CN110331374A - A kind of sample stage being prepared on a large scale surface enhanced Raman substrate - Google Patents

A kind of sample stage being prepared on a large scale surface enhanced Raman substrate Download PDF

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Publication number
CN110331374A
CN110331374A CN201910664729.1A CN201910664729A CN110331374A CN 110331374 A CN110331374 A CN 110331374A CN 201910664729 A CN201910664729 A CN 201910664729A CN 110331374 A CN110331374 A CN 110331374A
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China
Prior art keywords
substrate
sample stage
boss
enhanced raman
silver
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CN201910664729.1A
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Chinese (zh)
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张政军
樊易航
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Tsinghua University
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Tsinghua University
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Priority to CN201910664729.1A priority Critical patent/CN110331374A/en
Publication of CN110331374A publication Critical patent/CN110331374A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/225Oblique incidence of vaporised material on substrate
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50Substrate holders

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Toxicology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The sample stage that surface enhanced Raman substrate can be prepared on a large scale simultaneously the invention discloses one kind belongs to trace organic substance detection technique field for being prepared on a large scale surface enhanced Raman substrate.The sample stage includes support section and boss shape annulus, and the top diameter of the boss shape annulus is greater than base diameter, and the surface of the boss is arc-shaped shape.Sample stage of the invention, can be using inclination growth method simultaneously in multiple deposition on substrate Silver nanorods.The array film being made of more substrate Silver nanorods has preferable homogeneity of product, the production efficiency of traditional preparation methods can be improved.

Description

A kind of sample stage being prepared on a large scale surface enhanced Raman substrate
Technical field
The invention belongs to trace organic substance detection technique field, in particular to one kind can be prepared on a large scale surface enhanced drawing The sample stage of graceful substrate.
Background technique
Surface-enhanced Raman effects as a kind of trace materials detection method, it is highly sensitive with it, quickly detection, low take The fields such as environmental pollution analyte detection, food safety detection, biology and medical treatment are widely used in the advantages that, nondestructive analysis. The highly sensitive surface enhanced Raman substrate of the precious metal materials such as gold, silver or copper preparation is generallyd use, wherein silver nanostructured base The surface-enhanced Raman effect at bottom is best.Since the price of noble metal is higher, and the method for electron beam evaporation plating is spread due to space For spherical shape, a large amount of deposits materials cause a large amount of wastes in cavity wall.
In order to improve its deficiency, the present invention to tilt growing technology as basic principle, evaporation source beam direction and substrate at 86 degree, and simple cone-shaped ring structure is used, more substrates are pasted, reaches and the raw material evaporated is more sufficiently applied, And guarantee each substrate and evaporate the angle of line to be 86 degree needed.
Summary of the invention
The purpose of the present invention is design a kind of novel while largely to prepare the sample stage of surface enhanced Raman substrate.
In order to achieve the above object, the technical solution adopted by the present invention is that: one kind being prepared on a large scale surface-enhanced Raman base The sample stage at bottom, it is characterised in that: the sample stage includes support section and boss shape annulus, the top of the boss shape annulus Diameter is greater than base diameter, and the surface of the boss is arc-shaped shape.
The circular shape of the sample stage is entirely located in vertical direction.
The boss cone angle of the boss shape annulus is 6-8 degree, and cone angle bisector is being directed toward the center of circle of boss shape annulus just Lower section.
The method that the sample stage prepares surface enhanced Raman substrate, comprising the following steps:
(1) precondition substrate;
(2) pretreated substrate is pasted on sample stage;
(3) the outer circle center of circle of sample stage is aligned with evaporation source;
(4) e-beam evaporation chamber is vacuumized;
(5) in the oblique rod film of deposition on substrate nanometer of sample stage.
Step (1) pretreatment is that the silicon chip acetone of single-sided polishing, dehydrated alcohol, deionized water is ultrasonic one by one It cleans and dries.
Step (2) described substrate is evenly arranged on boss shape annulus inner side and outer side.
Step (3) evaporation source is crucible, is located at immediately below the center of circle of boss shape annulus.
The vacuum degree of step (4) described e-beam evaporation chamber is;4*10-4Pa。
Step (5) is described to be deposited on room temperature progress, uses metallic silver for target, the plating rate for controlling silver isIn sample It is co-deposited the silver-colored titanium that length is about 600nm in the substrate of platform and is dissolved the oblique rod film of nanometer.
By inclination growth method in step (5), evaporation source beam direction and substrate are at 86 degree, in multiple deposition on substrate silver Nanometer rods form Raman substrate by more substrate Silver nanorod forming array films.
Beneficial effects of the present invention, sample stage of the invention can be sunk on multiple substrates simultaneously using inclination growth method Product Silver nanorod.The array film being made of more substrate Silver nanorods has preferable homogeneity of product, traditional system can be improved The production efficiency of Preparation Method.
Detailed description of the invention
Fig. 1 is the outside drawing of sample stage of the present invention.
Fig. 2 is the sample stage photo that substrate has been pasted in the embodiment of the present invention.
The electromicroscopic photograph of the Silver nanorod array surface enhancing Raman substrate of Fig. 3 chip bench preparation of the present invention.
Fig. 4 is the R6G Molecular Raman enhancing of the Silver nanorod array of preparation of the embodiment of the present invention.
Specific embodiment
The present invention deposits the surface-enhanced Raman of multiple Silver nanorod arrays using inclination growth method simultaneously on sample stage Substrate.With reference to the accompanying drawing 1~4 and embodiment the present invention is illustrated.
Embodiment 1
(1) the silicon chip acetone of single-sided polishing, dehydrated alcohol, deionized water are cleaned by ultrasonic and are dried one by one;
(2) pretreated silicon chip is pasted on sample stage of the invention
(3) the outer circle center of circle of sample stage is aligned with crucible
(4) at room temperature, it uses metallic silver for target, the chamber of twin-cathode ray beam evaporation coating machine is evacuated to vacuum, vacuum Degree is;4*10-4Pa。
(5) it adjusts, the plating rate for controlling silver isThe Yin Na that length is about 600nm is co-deposited in the substrate of sample stage The oblique rod film of rice;
(6) 10 are prepared-5The R6G solution of mol/L;
(7) surface enhanced Raman substrate prepared by step (1)~(5) is put into the solution of step 6 preparation, impregnates 30 points Clock;
(8) surface enhanced Raman substrate for being adsorbed with trace methylene blue obtained by step (7) is put into Raman spectrometer, selected The light source that wavelength is 785nm is selected, the measurement of Raman spectrum is carried out;
It can be observed that the R6G signal peak strong signal of several substrates is essentially identical, while can see on several substrates The pattern of Silver nanorod array is almost the same, it can be said that the bright surface enhanced Raman substrate prepared by the sample stage Effect is almost consistent, has reached expected purpose.
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.

Claims (10)

1. a kind of sample stage for being prepared on a large scale surface enhanced Raman substrate, it is characterised in that: the sample stage includes support portion Divide and boss shape annulus, the top diameter of the boss shape annulus are greater than base diameter, the surface of the boss is arc-shaped shape.
2. sample stage according to claim 1, which is characterized in that the circular shape of the sample stage is entirely located in vertical side To.
3. sample stage according to claim 1, which is characterized in that the boss cone angle of the boss shape annulus is 6-8 degree, and And cone angle bisector is directed toward immediately below the center of circle of boss shape annulus.
4. the method that sample stage described in claims 1 to 3 any one prepares surface enhanced Raman substrate, which is characterized in that packet Include following steps:
(1) precondition substrate;
(2) pretreated substrate is pasted on sample stage;
(3) the outer circle center of circle of sample stage is aligned with evaporation source;
(4) e-beam evaporation chamber is vacuumized;
(5) in the oblique rod film of deposition on substrate nanometer of sample stage.
5. according to the method described in claim 4, it is characterized in that, step (1) pretreatment is by the silicon substrate of single-sided polishing Piece acetone, dehydrated alcohol, deionized water are cleaned by ultrasonic and dry one by one.
6. according to the method described in claim 4, it is characterized in that, step (2) described substrate is evenly arranged on the inside of boss shape annulus The outside and.
7. according to the method described in claim 4, it is characterized in that, step (3) evaporation source is crucible, positioned at boss shape Immediately below the center of circle of annulus.
8. according to the method described in claim 4, it is characterized in that, the vacuum degree of step (4) described e-beam evaporation chamber is; 4*10-4Pa。
9. according to the method described in claim 4, it is characterized in that, step (5) is described to be deposited on room temperature progress, using metallic silver For target, the plating rate for controlling silver isThe oblique rod film of silver nanoparticle that length is about 600nm is co-deposited in the substrate of sample stage.
10. according to the method described in claim 4, it is characterized in that, passing through inclination growth method, evaporation source line in step (5) Direction and substrate are formed and are drawn by more substrate Silver nanorod forming array films in multiple deposition on substrate Silver nanorods at 86 degree Graceful substrate.
CN201910664729.1A 2019-07-23 2019-07-23 A kind of sample stage being prepared on a large scale surface enhanced Raman substrate Pending CN110331374A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201141921Y (en) * 2008-01-09 2008-10-29 中国科学院上海光学精密机械研究所 Inclined deposition plated film device
US20130183540A1 (en) * 2012-01-12 2013-07-18 Yi-Jun Jen Metal nanopillars for surface-enhanced Raman Spectroscopy (SERS) substrate and method for preparing same
CN103590005A (en) * 2013-11-15 2014-02-19 浙江星星瑞金科技股份有限公司 Vacuum coating machine
CN205662594U (en) * 2016-05-03 2016-10-26 哈尔滨理工大学 Novel coating film tool
US20170045456A1 (en) * 2014-04-15 2017-02-16 Rutgers, The State University Of New Jersey Gold Nanostar Substrates for SERS Sensing in the Femtomolar Regime
CN106672897A (en) * 2016-12-29 2017-05-17 中国人民解放军国防科学技术大学 Array type silver nano-pillar coated with gold film at its surface and preparation method thereof
CN207904359U (en) * 2017-12-08 2018-09-25 光驰科技(上海)有限公司 A kind of plated film spherical surface umbrella stand

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201141921Y (en) * 2008-01-09 2008-10-29 中国科学院上海光学精密机械研究所 Inclined deposition plated film device
US20130183540A1 (en) * 2012-01-12 2013-07-18 Yi-Jun Jen Metal nanopillars for surface-enhanced Raman Spectroscopy (SERS) substrate and method for preparing same
CN103590005A (en) * 2013-11-15 2014-02-19 浙江星星瑞金科技股份有限公司 Vacuum coating machine
US20170045456A1 (en) * 2014-04-15 2017-02-16 Rutgers, The State University Of New Jersey Gold Nanostar Substrates for SERS Sensing in the Femtomolar Regime
CN205662594U (en) * 2016-05-03 2016-10-26 哈尔滨理工大学 Novel coating film tool
CN106672897A (en) * 2016-12-29 2017-05-17 中国人民解放军国防科学技术大学 Array type silver nano-pillar coated with gold film at its surface and preparation method thereof
CN207904359U (en) * 2017-12-08 2018-09-25 光驰科技(上海)有限公司 A kind of plated film spherical surface umbrella stand

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张政军等: ""倾斜生长法制备表面增强拉曼散射基底及其应用"", 《金属功能材料》 *

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