CN101493433B - Gold plated ZnO nano-bar array electrode and method for making same - Google Patents
Gold plated ZnO nano-bar array electrode and method for making same Download PDFInfo
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- CN101493433B CN101493433B CN2009100965032A CN200910096503A CN101493433B CN 101493433 B CN101493433 B CN 101493433B CN 2009100965032 A CN2009100965032 A CN 2009100965032A CN 200910096503 A CN200910096503 A CN 200910096503A CN 101493433 B CN101493433 B CN 101493433B
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Abstract
The invention discloses a gold-plated ZnO nanorod array electrode and a method for manufacturing the electrode. The gold-plated ZnO nanorod array electrode is plated with a gold layer on a surface with a ZnO nanorod, changes the conductivity of the gold-plated ZnO nanorod array electrode by the gold-plated layer, and causes the original ZnO nanorod array electrode to be conductive from non-conductive; by using the gold-plated ZnO nanorod array electrode for doing test, the sensitivity is very high. As the gold layer has stable chemical property, high temperature resistance, corrosion resistance, oxidation resistance, and low resistivity, better protective action can be obtained when the gold layer is coated outside the ZnO nanorod, the service life of the gold-plated ZnO nanorod array electrode can be greatly prolonged, and the structural property of one-dimensional nano-materials is preserved.
Description
Technical field
The present invention relates to be used for a kind of gold plated ZnO nano-bar array electrode of electrochemical field, relate in particular to the structure and the preparation method of this gold plated ZnO nano-bar array electrode.
Background technology
Nano-electrode have high mass transfer rate, low iR fall, hour between good characteristic such as constant, obtain more and more widely research and application.The electrochemical properties of nano-array electrode is not only relevant with the unipolar character of nanometer, but also has some characteristics of self, as obtaining the strength of current much bigger than the nanometer single electrode, has much higher signal to noise ratio (S/N ratio) of the conventional electrodes of more identical geometric area etc.These characteristics make nano-array electrode in preparation and application, more can satisfy actual requirement, and its research is become one of most active forward position, current electrochemical research field gradually.
For the monodimension nanometer material as electrochemical electrode, being grown in suprabasil electrod-array is that actual fabrication and application bring more facility.The masterplate method is adopted in the preparation work of this respect more, comprises based on the die version of alumina nanohole and the soft template method of some organic porous films.ZnO has the one-dimensional nano structure of various ways.Wherein, the ZnO nanometer stick array of high orientation is an important research focus.People utilize the unique property of this structured material, have realized the preparation of nano laser, the realization of an emission function, the test of piezoelectric property device and sensor etc.
In the preparation process of ZnO nanometer stick array, hydro-thermal method has remarkable advantages.Remove mild condition simply outside, the structure of its array and pattern can be at an easy rate be controlled through the parameter that changes in the preparation process, such as the concentration of pre-service, growth temperature, sedimentation time and the precursor of substrate etc.In the application process of reality, generally all be that deposition layer of ZnO nano thin-film can obtain the nano wire or the nanorod structure of oriented growth on this basis as Seed Layer in substrate.The ZnO nanometer stick array is a semiconductor material under regular situation, does not have electric conductivity, and originally dissolving and corrosion phenomenon is arranged in the WS, therefore is difficult to use as electrochemical electrode.
Summary of the invention
The technical matters that the present invention will solve provides a kind of gold plated ZnO nano-bar array electrode, and its ZnO nanometer rods has conductive capability, constitutes 1-dimention nano pole and can be used in electro-chemical test, and higher sensitivity is provided for electro-chemical test.
Another technical matters that will solve of the present invention provides a kind of method for preparing this gold plated ZnO nano-bar array electrode, can prepare the ZnO nanometer rods with conductive capability through this method.
For solving the problems of the technologies described above; The present invention adopts following technical scheme: this gold plated ZnO nano-bar array electrode; Which comprises at least silicon base, silica dioxide medium layer, ZnO Seed Layer and ZnO nanometer stick array layer, said silica dioxide medium layer is positioned on the silicon base, and said ZnO Seed Layer is positioned on the silica dioxide medium layer; Said ZnO nanometer stick array layer is positioned on the ZnO Seed Layer, and each ZnO nanorod surfaces of said ZnO nanometer stick array layer and ZnO Seed Layer surface are coated with the gold layer.The gold layer has good adhesion, corrosion resistivity and inoxidizability, therefore makes the ZnO nanometer rods obtain best protection, can prolong the serviceable life of gold plated ZnO nano-bar array electrode greatly.
As of the present invention preferred, said golden layer thickness is at least 100nm.Golden layer thickness like this can effectively reduce resistance, helps improving the test performance of gold plated ZnO nano-bar array electrode.
The method for preparing this gold plated ZnO nano-bar array electrode; Put into high temperature furnace after at first silicon chip being cleaned and carry out oxidation; Forming nano-ZnO thin film with sol-gel process in the silica surface deposition behind the silica dioxide medium layer to be generated is the ZnO Seed Layer; Immerse again in the equal-volume mixed solution of zinc nitrate and hexamethylene tetramine of same concentrations; Take out after the time response with 90-100 degree centigrade temperature and 1-3 hour in airtight reaction utensil and fully clean, dry up then and obtain gold plated ZnO nano-bar array electrode with deionized water, again through magnetically controlled sputter method at the direct deposited gold layer of the electrode surface that deposits the ZnO nanometer stick array.
As of the present invention preferred, said ZnO Seed Layer immerses in the mixed solution of zinc nitrate and hexamethylene tetramine through behind the UV-irradiation again.Because ZnO Seed Layer surface is not hydrophilic, so mixed solution can skewness on the ZnO Seed Layer.Through can make behind the UV-irradiation ZnO Seed Layer surface wettability by hydrophobic to hydrophilic transformation, the mixed solution on the ZnO Seed Layer is evenly distributed.As of the present invention preferred, said UV-irradiation process by the 8W UV-lamp apart from the ZnO Seed Layer at the most the scope internal radiation of 5cm accomplish after one hour.
The present invention adopts technique scheme: gold plated ZnO nano-bar array electrode is coated with the gold layer in the one side that the ZnO nanometer rods is arranged; Change the electric conductivity of gold plated ZnO nano-bar array electrode through Gold plated Layer; Original ZnO nano-bar array electrode is changed by non-conductive conductive, use this gold plated ZnO nano-bar array electrode to do test and have very high sensitivity.Because golden stratification stable in properties, high temperature resistant, corrosion-resistant, anti-oxidant, low resistance; Being wrapped in ZnO nanometer rods outside with it just can well play a protective role; Can prolong the serviceable life of gold plated ZnO nano-bar array electrode greatly, keep the architectural characteristic of monodimension nanometer material simultaneously.
Description of drawings
Below in conjunction with accompanying drawing and embodiment invention is done further and to be specified.
Fig. 1 is the structural representation of gold plated ZnO nano-bar array electrode of the present invention;
Fig. 2 is applied to detect the cyclic voltammetry curve figure of hydrogen peroxide for gold plated ZnO nano-bar array electrode of the present invention;
Fig. 3 is applied to detect the standard working curve of hydrogen peroxide for gold plated ZnO nano-bar array electrode of the present invention;
Fig. 4 is the field emission scanning electron microscope figure SEM and the ability spectrogram EDS of gold plated ZnO nano-bar array electrode of the present invention.
Embodiment
Like Fig. 1, shown in 4, the structure of this gold plated ZnO nano-bar array electrode is followed successively by silicon base 1, silica dioxide medium layer 2, ZnO Seed Layer 3 and ZnO nanometer stick array layer from the bottom up.Silica dioxide medium layer 2 is positioned on the silicon base 1, and ZnO Seed Layer 3 is positioned on the silica dioxide medium layer 2, and ZnO nanometer stick array layer is positioned on the ZnO Seed Layer 3.On each ZnO nanometer rods 4 surface of ZnO nanometer stick array layer and the surface of ZnO Seed Layer 3 be coated with one deck gold layer 5 of same thickness, its thickness is 150nm.
The preparation method of this gold plated ZnO nano-bar array electrode mainly comprises two steps, and the at first preparation of ZnO nanometer rods 4 arrays is that ZnO nanometer rods 4 arrays are gold-plated at last.Detailed process is following; P type or the n type monocrystalline silicon piece substrate as electrode is selected in the preparation of first step ZnO Seed Layer 3 for use, this silicon chip is put into high temperature furnace carry out thermal oxide after cleaning; Through thermal oxide under 1140 ℃ of temperature 40 minutes, substrate surface generated the thick silicon dioxide layer of 50nm.Adopting sol-gel process is ZnO Seed Layer 3 at silica surface depositing nano ZnO film.The preparation of second step ZnO nanometer rods 4 arrays, at first the ZnO Seed Layer on the 8W ultra violet lamp substrate is 3 one hours, and distance is controlled at 5cm.The above-mentioned substrate that deposits ZnO film is immersed in the equal-volume mixed liquor of zinc nitrate and hexamethylene tetramine of same concentrations, make its final concentration be respectively 0.02mol/L.The substrate surface of intending deposition ZnO nanometer rods 4 arrays is placed on downwards in the airtight reaction utensil, carries out 2 hours under 95 ℃.Reaction finishes the back deionized water fully cleans, and dries up subsequent use with nitrogen.The 3rd step Gold plated Layer 5 is at the direct magnetically controlled sputter method deposition of the electrode surface that deposits ZnO nanometer rods 4 arrays 150nm gold layer 5.
Gold plated ZnO nano-bar array electrode has the electric conductivity that is superior to original ZnO nano-bar array electrode, uses this gold plated ZnO nano-bar array electrode to do test and has very high sensitivity.For example gold plated ZnO nano-bar array electrode is used to test hydrogen peroxide; Electro-chemical test carries out in standard three-electrode cell system; Gold plated ZnO nano-bar array electrode is a working electrode, and saturated calomel electrode (SCE) is a contrast electrode, and the Pt plate electrode is to electrode.Adopt existing electrochemical workstation to test.
Respectively at PBS and contain the cyclic voltammetry scan that carries out gold plated ZnO nano-bar array electrode in the PBS solution of 70 * 10-6M hydrogen peroxide, voltage range is from-0.7V to 0.7V (with respect to SCE), sweep velocity 0.1Vs-1.The result is as shown in Figure 2.
The result shows, in superoxol, negative electrode and anode electrode current value are compared among the PBS obviously to be increased, and explains that redox reaction takes place on electrode hydrogen peroxide, and electric current goes out the peak position respectively about-0.4V and 0.2V.The increase of cathode current is more remarkable, shows that reduction reaction carries out quicker
As shown in Figure 3, gold plated ZnO nano-bar array electrode is to add the response diagram of 2.2 * 10-6M hydrogen peroxide continuously in the test fluid.Visible by Fig. 4, add sample liquid at every turn and can cause that all response current significantly increases, show electrode is to the good response of variable concentrations hydrogen peroxide.
Above said be specific embodiment of the present invention and the know-why used; If comply with the change that conception of the present invention is done; Like inert metal with other; Also be the change of doing according to conception of the present invention, when the function that it produced does not exceed spiritual that instructions and accompanying drawing contain yet, must belong to protection scope of the present invention.
Claims (5)
1. gold plated ZnO nano-bar array electrode; Which comprises at least silicon base (1), silica dioxide medium layer (2), ZnO Seed Layer (3) and ZnO nanometer stick array layer; Said silica dioxide medium layer (2) is positioned on the silicon base (1); Said ZnO Seed Layer (3) is positioned on the silica dioxide medium layer (2), and said ZnO nanometer stick array layer is positioned on the ZnO Seed Layer (3), it is characterized in that: each ZnO nanometer rods (4) surface and ZnO Seed Layer (3) surface of said ZnO nanometer stick array layer are coated with gold layer (5).
2. according to the said gold plated ZnO nano-bar array electrode of claim 1, it is characterized in that: said gold layer (5) thickness is at least 100nm.
3. method for preparing the said gold plated ZnO nano-bar array electrode of claim 1; It is characterized in that: put into high temperature furnace after at first silicon chip being cleaned and carry out oxidation; It is ZnO Seed Layer (3) that silica dioxide medium layer to be generated (2) back forms nano-ZnO thin film with sol-gel process in the silica surface deposition; Immerse again in the equal-volume mixed solution of zinc nitrate and hexamethylene tetramine of same concentrations; Make its final concentration be respectively 0.02mol/L; Take out after the time response with 90-100 degree centigrade temperature and 1-3 hour in airtight reaction utensil and fully clean, dry up then and obtain gold plated ZnO nano-bar array electrode with deionized water, again through magnetically controlled sputter method at the direct deposited gold layer of electrode surface (5) that deposits ZnO nanometer rods (4) array.
4. according to the said method for preparing gold plated ZnO nano-bar array electrode of claim 3, it is characterized in that: said ZnO Seed Layer (3) immerses in the mixed solution of zinc nitrate and hexamethylene tetramine through behind the UV-irradiation again.
5. according to the said method for preparing gold plated ZnO nano-bar array electrode of claim 4, it is characterized in that: said UV-irradiation process by the 8W UV-lamp apart from ZnO Seed Layer (3) at the most the scope internal radiation of 5cm accomplish after one hour.
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| CN102477291B (en) * | 2010-11-23 | 2014-05-21 | 海洋王照明科技股份有限公司 | Preparation method of ZnO nano-rod array |
| CN102156117B (en) * | 2011-03-22 | 2013-04-10 | 中国科学院长春应用化学研究所 | Substrate for surface enhanced Raman scattering and preparation method thereof |
| CN103614711B (en) * | 2013-12-02 | 2015-07-29 | 陕西科技大学 | A kind of method in metal or metal alloy surface grown on larger scale ZnO nano array |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200512451A (en) * | 2003-09-30 | 2005-04-01 | Hon Hai Prec Ind Co Ltd | Gas sensor of zinc oxide |
| CN1674230A (en) * | 2004-03-26 | 2005-09-28 | 北京大学 | Silicon substrate nano-zinc oxide and producing method and application thereof |
| WO2007114649A1 (en) * | 2006-04-04 | 2007-10-11 | Seoul National University Industry Foundation | Biosensor having nano wire and manufacturing method thereof |
| CN101250735A (en) * | 2008-04-09 | 2008-08-27 | 天津大学 | Apparatus and method for continuously composite plating metallic and nano particle on carbon fiber surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200512451A (en) * | 2003-09-30 | 2005-04-01 | Hon Hai Prec Ind Co Ltd | Gas sensor of zinc oxide |
| CN1674230A (en) * | 2004-03-26 | 2005-09-28 | 北京大学 | Silicon substrate nano-zinc oxide and producing method and application thereof |
| WO2007114649A1 (en) * | 2006-04-04 | 2007-10-11 | Seoul National University Industry Foundation | Biosensor having nano wire and manufacturing method thereof |
| CN101250735A (en) * | 2008-04-09 | 2008-08-27 | 天津大学 | Apparatus and method for continuously composite plating metallic and nano particle on carbon fiber surface |
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