrode of the present invention.
(1) by the ITO electro-conductive glass of the 1cm × 3cm cut out in advance respectively with analysis pure acetone, analysis straight alcohol and secondary Water is respectively cleaned by ultrasonic 3min, is placed in 50 DEG C of baking ovens and dries, and measures conducting surface with universal meter, spare.
(2) Pb (NO that 1mL concentration is 0.2mol/L is successively measured3)2Solution, the EDTA that 1mL concentration is 0.2mol/L are molten Liquid, 1.71mL concentration are the Na of 0.3mol/L2S2O3Solution, the dust technology that 1mL mass fraction is 3%, 1.71mL concentration are The SeO of 0.01mol/L2The Na that solution and 4mL concentration are 1.25mol/L2SO4Solution is placed in 20mL beaker and uniformly mixes, and is formed The electroplating solution of orange-yellow electro-deposition PbS/PbSe.
(3) when being electroplated, electroplating solution obtained in step (2) is placed in 30 DEG C of water-baths, and is built in electroplating solution Vertical three-electrode system, wherein working electrode is electro-conductive glass obtained in step (1), is Pt electrode, Ag/AgCl electricity to electrode Extremely reference electrode carries out electro-deposition with cyclic voltammetry, and electric potential scanning range is -1V~0V, scanning speed 0.05V/s, Scanning number of segment is 60 sections.After electro-deposition, electrode is taken out and is rinsed well with secondary water, can be obtained after air drying black Grey PbS/PbSe-ITO electrode.
(4) HAuCl that 100 μ L mass fractions are 1% is successively measured4, it is 5.8 that 300 μ L concentration, which are 0.2mol/L, pH, HAc-NaAc buffer solution, 80 μ L concentration are the hexadecyltrimethylammonium chloride solution and 5mL secondary water of 0.2mol/L, mixing Growth-promoting media is made, after grey black PbS/PbSe-ITO electrode incline obtained in step (3) is put into growth-promoting media, in 40 DEG C of water-baths Isothermal reaction 3h in pot, the i.e. meeting autonomous growth of gold nanoparticle take out electrode after black gray expandable electrode surface, 3h, are rushed with secondary water Wash clean is simultaneously dried, and the super-hydrophobic gold electrode that surface is sepia can be obtained.
ITO electro-conductive glass in the step (1) is the glass electrode of doped indium tin oxide.
By scanning electron microscope (SEM), the micromorphology of super-hydrophobic gold electrode prepared by the present invention is had studied, from figure As can be seen that super-hydrophobic gold electrode has micro-nano diadactic structure in 1, wherein Au nanoparticle is in almost spherical or elliposoidal
It is tested by contact angle (CA), has studied the surface moist of super-hydrophobic gold electrode prepared by the present invention.It can from Fig. 2 To find out, super-hydrophobic gold electrode surfaces contact angle CA is 150.5 °, is super-hydrophobic.
In conclusion super-hydrophobic gold electrode preparation process is easy, high-efficient, which has micro-nano diadactic structure, electrode Middle Au has nano-scale, and contact angle is 150.5 °, it is shown that ideal super-hydrophobicity.It is believed that super-hydrophobic gold electrode bioanalysis Field can have broad application prospects.

Claims (2)

1. a kind of preparation method of super-hydrophobic gold electrode, it is characterised in that specific steps are as follows:
(1) the ITO electro-conductive glass cut out in advance is respectively cleaned by ultrasonic with analysis pure acetone, analysis straight alcohol and secondary water respectively 3min is placed in 50 DEG C of baking ovens and dries, for use；
(2) Pb (NO that 1mL concentration is 0.2mol/L is successively measured3)2Solution, the EDTA solution that 1mL concentration is 0.2mol/L, 1.71mL concentration is the Na of 0.3mol/L2S2O3Solution, the dust technology that 1mL mass fraction is 3%, 1.71mL concentration are The SeO of 0.01mol/L2The Na that solution and 4mL concentration are 1.25mol/L2SO4Solution is placed in 20mL beaker and uniformly mixes, and is formed Orange-yellow electroplating solution；
(3) when being electroplated, electroplating solution obtained in step (2) is placed in 30 DEG C of water-baths, and three are established in electroplating solution Electrode system, wherein working electrode is electro-conductive glass obtained in step (1), is Pt electrode to electrode, and Ag/AgCl electrode is Reference electrode carries out electro-deposition with cyclic voltammetry, and electric potential scanning range is -1V~0V, scanning speed 0.05V/s, scanning Number of segment is 60 sections, after electro-deposition, and electrode is taken out and is rinsed well with secondary water, and black gray expandable can be obtained after air drying PbS/PbSe-ITO electrode；
(4) HAuCl that 100 μ L mass fractions are 1% is successively measured4, 300 μ L concentration are the HAc- that 0.2mol/L, pH are 5.8 NaAc buffer solution, 80 μ L concentration are the hexadecyltrimethylammonium chloride solution and 5mL secondary water of 0.2mol/L, are mixed to prepare Growth-promoting media, after grey black PbS/PbSe-ITO electrode incline obtained in step (3) is put into growth-promoting media, in 40 DEG C of water-baths Isothermal reaction 3h, the i.e. meeting autonomous growth of gold nanoparticle take out electrode behind grey black surface, 3h, are rinsed well simultaneously with secondary water The super-hydrophobic gold electrode that surface is sepia can be obtained in drying.
2. preparation method according to claim 1, it is characterised in that the ITO electro-conductive glass in the step (1) is doping The glass electrode of tin indium oxide.
CN201910431737.1A 2019-05-23 2019-05-23 A kind of preparation method of super-hydrophobic gold electrode Pending CN110231378A (en)

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Publication number Priority date Publication date Assignee Title
CN101255603A (en) * 2007-12-06 2008-09-03 上海大学 Method for preparing II-VI family semiconductor nano-wire by template electric-sedimentation
CN102331448A (en) * 2011-10-14 2012-01-25 北京工业大学 Method for preparing electrochemical luminescence electrode by directly electrodepositing CdS modified glassy carbon
CN102352494A (en) * 2011-09-30 2012-02-15 厦门大学 Preparation method of CdSe/CdS quantum dot sensitized TiO2 nanometer tube composite film
EP2674759B1 (en) * 2011-02-04 2016-01-06 Council of Scientific & Industrial Research Molecularly imprinted conducting polymer film based aqueous amino acid sensors
CN105499596A (en) * 2015-12-06 2016-04-20 桂林理工大学 Method for spontaneously growing Au nanometer particles on electro-deposited CdSe film
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CN106335873A (en) * 2016-10-26 2017-01-18 桂林理工大学 Method for preparing Pb3(PO4)2 nanowire film
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Patent Citations (8)

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Publication number Priority date Publication date Assignee Title
CN101255603A (en) * 2007-12-06 2008-09-03 上海大学 Method for preparing II-VI family semiconductor nano-wire by template electric-sedimentation
EP2674759B1 (en) * 2011-02-04 2016-01-06 Council of Scientific & Industrial Research Molecularly imprinted conducting polymer film based aqueous amino acid sensors
CN102352494A (en) * 2011-09-30 2012-02-15 厦门大学 Preparation method of CdSe/CdS quantum dot sensitized TiO2 nanometer tube composite film
CN102331448A (en) * 2011-10-14 2012-01-25 北京工业大学 Method for preparing electrochemical luminescence electrode by directly electrodepositing CdS modified glassy carbon
CN105499596A (en) * 2015-12-06 2016-04-20 桂林理工大学 Method for spontaneously growing Au nanometer particles on electro-deposited CdSe film
CN106044706A (en) * 2016-08-16 2016-10-26 曹健 CdSe/CdS nanoparticle co-sensitized ZnO photoelectrode preparation method
CN106335873A (en) * 2016-10-26 2017-01-18 桂林理工大学 Method for preparing Pb3(PO4)2 nanowire film
CN108715439A (en) * 2018-05-23 2018-10-30 中国科学技术大学先进技术研究院 A kind of cadmium base chalcogenide nanometer rods and preparation method, elctro-catalyst and application

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