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