CN104931568A - Indium tin oxide electrochemiluminescence reaction electrode regeneration cleaning method - Google Patents
Indium tin oxide electrochemiluminescence reaction electrode regeneration cleaning method Download PDFInfo
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- CN104931568A CN104931568A CN201510361611.3A CN201510361611A CN104931568A CN 104931568 A CN104931568 A CN 104931568A CN 201510361611 A CN201510361611 A CN 201510361611A CN 104931568 A CN104931568 A CN 104931568A
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- hydrogen peroxide
- electrochemiluminescence
- electrode surface
- ito
- cleaning liquid
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Abstract
The invention relates to an indium tin oxide electrochemiluminescence reaction electrode regeneration cleaning method in the technical field of electrochemiluminescence biology detection and aims to enable an indium tin oxide electrochemiluminescence reaction electrode to be capable of being used repeatedly for multiple times. The technical scheme includes that that indium tin oxide electrochemiluminescence reaction electrode regeneration cleaning method includes the steps of aqueous-solution cleaning liquid soaking and cleaning, absolute ethyl alcohol soaking and cleaning, electrode surface activating treatment, drying and the like.
Description
Technical field
The present invention relates to a kind of regeneration washing method to tin indium oxide electrochemiluminescence reaction electrode in electrochemiluminescence technical field of biological.
Background technology
Chemiluminescence (electrochemiluminescence) is the luminescence phenomenon produced in chemical reaction process.Electrochemiluminescence research starts from the '30s in last century.Nineteen twenty-nine Harvey etc. find in the basic conditions electrolysis luminol time can produce luminescence phenomenon on electrode, after this correlative study is carried out successively.Last century, the appearance of the eighties pyridine ruthenium electrochemical luminescence system was the major progress of one, this field.After this electrochemiluminescence analysis technology starts effectively to be applied in immunoassay, foranalysis of nucleic acids.
Reaction electrode is one of key factor participating in electrochemiluminescence reaction.Traditionally, electrochemiluminescence detecting electrode mainly adopts the conductive material such as gold, silver, carbon, carrys out intensifier electrode to the catalytic capability of chemical reaction occurring in its near surface, thus improve light signal strength by carrying out finishing to electrode.The conductive material such as traditional gold, silver, carbon owing to not having the transparency, so limit their range of application.
Tin indium oxide (Indium Tin Oxide, ITO) is the transparent electrode material that a kind of electric conductivity of inventing along with IT industry technical development is in recent years fabulous.Ito thin film has the electric conductivity of semiconductor, and lowest resistivity is close to 10
-5Ω cm magnitude.Ito thin film is extremely low at the light transmittance of ultraviolet region, and near-infrared region produces reflection due to the plasma oscillation phenomenon of charge carrier, so the light transmission rate of near-infrared region ito thin film is also very low simultaneously.But the transmitance of ito thin film in visible region is very good, in visible-range, average light transmitance is more than 90%.ITO is applicable to being processed into various types of electrochemical reaction electrode very much, it has stronger adhesion and good physical strength, ITO is stable chemical performance in the basic conditions, but is soluble in strong acid, therefore can prepare electrochemical electrode circuit with sulfuric acid solution wet-etching technology.At present, ITO electrode has been applied to electrochemiluminescence detection technique field more and more.
At semiconductor industry, the process of surface treatment of ITO circuit is mainly comprised the following steps: aqueous cleaning liquid cleaning → ethanol purge → acetone cleaning → pure water cleaning, and in cleaning process, use ultrasonic cleaning process, finally dry stand-by with IR bake.In addition, be the oxygen level of increase ITO circuit surface layer and the work function on ITO surface, also need to carry out surface activation process to the ITO circuit after cleaning.Conventional activation process mode is superoxol facture, use water: hydrogen peroxide: the mixed solution of ammoniacal liquor=5:1:1, at high temperature soak 10-20 minute, the Theil indices of ITO surface excess is reduced and the increase of the ratio of oxygen, the probability injected to increase hole with the work function improving ITO device surface.
In bioelectrochemistry application, ito thin film electrode surface processing method conventional at present comprises:
(1) powder mull method, the most frequently used abrasive flour is alumina powder, can be used alone or coordinate ultrasonic cleaning, solution soaking and washing etc., the advantage of powder mull method is directly simple, can remove the sediment that major part is attached to electrode surface, but this method exists on the physical damnification of electrode surface, affects the shortcomings such as electrode characterization parameter;
(2) solution ablution, solution used comprises aqueous cleaning liquid and organic solution cleaning fluid, this disposal route is ITO electrode surface clean method the most frequently used at present, its shortcoming needs to carry out cleaning treatment step repeatedly, and be difficult to find a kind of universal cleaning liquid simultaneously meeting various cleaning requirement;
(3) ultrasonic cleaning method, it is one of current more popular cleaning method, Ultrasonic Cleaning effect is mainly by frequency, power, the factor impacts such as action time, need balanced power, the relation of action time and cleaning performance, if selection power is too large or the processing time long electrode surface that all will cause produces erosion point or crackle, there is research display, load is when the ito thin film of optical fiber surface is greater than 4 minutes in the ul-trasonic irradiation time, the resistivity of ito thin film starts to increase, time between 16-20 minute, micro-crack starts expansion, show that the marginal time of the ultrasonic process of ito thin film is 4 minutes under analogue,
(4) ultraviolet-ozone surface treatment, fundamental purpose is the flatness removed the organism of ITO remained on surface, impel ITO surface oxidation, increase the work function on ITO surface, improve ITO surface.
Summary of the invention
The invention provides a kind of method of ITO electrode being carried out to regeneration washing, its object is to ITO electrode can be repeatedly used.
The technical solution used in the present invention comprises following steps: (1) steeps ITO electrode surfaces 10 ~ 20 minutes by 65 DEG C of aqueous cleaning immersions, then adopts ultrasonic process 2 ~ 6 minutes, discards aqueous cleaning liquid and cleans ITO electrode surface 2 ~ 3 times with pure water; (2) use 10 ~ 20 minutes, soaked in absolute ethyl alcohol ITO electrode surface under room temperature, then adopt ultrasonic process 2 ~ 6 minutes, discard absolute ethyl alcohol and clean ITO electrode surface 2 ~ 3 times with pure water; (3) by " ultraviolet-ozone method " or " hydrogen peroxide oxidation method ", activation process is carried out to ITO electrode surface; (4) stand-by in 70 DEG C of oven dry with IR bake.
Above mentioned aqueous cleaning liquid comprises: 0.1% ~ 2% SDS, 0.5% ~ 6% Na
2cO
3, 0.01% ~ 0.5% EDTA, ph9.0 ~ 12.0.
Above mentioned hydrogen peroxide/ammoniacal liquor mixed solution comprises: 4% ~ 6% hydrogen peroxide, 1% ~ 2% ammoniacal liquor.
The frequency range that above mentioned ultrasonic process relates to is between 28 ~ 120kHz, and power bracket is 5 ~ 50w.
Described in the instructions that above mentioned " ultraviolet-ozone method " provides according to used UV ozone cleaning machine manufacturer, operation steps operates, ultraviolet lamp tube wavelength used is 185nm and 253.7nm, institute's oxygen pressure is 0.03 ~ 0.05 MPa, 2 ~ 40 seconds action time.
Above mentioned " hydrogen peroxide oxidation method " treatment step comprises: soak ITO electrode surface 5 ~ 10 minutes with 65 DEG C of hydrogen peroxide/ammoniacal liquor mixed solution, discards hydrogen peroxide/ammoniacal liquor mixed solution and cleans ITO electrode surface 2 ~ 3 times with pure water.
Principle of the present invention is: (1) SDS is a kind of conventional ionic surfactant, SDS has stronger destructing and elute effect for water wettability or hydrophobicity organic macromolecule in a heated state, therefore can be attached to the organic molecule residue of electrode surface by wash-out preferably; (2) EDTA is a kind of important complexing agent, can form stable complex compound with the ruthenium ion in electrochemiluminescence reagent, thus reduces the absorption of ruthenium ion at electrode surface; (3) at high temperature soak the Theil indices minimizing and the increase of the ratio of oxygen that can make ITO surface excess with hydrogen peroxide/ammoniacal liquor mixed solution, thus improve the work function of ito thin film electrode surface, increase the probability that electrode surface hole is injected.
Embodiment
Specific embodiment one
According to following steps cleaning IPO membrane electrode surface:
(1) ITO electrode is placed in containing 1% SDS, 2% Na
2cO
3, soak 20 minutes in 65 DEG C of aqueous cleaning liquid of 0.1% EDTA, ph10.0, then adopt ultrasonic process (frequency 40kHz, power 20w) 4 ~ 5 minutes, discard aqueous cleaning liquid, clean ITO electrode surface 2 times with pure water;
(2) use 20 minutes, soaked in absolute ethyl alcohol ITO electrode surface under room temperature, then adopt ultrasonic process (frequency 40kHz, power 20w) 4 minutes, discard absolute ethyl alcohol and clean ITO electrode surface 2 times with pure water;
(3) soak ITO electrode surface 5 minutes with 65 DEG C of hydrogen peroxide/ammoniacal liquor mixed solution (5% hydrogen peroxide, 1% ammoniacal liquor), discard hydrogen peroxide/ammoniacal liquor mixed solution and clean ITO electrode surface 3 times with pure water;
(4) stand-by in 70 DEG C of oven dry with IR bake.
Specific embodiment two
" ultraviolet-ozone method " is adopted to carry out ITO electrode surface activation process: pending ITO electrode module to be placed on UV ozone cleaning machine objective table, the height of objective table is regulated according to ITO electrode module height, make ITO electrode surface as far as possible just to 185nm ultraviolet lamp tube, and distance ultraviolet lamp tube 15 ~ 20 centimetres; Oxygen supply pressure is regulated to be 0.03 ~ 0.05 MPa; Arranging action time is 5 ~ 20 seconds; Process latter static 10 minutes, then opened process chamber ventilation and remove residual ozone.
Claims (1)
1. the present invention relates to a kind of in electrochemiluminescence technical field of biological the regeneration washing method to tin indium oxide electrochemiluminescence reaction electrode, the method comprises: the cleaning of aqueous cleaning liquid soaking and washing, soaked in absolute ethyl alcohol, " ultraviolet-ozone method " or the step such as " hydrogen peroxide oxidation method " electrode surface activation process and oven dry, is characterized in that:
(1) adopt the mode of aqueous cleaning liquid and absolute ethyl alcohol alternately cleaning, and in the end use " ultraviolet-ozone method " or " hydrogen peroxide oxidation method " to carry out electrode surface activation process in step;
(2) aqueous cleaning liquid used contains: 0.1% ~ 2% SDS, 0.5% ~ 6% Na
2cO
3, 0.01% ~ 0.5% EDTA, the ph value of aqueous cleaning liquid is 9.0 ~ 12.0, and temperature is 65 DEG C;
(3) adopt immersion 10 ~ 20 minutes, then the ultrasonic process mode of 2 ~ 6 minutes is cleaned, and the frequency range that wherein ultrasonic process adopts is 28 ~ 120kHz, and power bracket is 5 ~ 50 watts;
(4) in " hydrogen peroxide oxidation method " treatment step, use 65 DEG C of hydrogen peroxide/ammoniacal liquor mixed solution to soak ITO electrode surface 5 ~ 10 minutes, the hydrogen peroxide used/ammoniacal liquor mixed solution is containing 4% ~ 6% hydrogen peroxide and 1% ~ 2% ammoniacal liquor.
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| CN201510361611.3A CN104931568A (en) | 2015-06-29 | 2015-06-29 | Indium tin oxide electrochemiluminescence reaction electrode regeneration cleaning method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106860972A (en) * | 2017-01-22 | 2017-06-20 | 杭州电子科技大学 | A kind of intelligent novopen |
| CN107393944A (en) * | 2017-07-12 | 2017-11-24 | 武汉华星光电半导体显示技术有限公司 | Display panel and preparation method |
| CN112808690A (en) * | 2021-01-21 | 2021-05-18 | 人和未来生物科技（长沙）有限公司 | Method for eliminating nucleic acid residues |
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| CN103526192A (en) * | 2013-08-29 | 2014-01-22 | 南京航空航天大学 | Novel high-selectivity chemical nickel plating method for ITO/FTO/AZO conductive glass |
| JP2015049138A (en) * | 2013-09-02 | 2015-03-16 | 株式会社堀場製作所 | Response glass cleaning fluid and response glass cleaning method for glass electrode |
| CN104478233A (en) * | 2014-12-18 | 2015-04-01 | 西安工业大学 | Preparation method of electrochromic polyaniline derivative film in covalent bond with ITO (indium tin oxide) |
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2015
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008056696A1 (en) * | 2006-11-08 | 2008-05-15 | Horiba, Ltd. | Washing storage solution for glass electrode and the like |
| CN102064090A (en) * | 2010-10-15 | 2011-05-18 | 北京通美晶体技术有限公司 | Method for cleaning compound semiconductor chip |
| CN103526192A (en) * | 2013-08-29 | 2014-01-22 | 南京航空航天大学 | Novel high-selectivity chemical nickel plating method for ITO/FTO/AZO conductive glass |
| JP2015049138A (en) * | 2013-09-02 | 2015-03-16 | 株式会社堀場製作所 | Response glass cleaning fluid and response glass cleaning method for glass electrode |
| CN104478233A (en) * | 2014-12-18 | 2015-04-01 | 西安工业大学 | Preparation method of electrochromic polyaniline derivative film in covalent bond with ITO (indium tin oxide) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106860972A (en) * | 2017-01-22 | 2017-06-20 | 杭州电子科技大学 | A kind of intelligent novopen |
| CN106860972B (en) * | 2017-01-22 | 2022-10-21 | 杭州电子科技大学 | Intelligent insulin pen |
| CN107393944A (en) * | 2017-07-12 | 2017-11-24 | 武汉华星光电半导体显示技术有限公司 | Display panel and preparation method |
| CN112808690A (en) * | 2021-01-21 | 2021-05-18 | 人和未来生物科技（长沙）有限公司 | Method for eliminating nucleic acid residues |
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Application publication date: 20150923 |