CN107091809A - A kind of Silver nanorod array surface strengthens the cleaning method of Raman scattering substrate - Google Patents

A kind of Silver nanorod array surface strengthens the cleaning method of Raman scattering substrate Download PDF

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Publication number
CN107091809A
CN107091809A CN201710465832.4A CN201710465832A CN107091809A CN 107091809 A CN107091809 A CN 107091809A CN 201710465832 A CN201710465832 A CN 201710465832A CN 107091809 A CN107091809 A CN 107091809A
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CN
China
Prior art keywords
substrate
washing lotion
raman scattering
cleaning
array surface
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Pending
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CN201710465832.4A
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Chinese (zh)
Inventor
韩彩芹
姚悦
赵奕平
王稳
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Jiangsu Normal University
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Jiangsu Normal University
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Priority to CN201710465832.4A priority Critical patent/CN107091809A/en
Publication of CN107091809A publication Critical patent/CN107091809A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15Preventing contamination of the components of the optical system or obstruction of the light path
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • G01N21/658Raman scattering enhancement Raman, e.g. surface plasmons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15Preventing contamination of the components of the optical system or obstruction of the light path
    • G01N2021/155Monitoring cleanness of window, lens, or other parts

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  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses the cleaning method that a kind of Silver nanorod array surface strengthens Raman scattering substrate, comprise the following steps:A, cleaning substrate:Used SERS substrates first are gripped with clean tweezers, are soaked in washing lotion, then are taken out with clean tweezers from washing lotion, and are rinsed with absolute methanol, clean substrate is obtained;B, wash after preserve:After after substrate in atmosphere natural air drying, you can reuse, or place the substrate above in clean culture dish, and use sealed membrane sealing preserve.Thus, obtain the repeatable biochemistry detection chip utilized to molecule with Raman enhancement effect, have the advantages that operating process is simple, cost is low, it is repeatable it is strong, significantly increase signal.

Description

A kind of Silver nanorod array surface strengthens the cleaning method of Raman scattering substrate
Technical field
It is to be related to one kind to be based on table specifically the present invention relates to a kind of cleaning method of high-performance biochemistry detection chip Face strengthens Raman scattering(SERS)Biochemistry detection substrate cleaning method, belong to technical field of material.
Background technology
At present, SERS has become a powerful analysis tool, and it extends surface vibration spectrum, The solution of possibility is provided for substantial amounts of Chemical Problem.In reagent diagnosis, have to some preferable SERS substrates Higher requirement, such as:Strengthen performance high, favorable repeatability, uniformity is strong, the life-span is stable, is simple to manufacture.
But, SERS substrates usually require the either physically or chemically formation by complexity, and majority does not possess and can weighed , so just there is resource and artificial waste, the problem of testing cost is improved in the characteristic used again.
The content of the invention
For above-mentioned existing technical problem, the present invention provides a kind of simple and effective Silver nanorod array surface enhancing and drawn The cleaning method of graceful scattering substrate, for used SERS substrates, dust technology or organic mixing using certain concentration Washing lotion, is modified substrate in the way of Chemical cleaning is combined with physical cleaning, makes substrate to repeat to make in certain number of times With.
To achieve the above object, the present invention, which provides a kind of Silver nanorod array surface, strengthens the cleaning side of Raman scattering substrate Method, comprises the following steps:
A, cleaning substrate:Used SERS substrates first are gripped with clean tweezers, are soaked in washing lotion, then with clean Tweezers take out from washing lotion, and are rinsed with absolute methanol, obtain clean substrate;
Further, the preparation method of the washing lotion is as follows:With absolute methanol as solvent, diluted concentration is 65% concentrated nitric acid, is obtained It is 10 to concentration-7 M dust technology washing lotion;Or, by absolute methanol and acetone with volume ratio 3:7 mixing, obtain organic mixing and wash Liquid.
Further, described tweezers use Teflon material.
Further, the soaking step requirement:Substrate is set to lie low in washing lotion, and growing nano-rod end face is upward.
Further, the rinsing step is as follows:Absolute methanol is drawn using disposable dropper and lightly rinses substrate surface 2-3 times.
B, wash after preserve:After after substrate in atmosphere natural air drying, you can reuse, or place the substrate above clean In culture dish, and use sealed membrane sealing preserve.
The inventive method is mainly for used substrate, by being preserved after preparing washing lotion, cleaning substrate, cleaning, Obtain the repeatable biochemistry detection chip utilized to molecule with Raman enhancement effect.Compared with prior art, with operation Process is simple, cost is low, it is repeatable it is strong, the advantages of significantly increase signal.
Brief description of the drawings
Fig. 1 is the cleaning process figure of the embodiment of the present invention 1;
Fig. 2 is the cleaning process figure of the embodiment of the present invention 3.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to following implementations Example.
Embodiment 1:SERS substrates are cleaned with dust technology washing lotion.
As shown in figure 1, the SERS substrates for depositing Silver nanorod on the glass sheet, after use, are washed using dust technology Silver oxide, impurity that liquid cleaning is adhered to thereon etc., the reusable substrate, concrete operation step is as follows.
1-1, preparation washing lotion:Cleaned up with absolute methanol after centrifuge tube, first take 65% nitric acid with 0.5-10 μ L liquid-transfering guns 6.82 μ L, are taken 1000 μ L absolute methanols with 100-1000 μ L liquid-transfering guns, both are mixed in centrifuge tube a, mixed using whirlpool Device is sufficiently mixed it, and it is 10 × 10 to obtain concentration-6M a liquid;Then 100 μ L a liquid are taken with 10-200 μ L liquid-transfering guns, with 900 μ L absolute methanols are mixed in centrifuge tube b, and it is sufficiently mixed using eddy mixer, and it is 10 × 10 to obtain concentration-7M b liquid; 200 μ L b liquid is taken again, is mixed in 1800 μ L absolute methanols in centrifuge tube c, is sufficiently mixed it using eddy mixer, obtains It is 10 × 10 to concentration-8M c liquid, is that required 2mL concentration is 10-7M dust technology washing lotion.
1-2, cleaning substrate:The edge of SERS substrates is carefully clamped with Teflon tweezers, it is gently put into the dilute nitre of 2mL In pickle, substrate is lain low in washing lotion as far as possible, and grow the end face of Silver nanorod upward so that washing lotion submerges substrate, The silver oxide of substrate surface is allowed fully to be contacted with dust technology, to remove the silver oxide layer and impurity on Silver nanorod;After about 1min, Cleaned substrate is gently taken out with Teflon tweezers, is gently rinsed at least twice with absolute methanol, washes away what is remained in substrate Silver oxide, impurity and waste liquid, obtain clean substrate.
1-3, wash after preserve:The methanol remained in substrate after to be cleaned is evaporated in atmosphere, and substrate is positioned over Preserved in clean culture dish, and culture dish is sealed with sealed membrane, in case next time, detection was used.
Embodiment 2:The substrate that BPE has been added dropwise is cleaned with dust technology washing lotion.
For depositing the SERS substrates of Silver nanorod on the glass sheet, and BPE molecules are added dropwise, after use, using dilute BPE molecules, silver oxide, impurity that the cleaning of nitric acid washing lotion is adhered to thereon etc., the reusable substrate, concrete operation step is such as Under.
2-1, preparation washing lotion:This example washing lotion uses 2mL concentration 10-7M dilute nitric acid solution, the same 1-1 of preparation method.
2-2, cleaning substrate:Silver nanorod array substrate that BPE molecules have been added dropwise carefully is clamped with Teflon tweezers Edge, it is gently put into 2mL dust technology washing lotions, substrate is lain low in washing lotion as far as possible, and grow the end of Silver nanorod Up so that washing lotion submerges substrate, allows the silver oxide of substrate surface fully to be contacted with dust technology, dust technology is by the oxidation on surface Silver reaction is simultaneously dissolved in washing lotion;After about 1min, cleaned Silver nanorod array substrate is gently taken out with Teflon tweezers, is used Absolute methanol is gently flushed three times, and washes away the washing lotion remained in substrate, and BPE molecules can be made to be taken off from Silver nanorod array It is attached to be dissolved in methanol leacheate, the impurity on silver nanoparticle array substrate surface is removed, clean substrate is obtained.
2-3, wash after preserve:The methanol remained in substrate after to be cleaned evaporates in atmosphere, you can recycling The substrate is detected again to BPE.
Embodiment 3:SERS substrates are cleaned with organic mixing washing lotion.
As shown in Fig. 2 the SERS substrates of silver oxide are covered on Silver nanorod, and nanometer rods for depositing on the glass sheet, Cleaned using organic mixing washing lotion, to reuse substrate, concrete operation step is as follows.
3-1, cleaned up after centrifuge tube with absolute methanol, with the μ L of 100-1000 μ L liquid-transfering guns methanol 600, use 100-1000 The 1400 μ L acetone that μ L liquid-transfering guns take, both are mixed in centrifuge tube, it is sufficiently mixed using eddy mixer, body is obtained Product is than being 3:7 methanol and acetone mixing washing lotion.
3-2, the edge for carefully clamping with Teflon tweezers SERS substrates, it are gently put into 2mL dust technology washing lotions, Substrate is set to lie low in washing lotion as far as possible, and the end face for growing Silver nanorod is upward, makes the organic mixing washing lotion submergence substrates of 2mL, The silver oxide of substrate surface is allowed fully to be contacted with organic mixing washing lotion, the meeting under the catalytic action of oxygen of the methanol in organic washing lotion Reacted with silver oxide, to remove the silver oxide layer on Silver nanorod;Methanol and acetone can dissolve most substrate surfaces The impurity of residual;After about 1min, cleaned SERS substrates are gently taken out with Teflon tweezers, gently rinsed with absolute methanol to It is few to wash away the silver oxide remained in substrate, impurity and waste liquid twice, obtain clean substrate.
3-3, wash after preserve:The methanol remained in substrate after to be cleaned is evaporated in atmosphere, and substrate is positioned over Preserved in clean culture dish, culture dish is sealed with sealed membrane.After substrate is taken out, rhodamine B to be measured is added dropwise thereon molten Liquid, obtains rhodamine S ERS signals, you can for subsequent detection.
To sum up, it is known that the present invention is applied to clean used SERS substrates, it is reused in certain number of times, drops Low testing cost, improves resource utilization.

Claims (6)

1. a kind of Silver nanorod array surface strengthens the cleaning method of Raman scattering substrate, it is characterised in that comprise the following steps:
A, cleaning substrate:Used SERS substrates first are gripped with clean tweezers, are soaked in washing lotion, then with clean Tweezers take out from washing lotion, and are rinsed with absolute methanol, obtain clean substrate;
B, wash after preserve:After after substrate in atmosphere natural air drying, you can reuse, or place the substrate above clean culture In ware, and use sealed membrane sealing preserve.
2. a kind of Silver nanorod array surface according to claim 1 strengthens the cleaning method of Raman scattering substrate, it is special Levy and be, the preparation method of the washing lotion is as follows:With absolute methanol as solvent, diluted concentration is 65% concentrated nitric acid, is obtained Concentration is 10-7M dust technology washing lotion.
3. a kind of Silver nanorod array surface according to claim 1 strengthens the cleaning method of Raman scattering substrate, it is special Levy and be, the preparation method of the washing lotion is as follows:By absolute methanol and acetone with volume ratio 3:7 mixing, obtain organic mixing and wash Liquid.
4. a kind of Silver nanorod array surface according to claim 1 or 2 or 3 strengthens the cleaning side of Raman scattering substrate Method, it is characterised in that described tweezers use Teflon material.
5. a kind of Silver nanorod array surface according to claim 1 or 2 or 3 strengthens the cleaning side of Raman scattering substrate Method, it is characterised in that the soaking step requirement makes substrate lie low in washing lotion, and growing nano-rod end face is upward.
6. a kind of Silver nanorod array surface according to claim 1 or 2 or 3 strengthens the cleaning side of Raman scattering substrate Method, it is characterised in that the rinsing step is as follows:Absolute methanol is drawn using disposable dropper and lightly rinses substrate surface 2- 3 times.
CN201710465832.4A 2017-06-19 2017-06-19 A kind of Silver nanorod array surface strengthens the cleaning method of Raman scattering substrate Pending CN107091809A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108375567A (en) * 2018-02-24 2018-08-07 国家纳米科学中心 A kind of surface-enhanced Raman substrate and preparation method thereof
WO2019179006A1 (en) * 2018-03-22 2019-09-26 苏州天际创新纳米技术有限公司 Method for preparing, saving and loading sers chip

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103048304A (en) * 2012-12-07 2013-04-17 江苏大学 Preparation method of recyclable surface-enhanced Raman-spectrum active substrate
CN104251853A (en) * 2014-05-14 2014-12-31 苏州佳因特光电科技有限公司 Method for detecting perchlorate radical in water by using surface enhanced Raman scattering technology
CN106731885A (en) * 2016-12-19 2017-05-31 中国科学院宁波材料技术与工程研究所 A kind of metal organic framework/metal nano ion composite filtering film and its preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103048304A (en) * 2012-12-07 2013-04-17 江苏大学 Preparation method of recyclable surface-enhanced Raman-spectrum active substrate
CN104251853A (en) * 2014-05-14 2014-12-31 苏州佳因特光电科技有限公司 Method for detecting perchlorate radical in water by using surface enhanced Raman scattering technology
CN106731885A (en) * 2016-12-19 2017-05-31 中国科学院宁波材料技术与工程研究所 A kind of metal organic framework/metal nano ion composite filtering film and its preparation method and application

Non-Patent Citations (2)

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Title
JIE CHENG 等: "Highly Sensitive Detection of Melamine Using a One-Step Sample Treatment Combined with a Portable Ag Nanostructure Array SERS Sensor", 《PLOS ONE》 *
吕明阳: "三维金/蝉翅基底的表面增强拉曼散射性能研究及其在生物检测方面的应用", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108375567A (en) * 2018-02-24 2018-08-07 国家纳米科学中心 A kind of surface-enhanced Raman substrate and preparation method thereof
WO2019179006A1 (en) * 2018-03-22 2019-09-26 苏州天际创新纳米技术有限公司 Method for preparing, saving and loading sers chip

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