CN1356543A - Process for preparing film electrode of gold-monocrystal nano island array - Google Patents
Process for preparing film electrode of gold-monocrystal nano island array Download PDFInfo
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- CN1356543A CN1356543A CN 01140468 CN01140468A CN1356543A CN 1356543 A CN1356543 A CN 1356543A CN 01140468 CN01140468 CN 01140468 CN 01140468 A CN01140468 A CN 01140468A CN 1356543 A CN1356543 A CN 1356543A
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- plating liquid
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- oxyammonia
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Abstract
A process for preparing gold (III) monocrystal nano island array film and electrode uses the saturated self-assembled single-layer film of 2.5nm gold particles on the glass modified by aminopropyltrimethoxyl silicon or the electrically conducting indium tin oxide glass as catalytic template and the chloraurin acid/oxyammonia as gold-plating liquid and features that the raction time is controlled at constant temp to control the orientating growth of island-shaped gold film in nano range. Its advantages include simple operation and good repeatability.
Description
Technical field: the preparation method who the invention belongs to film electrode of gold-monocrystal nano island array.Concrete is the wet chemical preparation method of Au (111) monocrystal nano island array film and electrode thereof.
Background technology: on the nanoscale level, metallic film (comprising metallic island films) is carried out thickness and the controlled preparation of pattern is significant.This metalloid film is owing to having the extensive concern that unique regulatable optical property and many potential application prospects obtain people.For example, present promising Surface enhanced raman spectroscopy (SERS) and surface plasma body resonant vibration (SPR) spectral technique all require gold or money base basal surface to have the roughness of nanoscale.In Surface enhanced raman spectroscopy, molecule adsorbs on the island film of gold, silver with suitable surfaceness and copper can make raman scattering spectrum obtain up to a million times enhancing.Studies show that the roughness of submicroscopic surfaceness (particle size is at 5-20nm) and atomic scale is the requirement that obtains the Surface enhanced raman spectroscopy response.Although there are many methods to be used to prepare SERS response substrate, prepare favorable reproducibility, stablize and in the 3-100nm scope, have SERS substrate still very difficult (Freeman, the R.G. of even roughness degree; Natan, M.J.et al.Science, 1995,267,1629-1632.).In addition, in galvanochemistry, the electrochemical behavior of molecule is not only relevant with the orderly atomic arrangement mode of electrode surface, and with the size of electrode confidential relation is arranged.Just because of this, nano-electrode and array integral body thereof receive very big concern.Theoretical this class electrode of prophesy can be studied ultrafast electron transfer reaction and have some unusual electrochemical phenomenas.Yet, owing to make real nano-electrode and array integral body quite difficult (Menon, V.P.; Martin, C.R.Anal.Chem.1995,67,1920-1928.), make in this field, to test at present to lag behind theory.
Summary of the invention: the preparation method who the purpose of this invention is to provide a kind of film electrode of gold-monocrystal nano island array.This method is at first based on the saturated self assembly of golden nanometer particle on TSL 8330 (APTMS) modification slide or tin indium oxide (ITO) electro-conductive glass, be catalytic templating with this golden nanometer particle monofilm then, static electroless plating technology by surface limited obtains to have nano particle self-assembled monolayer template ordered structure Au (111) monocrystal nano island array film and electrode feature, (111) oriented growth at the oriented growth of nanoscale scope inner control Jin Dao.This legal system is equipped with Au (111) monocrystal nano island array membrane electrode, and not only cost is low, simple to operate, and the electrode that makes has the global feature electrochemical behavior of Au (111) nano-electrode array, is expected to be applied in galvanochemistry.
Select for use particle diameter to be about the golden nanometer particle of 2.5nm among the present invention as the nucleation site, on the slide of TSL 8330 (APTMS) modified or tin indium oxide (ITO) electro-conductive glass, form the individual layer film of nanoparticles of the saturated assembling of one deck, with this preparation template as gold nano island array film and electrode by self assembly.HAuCl under the control surface constrained state
4/ NH
2The concentration of OH chemical gold plating liquid and static plated film time, can obtain the nano island array film and the electrode of Au (111) oriented growth in the size on nanoscale scope inner control nm of gold island under room temperature.
The present invention will approach microslide earlier through the chromic acid lotion soaked overnight, and be 3: 1 dense H in volume ratio
2SO
4/ 30%H
2O
2After soaking 10-30min under 70 ℃ in the mixed solution, clean with deionized water and spectroscopic pure methanol rinse, immerse then and carry out the processing of slide silanization in the 4-8ml methanol solution that contains 0.4-0.8ml TSL 8330 (APTMS).After treating 12-18 hour, take out the slide of silanization, use washed with methanol three times, and immersion is about in the aurosol of 2.0-3.0nm with the average particulate diameter that sodium citrate/sodium borohydride reduction prepares immediately, carries out self assembly 12-18 hour.Take out slide, promptly immerse after washing is clean in the mixing gold plating liquid of gold chloride of the oxyammonia of 4-8ml0.1-1mM and 0.05-0.15% (w/v), under the room temperature static condition, the control reaction time can obtain the nano island array film of Au (111) oriented growth at 5-10min.Atomic force microscope pattern sign, X-ray diffraction analysis and direct current resistance are measured (insulation, resistance＞10
7Ω) show that this island film definition is intact, defective is few, is Au (111) oriented growth basically, and the size on island arrives between the nanometers up to a hundred tens.The preparation of Au (111) nano island array membrane electrode is to be substrate with the ITO electro-conductive glass.Earlier the ITO electro-conductive glass is soaked 10-20min in 10% (w/v) NaOH solution, promptly immerse after washing is clean as mentioned above in the silylating reagent, other step is identical.
The film electrode of gold-monocrystal nano island array of the present invention's preparation has the ordered structure feature of nano particle self-assembled monolayer template, and defective is few, favorable reproducibility.This legal system is equipped with Au (111) monocrystal nano island array membrane electrode, and not only cost is low, simple to operate, and the electrode that makes has the global feature electrochemical behavior of Au (111) nano-electrode array, is expected to be applied in galvanochemistry.In addition, this method is owing to the ability that has in nanoscale scope inner control gold island size, and method is not subjected to the restriction of substrate shape, size etc., therefore have certain universality, be expected in SERS response substrate and some nano-array photoelectric devices, to be applied based on surperficial enhancement effect.
Embodiment:
Embodiment 1: get a slide, the dense H through chromic acid lotion and 3: 1
2SO
4/ 30%H
2O
2After mixed solution embathes, use deionized water and each rinsing of spectroscopic pure methyl alcohol three times, immerse then and carry out the processing of slide silanization in the 4ml methanol solution that contains 0.4ml APTMS.After 12 hours, take out the slide of silanization, use methanol rinse three times, and immersion is about in the aurosol of 2.0-3.0nm with the average particulate diameter that sodium citrate/sodium borohydride reduction prepares immediately, carries out self assembly 12 hours.Take out slide, after washing is clean, immerse immediately in the gold plating liquid of gold chloride of 1mM oxyammonia and 0.05% (w/v) of 8ml, under the room temperature static condition, in the 10 minutes reaction time of control, promptly obtain the island array film of particle size at 75-100nm.Atomic force microscope pattern sign, X-ray diffraction analysis and direct current resistance are measured (insulation, resistance＞10
7Ω) showing that the island membrane structure is even, defective is few, is Au (111) oriented growth basically, and poorly conductive between island and the island, is the isolating insulation state basically.
Embodiment 2: get a slide, the dense H through chromic acid lotion and 3: 1
2SO
4/ 30%H
2O
2After mixed solution embathes, use deionized water and each rinsing of spectroscopic pure methyl alcohol three times, immerse then and carry out the processing of slide silanization in the 6ml methanol solution that contains 0.6ml APTMS.After 18 hours, take out the slide of silanization, use methanol rinse three times, and immersion is about in the aurosol of 2.0～3.0nm with the average particulate diameter that sodium citrate/sodium borohydride reduction prepares immediately, carries out self assembly 18 hours.Take out slide, after washing is clean, immerse immediately in the gold plating liquid of gold chloride of 0.4mM oxyammonia and 0.1% (w/v) of 6ml, under the room temperature static condition, in the 8 minutes reaction time of control, promptly obtain the island array film of particle size at 60-80nm.Atomic force microscope pattern sign, X-ray diffraction analysis and direct current resistance are measured (insulation, resistance＞10
7Ω) showing that the island membrane structure is even, defective is few, is Au (111) oriented growth basically, and poorly conductive between island and the island, is the isolating insulation state basically.
Embodiment 3: get an ITO electro-conductive glass, after 10%NaOH solution soaks 15min, use deionized water and each rinsing of spectroscopic pure methyl alcohol three times, immerse then and carry out the processing of slide silanization in the 6ml methanol solution that contains 0.6ml APTMS.After 12 hours, take out the ITO electro-conductive glass of silanization, use methanol rinse three times, and immersion is about in the aurosol of 2.0-3.0nm with the average particulate diameter that sodium citrate/sodium borohydride reduction prepares immediately, carries out self assembly 12 hours.Take out the ITO electro-conductive glass, after washing is clean, immerse immediately in the gold plating liquid of gold chloride of 0.4mM oxyammonia and 0.1% (w/v) of 6ml, under the room temperature static condition, in the 10 minutes reaction time of control, promptly obtain the island array film of particle size at 75-100nm.Atomic force microscope pattern sign, X-ray diffraction analysis and direct current resistance are measured (insulation, resistance＞10
7Ω) showing that the island membrane structure is even, defective is few, is Au (111) oriented growth basically, and poorly conductive between island and the island, is the isolating insulation state basically.It as working electrode, is immersed the H of 0.1M
2SO
4In the aqueous solution, in-0.2-+1.6V potential range, carry out the cyclic voltammetric electrochemistry experiment, can obtain the global feature electrochemical response of Au (111) nano-electrode array with the 10mV/s sweep velocity.+ 0.99 ,+1.05 and+the 1.25V place, three typical oxides occur and form peaks, its peak current is than the little order of magnitude of conventional large electrode of identical working area.
Claims (5)
1, a kind of preparation method of gold-monocrystal nano island array film, its step is as follows:
(1) will approach microslide or tin indium oxide (ITO) electro-conductive glass soaks through chromic acid lotion;
(2) at dense H
2SO
4/ 30%H
2O
2Add heat soaking in the mixed solution;
(3) clean with deionized water and methanol rinse;
(4) immerse and to carry out the slide silanization in the methanol solution contain TSL 8330 (APTMS) and handle;
(5) take out the slide of silanization, use washed with methanol, and immerse in the aurosol for preparing with sodium citrate/sodium borohydride reduction immediately, carry out self assembly;
(6) take out slide, promptly immerse in the mixing gold plating liquid of oxyammonia and gold chloride after washing is clean, under the room temperature static condition, react;
Wherein
Described dense H
2SO
4/ 30%H
2O
2The ratio of mixed solution is 3: 1, and heating-up temperature is 70 ℃, and soak time is 10-30min;
Described methyl alcohol is spectroscopic pure;
The content of TSL 8330 (APTMS) is 0.4-0.8ml in the methanol solution that described silanization is handled; The consumption of solution is 4-8ml;
The described silanization processing time is 12-18 hour;
The average particulate diameter of gold particle is 2.0-3.0nm in the described aurosol, and the self assembly time is 12-18 hour;
The content of oxyammonia is 0.1-1mM in the described mixing gold plating liquid, and the content of gold chloride is 0.05-0.15% (w/v), and the consumption that mixes gold plating liquid is 4-8ml, and the reaction time is 5-10min.
2, the preparation method of film electrode of gold-monocrystal nano island array as claimed in claim 1, it is characterized in that, in the gold plating liquid of the gold chloride of the 1mM oxyammonia and 0.05% (w/v) of immersion 8ml, under the room temperature static condition, in the 10 minutes reaction time of control, promptly obtain the island array film of particle size at 75-100nm.
3, the preparation method of film electrode of gold-monocrystal nano island array as claimed in claim 1, it is characterized in that, in the gold plating liquid of the gold chloride of the 0.4mM oxyammonia and 0.1% (w/v) of immersion 6ml, under the room temperature static condition, in the 8 minutes reaction time of control, promptly obtain the island array film of particle size at 60-80nm.
4, a kind of preparation method of film electrode of gold-monocrystal nano island array, its step is as follows:
(1) tin indium oxide (ITO) electro-conductive glass is soaked through NaOH;
It is (2) clean with rinsed with deionized water,
(3) immerse and to carry out the slide silanization in the methanol solution contain TSL 8330 (APTMS) and handle;
(4) take out the slide of silanization, use washed with methanol, and immerse in the aurosol for preparing with sodium citrate/sodium borohydride reduction immediately, carry out self assembly;
(5) take out slide, promptly immerse in the mixing gold plating liquid of oxyammonia and gold chloride after washing is clean, under the room temperature static condition, react;
Wherein
The concentration of described NaOH solution is 10% (wv), and soak time is 10-20min;
The content of TSL 8330 (APTMS) is 0.4-0.8ml in the methanol solution that described silanization is handled; The consumption of solution is 4-8ml;
The described silanization processing time is 12-18 hour;
The average particulate diameter of gold particle is 2.0-3.0nm in the described aurosol, and the self assembly time is 12-18 hour;
The content of oxyammonia is 0.1-1mM in the described mixing gold plating liquid, and the content of gold chloride is 0.05-0.15% (w/v), and the consumption that mixes gold plating liquid is 4-8ml, and the reaction time is 5-10min.
5, the preparation method of film electrode of gold-monocrystal nano island array as claimed in claim 4, it is characterized in that, in the gold plating liquid of the gold chloride of the 0.4mM oxyammonia and 0.1% (w/v) of immersion 6ml, under the room temperature static condition, in the 10 minutes reaction time of control, promptly obtain the island array film of particle size at 75-100nm.
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