CN104458855A - Preparation method of nano-Au-silica sol-polyvinyl pyrrolidone (PVP) modified Au electrode - Google Patents
Preparation method of nano-Au-silica sol-polyvinyl pyrrolidone (PVP) modified Au electrode Download PDFInfo
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- CN104458855A CN104458855A CN201410760580.4A CN201410760580A CN104458855A CN 104458855 A CN104458855 A CN 104458855A CN 201410760580 A CN201410760580 A CN 201410760580A CN 104458855 A CN104458855 A CN 104458855A
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Abstract
The invention discloses a preparation method of a nano-Au-silica sol-polyvinyl pyrrolidone (PVP) modified Au electrode. The preparation method comprises the following steps: heating a chloroauric acid solution under the condition of stirring and then adding trisodium citrate to prepare nano-Au; polishing and activating an Au electrode and repeatedly scanning the Au electrode until a stable CV (control vertex) curve is obtained; mixing silica sol, nano-Au and 1% PVP to obtain a nano-Au-silica sol-PVP compound liquid, soaking the treated Au electrode in the compound liquid for 30 seconds and airing the Au electrode at room temperature, thus preparing the Au electrode. The preparation method has the beneficial effects that with a three-dimensional net structure, the silica sol has the characteristics of higher adsorbability and adhesivity, better biocompatibility and catalytic activities, and the like; meanwhile, the defect that the silica sol is easy to crack is overcome by adding PVP K-30; nano-Au has the characteristics of high surface activity, large specific surface area, good electrical conductivity, and the like and can conduce to promoting electron transfer between the electrode and a surface modifier.
Description
Technical field
The present invention relates to the preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode.
Background technology
Electrochemiluminescence (Electrochemiluminescence, ECL) analytic approach has that instrument is simple, the range of linearity is wide, highly sensitive and be convenient to the advantages such as detection.Chemically modified electrode to raising sensitivity and selectivity very favourable, it is combined with electrochemiluminescence analysis method, has widened the investigation and application category of ECL method.At present, the main method of preparative chemistry modified electrode has drop-coating, covalent bonding method, absorption method, polymer thin embrane method etc.But all there is respective weak point in these methods: the modified electrode reappearance as obtained by drop-coating is poor; Covalent bonding method preparation process is loaded down with trivial details and electrode surface coverage rate is low; Modified electrode prepared by absorption method easily comes off from electrode surface, less stable, and serviceable life is subject to certain restrictions; Nafion applies maximum a kind of cationic high-molecular materials in polymer thin embrane method, but Nafion film is dense, exists analyzing the defects such as the mass transfer velocity of thing is slower.
Summary of the invention
Object of the present invention is exactly for above-mentioned defect of the prior art, provides the preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode.
To achieve these goals, technical scheme provided by the invention is: the preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode, under agitation chlorauric acid solution is heated, trisodium citrate is added after boiling, solution colour changes, after stable, stop heating, place room temperature and can obtain nm of gold; After being ground on emery paper by gold electrode, deerskin towel uses Al
2o
3throw to minute surface, use water, 1:1 ethanol, water ultrasonic cleaning after washing away electrode surface burnishing powder respectively, be then placed in 0.1 mol/L sulfuric acid solution and carry out cyclic voltammetry activation, in-0.2 ~+1.4 V, be repeatedly scanned up to and obtain stable CV curve; Silicasol, nm of gold, 1% PVP are mixed to get nm of gold-silicasol-polyvinyl pyrrolidone complex liquid, the gold electrode after process are immersed 30s in this complex liquid, dries under room temperature.
Beneficial effect of the present invention is: the preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode, the three-dimensional net structure of silicasol (Silica sol), makes it have higher adsorbability and cohesiveness, the preferably feature such as biocompatibility and catalytic activity.Meanwhile, PVP K-30 (PVP) add the defect improving silicasol and easily chap.Nm of gold (Nano-Au) has that surfactivity is high, specific surface area is large and the feature such as good conductivity, can promote the electron transmission of electrode and surface modification.
Embodiment
embodiment 1:
The preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode, heated by chlorauric acid solution under agitation, add trisodium citrate after boiling, solution colour changes, after stable, stop heating, places room temperature and can obtain nm of gold; After being ground on emery paper by gold electrode, deerskin towel uses Al
2o
3throw to minute surface, use water, 1:1 ethanol, water ultrasonic cleaning after washing away electrode surface burnishing powder respectively, be then placed in 0.1 mol/L sulfuric acid solution and carry out cyclic voltammetry activation, in-0.2 ~+1.4 V, be repeatedly scanned up to and obtain stable CV curve; Silicasol, nm of gold, 1% PVP are mixed to get nm of gold-silicasol-polyvinyl pyrrolidone complex liquid, the gold electrode after process are immersed 30s in this complex liquid, dries under room temperature.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the preparation method of nm of gold-silicasol-polyvinyl pyrrolidone modified gold electrode, is characterized in that, is heated by chlorauric acid solution under agitation, trisodium citrate is added after boiling, solution colour changes, after stable, stop heating, places room temperature and can obtain nm of gold; After being ground on emery paper by gold electrode, deerskin towel uses Al
2o
3throw to minute surface, use water, 1:1 ethanol, water ultrasonic cleaning after washing away electrode surface burnishing powder respectively, be then placed in 0.1 mol/L sulfuric acid solution and carry out cyclic voltammetry activation, in-0.2 ~+1.4 V, be repeatedly scanned up to and obtain stable CV curve; Silicasol, nm of gold, 1% PVP are mixed to get nm of gold-silicasol-polyvinyl pyrrolidone complex liquid, the gold electrode after process are immersed 30s in this complex liquid, dries under room temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410760580.4A CN104458855A (en) | 2014-12-12 | 2014-12-12 | Preparation method of nano-Au-silica sol-polyvinyl pyrrolidone (PVP) modified Au electrode |
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| CN201410760580.4A CN104458855A (en) | 2014-12-12 | 2014-12-12 | Preparation method of nano-Au-silica sol-polyvinyl pyrrolidone (PVP) modified Au electrode |
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| CN104458855A true CN104458855A (en) | 2015-03-25 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628682A (en) * | 2016-01-04 | 2016-06-01 | 广西科技大学 | Method for detecting content of sophocarpidine in medicine by using electrogenerated chemiluminescence behavior of composite modifier loaded pyrolysis graphite electrode |
| CN105675583A (en) * | 2016-01-04 | 2016-06-15 | 广西科技大学 | Method for determination of content of verapamil hydrochloride in drug by using electrogenerated chemiluminescence behavior of composite modifier-supported pyrolytic graphite electrode |
| CN110542712A (en) * | 2019-09-20 | 2019-12-06 | 肇庆学院 | preparation method of electrochemical sensor for detecting copper ions with high sensitivity |
| CN114163566A (en) * | 2021-12-10 | 2022-03-11 | 沈阳先进涂层材料产业技术研究院有限公司 | Nano-gold-containing polyvinylpyrrolidone/poly-N-vinylcaprolactam hybrid microgel and preparation method thereof |
-
2014
- 2014-12-12 CN CN201410760580.4A patent/CN104458855A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105628682A (en) * | 2016-01-04 | 2016-06-01 | 广西科技大学 | Method for detecting content of sophocarpidine in medicine by using electrogenerated chemiluminescence behavior of composite modifier loaded pyrolysis graphite electrode |
| CN105675583A (en) * | 2016-01-04 | 2016-06-15 | 广西科技大学 | Method for determination of content of verapamil hydrochloride in drug by using electrogenerated chemiluminescence behavior of composite modifier-supported pyrolytic graphite electrode |
| CN105675583B (en) * | 2016-01-04 | 2018-04-06 | 广西科技大学 | Utilize the method for verapamil hydrochloride content in composite modified dose of load pyrolytic graphite electrode electrogenerated chemiluminescence behavior determination medicine |
| CN105628682B (en) * | 2016-01-04 | 2018-04-06 | 广西科技大学 | Utilize the method for matrine content in composite modified dose of load pyrolytic graphite electrode electrogenerated chemiluminescence behavior determination medicine |
| CN110542712A (en) * | 2019-09-20 | 2019-12-06 | 肇庆学院 | preparation method of electrochemical sensor for detecting copper ions with high sensitivity |
| CN110542712B (en) * | 2019-09-20 | 2020-04-24 | 肇庆学院 | Preparation method of electrochemical sensor for detecting copper ions with high sensitivity |
| CN114163566A (en) * | 2021-12-10 | 2022-03-11 | 沈阳先进涂层材料产业技术研究院有限公司 | Nano-gold-containing polyvinylpyrrolidone/poly-N-vinylcaprolactam hybrid microgel and preparation method thereof |
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Application publication date: 20150325 |