CN107741418A - Method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal - Google Patents
Method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal Download PDFInfo
- Publication number
- CN107741418A CN107741418A CN201710974599.2A CN201710974599A CN107741418A CN 107741418 A CN107741418 A CN 107741418A CN 201710974599 A CN201710974599 A CN 201710974599A CN 107741418 A CN107741418 A CN 107741418A
- Authority
- CN
- China
- Prior art keywords
- gold nano
- triangular plate
- solution
- gold
- nano triangular
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/653—Coherent methods [CARS]
- G01N2021/655—Stimulated Raman
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/653—Coherent methods [CARS]
- G01N2021/656—Raman microprobe
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, it is characterised in that：Comprise the following steps：A, gold nano triangular plate synthesizes：A1, using surfactant cetyl trimethylammonium bromide to gold chloride carry out hydro-thermal process；A2, with centrifuge the obtained reaction products of step A13 are centrifuged, and precipitation is cleaned with ultra-pure water；A3, repeat A2 steps three times, obtain gold nano triangular plate；B, the preparation of the encapsulating structure of gold nano triangular plate；B1, silicon chip surface sputter layer of metal film；B2, metal film soaked in 4 nitro thiophenol molecule alcoholic solutions, be then rinsed successively with alcohol, ultra-pure water, then dried up with nitrogen；B3, the colloidal solution of gold nano triangular plate is spin-coated on metal film, and allows it to volatilize naturally；C, to the detection of the encapsulating structure interior molecules Raman signal of gold nano triangular plate；It the composite can be widely applied to the production and detection of micro-nano device.
Description
Technical field
The present invention relates to molecular signal detection method multi-modulus frequency divider circuit, more particularly to one kind to be based on pinpoint enhanced Raman
The method of technology for detection Metal Packaging interior molecules signal.
Background technology
Raman spectrum can cover all frequency separations of molecular vibration, study respectively as a kind of vibrational spectrum technology
Gu there is the advantage of uniqueness in kind of solid-liquid, solid/gas and solid/section system, can more be used for deeply characterizing various tables from molecular level
The structure and process in face (interface).Limited by its detection sensitivity, after finding SERS phenomenon,
It is widely used in the research in the fields such as material, surface and life.But largely receive metal because it strengthens performance
The limitation of nanostructured, so many fields are also only limitted to the application and research in laboratory, it can not still realize and be led in Practical Project
Application in domain.Until the discovery of Tip-Enhanced Raman Spectroscopy technology, just preliminary to realize the sky for utilizing means acquisition higher
Between resolution technique.
Pinpoint enhanced Raman technology is being used in combination Scanning probe technique and Raman spectroscopy, and cardinal principle is profit
Gold/acupuncture needle point that radius of curvature is tens nanometers is manipulated with the control system of Scanning probe technique, is realized with sample closely
Contact, and in the case where the laser of appropriate wavelength coordinates, reach the plasma resonance at minim gap between needle point and sample
Generation, so as to obtain the very big enhancing of the region electromagnetic field, be finally reached the acquisition of signal near field range.Encapsulating structure is made
To be common to protect its internal material technology, it is commonly used for the protection of chip internal integrated circuit or the guarantor of other nano materials
Shield, such as protection for fluorescence quantum, can greatly improve the composite that fluorescence quantum micro-nano encapsulates uses the longevity
Life.And in the research process of metal Nano structure, we are it is often found that institute's self-assembling formation between some metal levels and molecular layer
Encapsulating structure, be that randomness is bigger the characteristics of such encapsulating structure；Pass through the research to such encapsulating structure and needle point
Strengthen the application of Raman detection technology, detection and research to large area encapsulating structure can be done step-by-step in we.This technology
Production and the detection part of micro-nano device can be widely used in, the production to following high precision instrument has great with application
Practical value.
With the development of micro-nano chip technology, the miniaturization of product has become the final home to return to of following production；So pin
Detection to miniature nano-device specific position running status becomes particularly important, and in order to improve the use longevity of particular device
Life is usually packaged coating protection to device, and this causes very big interference for the status monitoring of late device.Increase with reference to needle point
Strong Raman technology it is lossless, non-contact, high-precision the advantages that, the patent proposes one kind to be based on pinpoint enhanced Raman technology for detection
The method of Metal Packaging interior molecules signal.
The content of the invention
The technical problems to be solved by the invention are that providing one kind is based on pinpoint enhanced Raman technology for detection Metal Packaging
The method of interior molecules signal.
In order to solve the above-mentioned technical problem the present invention, adopts the following technical scheme that：
A kind of method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, it is characterised in that：Bag
Include following steps：
A, gold nano triangular plate synthesizes
A1, using surfactant cetyl trimethylammonium bromide to gold chloride carry out hydro-thermal process；
A11, first by surfactant cetyl trimethylammonium bromide in mass ratio be 1：780~1:790 ratio
It is added drop-wise in distilled water, it is lasting at room temperature to stir until cetyl trimethylammonium bromide is dissolved completely in distilled water；
A12, by concentration be 12~13mmol/L chlorauric acid solution add cetyl trimethylammonium bromide solution in, chlorine
Auric acid solution is 1 by volume with cetyl trimethylammonium bromide solution:20 ratio mixing, and continue to stir, until molten
Liquid gradually becomes light yellow by colourless；
A13, the obtained mixed solutions of step A12 are transferred in stainless steel water heating kettle again, seal and it is placed on 160~
In 180 DEG C of heating furnaces after 6~8h of continuous heating, room temperature is naturally cooled to；
A2, with centrifuge the obtained reaction products of step A13 are centrifuged, and precipitation is cleaned with ultra-pure water；
A3, repeat A2 steps three times, finally obtain gold nano triangular plate；
B, the preparation of the encapsulating structure of gold nano triangular plate
B1, using electron beam evaporation technique silicon chip surface sputter a layer thickness be 80nm-120nm metal film；
B2, metal film soaked into 2h in 4- nitro thiophenol molecule alcoholic solutions, then, successively with alcohol, ultra-pure water
It is rinsed, to remove molecular cluster unnecessary on metal film；Dried up again with nitrogen, it is ensured that form one layer in metallic film surface
The monolayer of even distribution；
B3, gold nano triangular plate is dissolved in alcoholic solution, the colloidal solution of gold nano triangular plate obtained, by gold nano
The colloidal solution of triangular plate is spin-coated on metal film, and allows it to volatilize naturally；
C, to the detection of the encapsulating structure interior molecules Raman signal of gold nano triangular plate.
According to the method for the present invention based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal
Preferred scheme, step C are：
From the Au probe or silver-colored probe that radius of curvature is tens nanometers, probe is moved to position residing for gold nano triangular plate
Put, the Raman signal of encapsulating structure inside 4- nitro thiophenol molecules is detected.
According to the method for the present invention based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal
Preferred scheme, step C comprise the following steps：
C1, gold nano grain synthesis
C11, it is 1 by volume:2：50 ratio by mass fraction be 20% poly- hexadiene dimethylammonium chloride ammonium salt solution,
Concentration is that 1mol/L phosphoric acid solution is added to stirring 5min~10min in ethylene glycol solution,
C12, by the chlorauric acid solution that concentration is 0.5mol/L it is again 1 by volume:1000 ratio is added to step C11
In obtained mixed solution, then persistently stir 15~20min；Then heating continues stirring 30 under 180~200 DEG C of constant temperatures
~40min, then room temperature persistently stirs 1h until mixed solution cools down；
C13 then again by volume be 1:4000 ratio adds concentration and is 0.5mol/L chlorauric acid solution, and holds
After continuous stirring 20h, it was observed that there is the generation of gold particles suspension in solution, mixed solution is put into 190~200 DEG C of conditions again
After lower heated at constant temperature 1h, room temperature cooling 1h, gold nano grain is obtained；
Repeat step C13 is acted, and can obtain the bigger and more round shape gold nano grain of size；
C2, gold nano triangular plate prepared by step B3 is added drop-wise to after the gold nano grain of preparation is diluted with absolute alcohol solution
Encapsulating structure on, after volatilizing naturally, found under the auxiliary of light microscope and include the gold nano triangle of gold nano grain
Chip package, and simultaneously using position instrument copper mesh to the position carry out telltale mark；
C3, using the test position demarcated in burnt micro Raman spectra detection platform detecting step C2 is copolymerized, to encapsulation
The Raman signal of inside configuration 4- nitro thiophenol molecules is detected.
A kind of method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal of the present invention
Beneficial effect is：The present invention using pinpoint enhanced Raman technology it is lossless, non-contact, high-precision the advantages that to this special micro-nano
Encapsulating structure is detected, and is combined simulation result and carried out theory analysis to experimental result, and the present invention can be widely used in micro-
The production and detection of nano parts, the production to following high precision instrument have great practical value with application.
Brief description of the drawings
Fig. 1 is Fig. 1 Golden Triangle chip package schematic diagram.
Fig. 2 needle points Raman technology detects encapsulating structure schematic diagram.
Fig. 3 gold nano triangle chip package telltale marks position.
Fig. 4 pinpoint enhanced Raman technology for detection encapsulating structure schematic diagrams.
Fig. 5 is pinpoint enhanced Raman technology for detection encapsulating structure result.
Fig. 6 is pinpoint enhanced Raman technology for detection encapsulating structure simulation result.
Embodiment
Referring to Fig. 1 to Fig. 4,
Embodiment 1：A kind of method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, including such as
Lower step：
A, gold nano triangular plate synthesizes
Using surfactant assisted Reduction method, gold nano triangular plate synthesis is carried out, is specially：
A1, using surfactant cetyl trimethylammonium bromide (CATB) to gold chloride carry out hydro-thermal process, specifically
For：
A11, first by surfactant cetyl trimethylammonium bromide in mass ratio be 1：780-1:790 ratio drop
It is added in distilled water, it is lasting at room temperature to stir until cetyl trimethylammonium bromide is dissolved completely in distilled water；
A12, the chlorauric acid solution addition cetyl trimethylammonium bromide CATB solution by 1mL concentration for 12.5mmol/L
In, chlorauric acid solution is 1 by volume with CATB solution：20 mixing, and continue stir 30-40min, until solution by it is colourless by
Fade to light yellow；
A13, the mixed solution for again obtaining A12 are transferred in 50mL stainless steel water heating kettle, seal and it is placed on 160~
In 180 DEG C of heating furnaces after 6~8h of continuous heating, room temperature is naturally cooled to；
A2, with centrifuge the reaction product that A13 is obtained is centrifuged 5~10min, rotating speed 10000rpm-
12000rpm, and clean precipitation with ultra-pure water；
A3, repeat A2 steps three times, finally obtain gold nano triangular plate particle；
B, the preparation of the encapsulating structure of gold nano triangular plate
B1, using electron beam evaporation technique silicon chip surface sputter a layer thickness be 80nm~120nm metal film；
B2, by metal film concentration be 5 × 1052h is soaked in mol/L 4- nitro thiophenol 4NBT molecule alcoholic solutions,
Then, 5~10min is rinsed with alcohol, ultra-pure water successively, then is dried up with nitrogen, it is ensured that form one layer in metallic film surface
Equally distributed monolayer；
B3, gold nano triangular plate is dissolved in alcoholic solution, the colloidal solution of gold nano triangular plate obtained, by gold nano
The colloidal solution of triangular plate is spin-coated on metal film, and after allowing it to volatilize naturally, obtains the encapsulating structure of gold nano triangular plate；
C, Metal Packaging interior molecules Raman signal is detected
The joint of application scanning probe microscopy and Raman spectroscopy, the encapsulating structure that direct detecting step B makes.
From the Au probe or silver-colored probe that radius of curvature is 10 nanometers to 90 nanometers, and by scanning probe microscopy control system and
Probe is moved to the package position of gold nano triangular plate by optical microscopy imaging system, to encapsulating structure inside 4- nitrobenzene
The Raman signal of thiophenol 4NBT molecules is detected；Raman spectrum detection parameters are：Optical maser wavelength is from 633nm, laser power
It it is 5 times for 10mw, time of integration 5s, integral number of times, slit width is 10 μm, from 1200 grooves/600nm type gratings, is adopted
With business spectrometer (HORIBA iHR550), spectral detection scope is 1000-1700cm-1。
Embodiment 2：A kind of method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, including such as
Lower step：
A, gold nano triangular plate synthesizes
Using surfactant assisted Reduction method, gold nano triangular plate synthesis is carried out, is specially：
A1, using surfactant cetyl trimethylammonium bromide (CATB) to gold chloride carry out hydro-thermal process, specifically
For
A11, it is first specially 1 in mass ratio by surfactant cetyl trimethylammonium bromide：780-1:790 drops
It is added in 20mL distilled water, it is lasting at room temperature to stir until cetyl trimethylammonium bromide is dissolved completely in distilled water；
A12, by 1mL concentration be 13mmol/L chlorauric acid solution add CATB solution in, chlorauric acid solution is molten with CATB
Liquid is 1 by volume：20 mixing, and continue to stir 30-40min, until solution gradually becomes light yellow by colourless；
A13, the mixed solution for again obtaining A12 are transferred in 50mL stainless steel water heating kettle, seal and it is placed on 160~
In 180 DEG C of heating furnaces after 6~8h of continuous heating, room temperature is naturally cooled to；
A2, with centrifuge the reaction product that A13 is obtained is centrifuged 5-10min, rotating speed 10000rpm-
12000rpm, and clean precipitation with ultra-pure water；
A3, repeat A2 steps three times, finally obtain gold nano triangular plate particle；
B, the preparation of the encapsulating structure of gold nano triangular plate
B1, using electron beam evaporation technique silicon chip surface sputter a layer thickness be 80nm~120nm metal film；
B2, by metal film concentration be 5 × 105Soaked in mol/L 4- nitro thiophenols (4NBT) molecule alcoholic solution
2h, then, 5~10min is rinsed with alcohol, ultra-pure water successively, then dried up with nitrogen, it is ensured that form one in metallic film surface
The equally distributed monolayer of layer；
B3, gold nano triangular plate is dissolved in alcoholic solution, the colloidal solution of gold nano triangular plate obtained, by gold nano
The colloidal solution of triangular plate is spin-coated on metal film, and after allowing it to volatilize naturally, obtains the encapsulating structure of gold nano triangular plate；
C, Metal Packaging interior molecules Raman signal is detected
C1, gold nano grain synthesis
C11, it is 1 by volume:2：50 ratio by mass fraction be 20% poly- hexadiene dimethylammonium chloride ammonium salt solution,
Concentration is added in ethylene glycol solution for 1mol/L phosphoric acid solution and stirs 5-10min,
C12, by the chlorauric acid solution that concentration is 0.5mol/L it is again 1 by volume:1000 ratio is added to step C11
In obtained mixed solution, then persistently stir 15-20min；Then heating continues to stir 30- under 180~200 DEG C of constant temperatures
40min, then room temperature persistently stirs 1h until mixed solution cools down；
C13 then again by volume be 1:4000 ratio adds concentration and is 0.5mol/L chlorauric acid solution, and holds
After continuous stirring 20h, it was observed that after having the generation of gold particles suspension in solution, mixed solution is put into 190~200 DEG C of bars again
After heated at constant temperature 1h under part, room temperature cooling 1h, gold nano grain is obtained；
C13 actions are repeated, the bigger and more round shape gold nano grain of size can be obtained；
C2, the gold nano triangle that step B3 preparations will be added drop-wise to after the appropriate absolute alcohol solution dilution of the gold nano grain of preparation
On the encapsulating structure of piece, after volatilizing naturally, the gold nano three for including gold nano grain is found under the auxiliary of light microscope
Cornual plate encapsulating structure, and simultaneously using instrument copper mesh is positioned, telltale mark is carried out to the position；Copper mesh can be bought in Zhong Jing sections
The copper mesh of instrument company.
C3, using the test position demarcated in burnt micro Raman spectra detection platform detecting step C2 is copolymerized, to encapsulation
The Raman signal of 4- nitro thiophenols molecule is detected in structure.During detection, optical maser wavelength is from 633nm, laser power
10mw, time of integration 5s, integral number of times are 5 times, and slit width is 10 μm, from 1200 grooves/600nm type gratings, are used
Business spectrometer (HORIBA iHR550), spectral detection scope are 1000-1700cm-1.Its principle is as shown in Figure 4.
Embodiment 3：Referring to Fig. 5, Fig. 6, Fig. 6 is pinpoint enhanced Raman technology for detection encapsulating structure simulation result, wherein,
(b) it is to have encapsulating structure built-in field distribution map at particle；(c) it is without encapsulating structure built-in field distribution map at particle.
The test data of embodiment 1 and embodiment 2 is analyzed, does not have gold nano grain to deposit on gold nano triangular plate
When Raman signal it is very weak, and the position at peak is in 1084,1175,1336 and 1589cm-1Place, these are all 4- nitro thiophenols
The normalized Raman characteristic peak of molecule.And for there is the position of gold nano grain (curve 1 in Fig. 5) to find Raman signal ratio without Jenner
Several times of the signal enhancing of (curve 2 in Fig. 5) at rice grain, and in 1143,1390 and 1432cm-1Place additionally has more three Ramans
Peak, the i.e. characteristic peak of 4,4'- disulfide groups azobenzene (DMAB).
Test result indicates that：In the position for having gold nano grain, electric field makes metal surface produce substantial amounts of thermoelectron enough,
So as to driving surface catalytic reaction and generate DMAB；It is weaker in the position electric field of no gold nano grain, so corresponding Raman letter
It is number weaker, the catalytic reaction (4NBT catalysis generations DMAB) of molecule can not be realized.In addition, by Fig. 6 simulation result we can be with
It was observed that the opening position of gold nano grain be present, very big electric field is produced between nanostructured gap, its field strength is about nothing
40 times of gold nano grain opening position, this is consistent with laboratory test results.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
In the case of departing from the principle and objective of the present invention a variety of change, modification, replacement and modification can be carried out to these embodiments, this
The scope of invention is limited by claim and its equivalent.
Claims (3)
- A kind of 1. method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, it is characterised in that：Including Following steps：A, gold nano triangular plate synthesizesA1, using surfactant cetyl trimethylammonium bromide to gold chloride carry out hydro-thermal process；A11, first by surfactant cetyl trimethylammonium bromide in mass ratio be 1：780~1:790 ratio is added dropwise It is lasting at room temperature to stir until cetyl trimethylammonium bromide is dissolved completely in distilled water into distilled water；A12, by concentration be 12~13mmol/L chlorauric acid solution add cetyl trimethylammonium bromide solution in, gold chloride Solution is 1 by volume with cetyl trimethylammonium bromide solution:20 ratio mixing, and continue to stir, until solution by It is colourless to gradually become light yellow；A13, the obtained mixed solutions of step A12 are transferred in stainless steel water heating kettle again, seal and be placed on 160~180 DEG C In heating furnace after 6~8h of continuous heating, room temperature is naturally cooled to；A2, with centrifuge the obtained reaction products of step A13 are centrifuged, and precipitation is cleaned with ultra-pure water；A3, repeat A2 steps three times, finally obtain gold nano triangular plate；B, the preparation of the encapsulating structure of gold nano triangular plateB1, using electron beam evaporation technique silicon chip surface sputter a layer thickness be 80nm~120nm metal film；B2, metal film soaked into 2h in 4- nitro thiophenol molecule alcoholic solutions, then, carried out successively with alcohol, ultra-pure water Rinse；Dried up again with nitrogen, it is ensured that form one layer of equally distributed monolayer in metallic film surface；B3, gold nano triangular plate is dissolved in alcoholic solution, the colloidal solution of gold nano triangular plate obtained, by gold nano triangle The colloidal solution of piece is spin-coated on metal film, and allows it to obtain the encapsulating structure of gold nano triangular plate after volatilizing naturally；C, the encapsulating structure interior molecules Raman signal of gold nano triangular plate is detected.
- 2. the method according to claim 1 based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, It is characterized in that：Step C is：From the Au probe or silver-colored probe that radius of curvature is 10 nanometers to 90 nanometers, and probe is moved to gold nano triangular plate Package position, the Raman signal of encapsulating structure inside 4- nitro thiophenol molecules is detected.
- 3. the method according to claim 1 based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal, It is characterized in that：Step C comprises the following steps：C1, gold nano grain synthesisC11, it is 1 by volume:2：50 ratio by mass fraction be 20% poly- hexadiene dimethylammonium chloride ammonium salt solution, concentration It is added in ethylene glycol solution and stirs for 1mol/L phosphoric acid solution；C12, by the chlorauric acid solution that concentration is 0.5mol/L it is again 1 by volume:1000 ratio is added to step C11 and obtained Mixed solution in, then persistently stir；Then heating continues to stir under 180~200 DEG C of constant temperatures, then room temperature persistently stirs Until mixed solution cools down；C13 then again by volume be 1:4000 ratio adds concentration and is 0.5mol/L chlorauric acid solution, and persistently stirs After mixing 20h, it was observed that after having the generation of gold particles suspension in solution, mixed solution is put under the conditions of 190~200 DEG C again After heated at constant temperature 1h, room temperature cooling 1h, gold nano grain is obtained；C2, the envelope by the gold nano grain of preparation with the gold nano triangular plate that step B3 preparations are added drop-wise to after the dilution of absolute alcohol solution On assembling structure, after volatilizing naturally, the gold nano triangular plate envelope comprising gold nano grain is found under the auxiliary of light microscope Assembling structure, and telltale mark is carried out to the position using the instrument that positions simultaneously；C3, using the test position demarcated in burnt micro Raman spectra detection platform detecting step C2 is copolymerized, to encapsulating structure The Raman signal of internal 4- nitro thiophenols molecule is detected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710974599.2A CN107741418B (en) | 2017-10-19 | 2017-10-19 | Method for detecting internal molecular signals of metal package based on needle-tip enhanced Raman technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710974599.2A CN107741418B (en) | 2017-10-19 | 2017-10-19 | Method for detecting internal molecular signals of metal package based on needle-tip enhanced Raman technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107741418A true CN107741418A (en) | 2018-02-27 |
| CN107741418B CN107741418B (en) | 2020-05-22 |
Family
ID=61237037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710974599.2A Active CN107741418B (en) | 2017-10-19 | 2017-10-19 | Method for detecting internal molecular signals of metal package based on needle-tip enhanced Raman technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107741418B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111781191A (en) * | 2020-07-20 | 2020-10-16 | 济南大学 | Composite nano array monitoring 4-nitrothiophenol based on SERS mechanism |
| CN112014308A (en) * | 2020-09-07 | 2020-12-01 | 中国石油大学(华东) | Raman-enhanced electrochemical corrosion cell and control method thereof |
| CN113463020A (en) * | 2021-06-24 | 2021-10-01 | 浙江大学 | Preparation method and spectrum detection method of multiband adjustable multi-scale metamaterial |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080069058A (en) * | 2007-01-22 | 2008-07-25 | 한국생명공학연구원 | Sythesis of gold nanoparticles of various crystal shapes using halide ion |
| WO2013128458A1 (en) * | 2012-03-01 | 2013-09-06 | Ramot At Tel-Aviv University Ltd. | Conductive nanowire films |
| CN104155283A (en) * | 2014-07-17 | 2014-11-19 | 吉林大学 | Method for preparing high-sensitivity surface enhanced raman scattering (SERS) substrate |
| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
-
2017
- 2017-10-19 CN CN201710974599.2A patent/CN107741418B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080069058A (en) * | 2007-01-22 | 2008-07-25 | 한국생명공학연구원 | Sythesis of gold nanoparticles of various crystal shapes using halide ion |
| WO2013128458A1 (en) * | 2012-03-01 | 2013-09-06 | Ramot At Tel-Aviv University Ltd. | Conductive nanowire films |
| CN104155283A (en) * | 2014-07-17 | 2014-11-19 | 吉林大学 | Method for preparing high-sensitivity surface enhanced raman scattering (SERS) substrate |
| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
Non-Patent Citations (2)
| Title |
|---|
| A MECHLER: "The formation of gold nanoparticles using hydroquinone as a reducing agent through a localized pH change upon addition of NaOH to a solution of HAuCl4", 《COLLOIDS AND SURFACES A: PHYSICOCHEMICAL AND ENGINEERING ASPECTS》 * |
| 杨艳娜: "金属纳米片-分子-金属膜三明治体系中的表面等离激元研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111781191A (en) * | 2020-07-20 | 2020-10-16 | 济南大学 | Composite nano array monitoring 4-nitrothiophenol based on SERS mechanism |
| CN112014308A (en) * | 2020-09-07 | 2020-12-01 | 中国石油大学(华东) | Raman-enhanced electrochemical corrosion cell and control method thereof |
| CN113463020A (en) * | 2021-06-24 | 2021-10-01 | 浙江大学 | Preparation method and spectrum detection method of multiband adjustable multi-scale metamaterial |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107741418B (en) | 2020-05-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Maity et al. | Engineering atomically precise copper nanoclusters with aggregation induced emission | |
| Ashenfelter et al. | Fluorescence from molecular silver nanoparticles | |
| Liu et al. | Crystal and solution photoluminescence of MAg24 (SR) 18 (M= Ag/Pd/Pt/Au) nanoclusters and some implications for the photoluminescence mechanisms | |
| CN106885797B (en) | A kind of orientation surface enhancing Raman spectra detection process based on high activity site | |
| Joshi et al. | Tuning properties in silver clusters | |
| Liu et al. | Electrochemiluminescence tuned by electron–hole recombination from symmetry-breaking in wurtzite ZnSe | |
| Zhang et al. | Surface enhanced fluorescence and Raman scattering by gold nanoparticle dimers and trimers | |
| Weber et al. | Super-resolution imaging reveals a difference between SERS and luminescence centroids | |
| Ghosh et al. | Photoluminescence of carbon nanodots: dipole emission centers and electron–phonon coupling | |
| Qian et al. | Conversion of polydisperse Au nanoparticles into monodisperse Au25 nanorods and nanospheres | |
| Crozier et al. | Plasmonics for surface enhanced raman scattering: Nanoantennas for single molecules | |
| Wang et al. | Rapid visualization of latent fingerprints with color‐tunable solid fluorescent carbon dots | |
| Salorinne et al. | Nondestructive size determination of thiol-stabilized gold nanoclusters in solution by diffusion ordered NMR spectroscopy | |
| CN107741418A (en) | Method based on pinpoint enhanced Raman technology for detection Metal Packaging interior molecules signal | |
| Montaño-Priede et al. | Near-electric-field tuned plasmonic Au@ SiO2 and Ag@ SiO2 nanoparticles for efficient utilization in luminescence enhancement and surface-enhanced spectroscopy | |
| Lam et al. | Synthesis, Characterisation and Photophysical Study of Alkynylrhenium (I) Tricarbonyl Diimine Complexes and Their Metal‐Ion Coordination‐Assisted Metallogelation Properties | |
| Damm et al. | Surface enhanced luminescence and Raman scattering from ferroelectrically defined Ag nanopatterned arrays | |
| Soleilhac et al. | Size characterization of glutathione-protected gold nanoclusters in the solid, liquid and gas phases | |
| CN102103086A (en) | Method for detecting single molecule of single silicon nanowire in real time based on surface enhanced raman scattering effect | |
| Wang et al. | Valence-state-engineered electrochemiluminescence from Au nanoclusters | |
| Zhu et al. | Surface-enhanced Raman scattering of 4-mercaptobenzoic acid and hemoglobin adsorbed on self-assembled Ag monolayer films with different shapes | |
| Liu et al. | Water-soluble coumarin oligomer based ultra-sensitive iron ion probe and applications | |
| You et al. | Plasmon-enhanced fluorescence of phosphors using shell-isolated nanoparticles for display technologies | |
| Yang et al. | An ultrasensitive near-infrared satellite SERS sensor: DNA self-assembled gold nanorod/nanospheres structure | |
| Lin et al. | Plasmonic core–shell nanoparticle enhanced spectroscopies for surface analysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |