CN107449768A - Surface enhanced Raman substrate that a kind of silver and silica are mutually inlayed and preparation method thereof - Google Patents
Surface enhanced Raman substrate that a kind of silver and silica are mutually inlayed and preparation method thereof Download PDFInfo
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- CN107449768A CN107449768A CN201710596278.3A CN201710596278A CN107449768A CN 107449768 A CN107449768 A CN 107449768A CN 201710596278 A CN201710596278 A CN 201710596278A CN 107449768 A CN107449768 A CN 107449768A
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- 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
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Abstract
Surface enhanced Raman substrate that a kind of silver and silica are mutually inlayed and preparation method thereof, belongs to trace materials detection technique field.The surface enhanced Raman substrate is made up of nanometer stick array, and the silver in the nanometer stick array exists with nano level particle form, and the silicon oxide layer of amorphous is uniformly coated on Argent grain surface, forms the structure that silver and silica are mutually inlayed.Its preparation method is to use twin-cathode ray beam deposition system, using tilting growing method, deposition of silver and silica simultaneously on substrate, obtains the surface enhanced Raman substrate for the nanometer stick array that silver and silica are mutually inlayed.The present invention can realize in atmosphere storage for a long time and SERS loss of activity is less；Structural stability of the substrate in high temperature can be significantly improved simultaneously；It is cost-effective to a certain extent on the premise of SERS Basal Activities are maintained, and used beneficial to scale.
Description
Technical field
The invention belongs to trace materials detection technique field, more particularly to a kind of there is silver and the mutual mosaic texture of silica
Nanometer stick array surface-enhanced Raman (SERS) substrate and preparation method thereof.
Background technology
SERS effects have the advantages that non-destructive is widely used each because of its convenient, high sensitivity of detection
In individual field, such as environment measuring, food safety detection, medical diagnosis on disease etc..At present, the preparation method of SERS substrates in the prior art
Mainly have：Sol-gel process, electrochemical corrosion/sedimentation, masterplate method etc..In general, process above there may be preparation
Complex process, the substrate prepared are difficult to preferably preserve, are easily introduced impurity, are difficult to the deficiencies of large area deposition.
On the other hand, nano silver-group bottom was applied to by more due to the advantages that its enhancing effect is preferable and price is suitable
SERS substrates, but the shortcomings that some are serious be present in it, such as：(oxidation or vulcanization occurs) apt to deteriorate in atmosphere, seriously
Influence the preservation life-span of substrate；Due to nano metal club shaped structure non-refractory, therefore it is not particularly suited for detecting high temperature determinand
Matter, simultaneously as the cost that noble metal is high, also limits its extensive use to a certain extent.In order to improve its deficiency, tradition
Way typically by the techniques such as electrochemical reaction, ald prepare complete silver nanoparticle substrate on continue to superscribe
One layer of inert material, but the shortcomings of complex process, production cost increase be present in this.
The content of the invention
It is an object of the invention to provide a kind of new nanometer stick array table with silver and the mutual mosaic texture of silica
Face enhancing Raman substrate and preparation method thereof, make its can not only keep higher detection sensitivity, excellent heat endurance and when
Between stability, while the more usage amount for saving noble silver.
In order to achieve the above object, the present invention adopts the technical scheme that：
The SERS substrates that a kind of silver and silica are mutually inlayed, it is characterised in that：The substrate is made up of nanometer stick array, should
Silver in nanometer stick array exists with nano level particle form, and the silicon oxide layer of amorphous is uniformly coated on Argent grain surface,
Form the structure that silver and silica are mutually inlayed.
In above-mentioned technical proposal, Argent grain is discrete in described nanometer rods, and the diameter of Argent grain is in 3-8nm.
A kind of preparation method for the surface enhanced Raman substrate that silver and silica provided by the invention are mutually inlayed, its feature exist
Comprise the following steps in this method：
1) substrate of single-sided polishing is immersed in cleaning agent, is cleared up and carry out drying process, be then placed within substrate
On platform；
2) use twin-cathode ray beam deposition system, in the system two evaporation source centre distances controls utilize inclination in 3-6cm
Growing method, set electron beam incident angle degree between 86 ° -88 °, on substrate simultaneously deposition of silver and silica；
3) control silver sedimentation rate beThe rotary speed of chip bench is 0-100r/s, the speed of deposition of silver
The speed ratio of rate and cvd silicon oxide is 5:1-1:1, obtain the surface being made up of the nanometer stick array that silver and silica are mutually inlayed
Strengthen Raman substrate.
Preferably, the sedimentation time of silver and silica is 8min-12min in step 3).
Preferably, the substrate described in step 1) uses silicon chip, quartz plate or optical glass.
The present invention has the technique effect of advantages below and high-lighting：1. silver and silica prepared by the present invention are uniformly mutually inlayed
Embedding nanometer stick array can realize in atmosphere storage (at least one moon) for a long time and SERS loss of activity is less.2. the present invention
The nanometer stick array substrate that the silver and silica of preparation are uniformly mutually inlayed at 400 DEG C, do not send out yet by the nanostructured morphologies of substrate
Raw significant change, and the nanometer stick array of fine silver its nanostructured at 100 DEG C or so changes (see Fig. 4), shows
The invention can significantly improve structural stability of the substrate in high temperature.3. silver and silica prepared by the present invention are uniformly mutually inlayed
Nanometer stick array substrate on the premise of SERS Basal Activities are maintained, can be cost-effective to a certain extent, and beneficial to rule
Modelling uses.
Brief description of the drawings
Fig. 1 is the device structure schematic diagram of the preparation silver that the present invention uses and silica composite nanorod SERS substrates.
In Fig. 1, the evaporation sources of 1- first；The evaporation sources of 2- first；3- baffle plates；The crystal-vibration-chips of 4- first；The crystal-vibration-chips of 5- second；6- bases
Piece platform.
Fig. 2A -2D are respectively the cross section structure ESEM photograph of silver prepared by embodiment 1-4 and silica composite nanorod
Piece.
Fig. 3 A, 3B are respectively the cross section structure transmission of silver prepared by embodiment 3 and embodiment 4 and silica composite nanorod
Electromicroscopic photograph.
Fig. 4 is the silver and silica composite base obtained using luminous power thermal analyzer to the embodiment of the present invention 2 and embodiment 3
Obtained light reflectivity variation with temperature relation is tested at bottom.
Fig. 5 is silver prepared by 1-4 of the embodiment of the present invention and silica composite nanorod SERS substrates to 10 μM of rhodamine
The SERS figures of 6G (R6G) aqueous solution.
Fig. 6 is that silver prepared by the embodiment of the present invention 3 and silica composite nanorod SERS substrates placed 20 days to 10 μ
The SERS figures of the M R6G aqueous solution.
Embodiment
The present invention will be further explained with reference to the accompanying drawings and examples.
Fig. 1 is the device structure schematic diagram of the preparation silver that the present invention uses and silica composite nanorod SERS substrates, should
Equipment mainly includes the first evaporation source 1, the second evaporation source 2, baffle plate 3, the first crystal-vibration-chip 4 for detecting the first evaporation source and detection the
The second crystal-vibration-chip 5 and chip bench 6 of two evaporation sources.
Fig. 2A-Fig. 2 C are the scanned photograph of silver prepared by the present invention and silica composite nanorod SERS substrates.
Fig. 3 A-3B are silver prepared by the present invention and the transmission photo of silica composite nanorod SERS substrates.
Fig. 4 is the light reflectivity variation with temperature pass of silver prepared by the present invention and silica composite nanorod SERS substrates
System, the temperature of pattern change occurs by substrate can be obtained in figure.
Fig. 5 is silver prepared by the present invention and the SERS figures of silica composite nanorod SERS substrates, is to the sensitive of substrate
The investigation of degree.
Fig. 6 is the SERS figures that silver prepared by the present invention and silica composite nanorod SERS substrates place a period of time, is
Investigation to the stability of substrate.
The SERS substrates that a kind of silver and silica provided by the invention are mutually inlayed are made up of nanometer stick array, the nanometer rods
Silver in array exists with nano level particle form, and the silicon oxide layer of amorphous is uniformly coated on Argent grain surface, forms silver
The structure mutually inlayed with silica, wherein, Argent grain is discrete in nanometer rods, the general diameter of Argent grain in 3-8nm (such as
Shown in Fig. 3 A, 3B).
A kind of preparation method for the SERS substrates that silver and silica provided by the invention are mutually inlayed, it specifically includes following step
Suddenly：
1) substrate (silicon chip, quartz plate or optical glass etc.) of single-sided polishing is immersed in cleaning agent, carries out cleaning and go forward side by side
Row drying process；It is then placed within chip bench；
2) use twin-cathode ray beam deposition system, in the system two evaporation source centre distances controls utilize inclination in 3-6cm
Growing method, the incident angle of electron beam is set between 86 ° -88 °, in substrate simultaneously deposition of silver and silica；
3) speed of setting deposition of silver isThe speed of deposition of silver：Speed=5 of cvd silicon oxide:1-1:
1, the rotary speed of chip bench is 0-100r/s, obtains the nanometer stick array that silver and silica are mutually inlayed.Twin-cathode ray beam is deposited altogether
During, the evaporation rate in two sources independently can be monitored and regulated and controled, and can regulate and control silver by changing the evaporation rate of the two
With the component ratio and microscopic appearance of silica.
Embodiment 1
1) silicon chip of single-sided polishing is immersed in cleaning agent, carrying out ultrasonic wave to silicon chip cleans 30 minutes, then spend from
Processing is dried in the silicon chip that sub- water is rinsed after ultrasonic wave cleaning, then the silicon chip to rinsing well.
2) Argent grain and silicon oxide particle are respectively placed in 4cm two crucibles, it is real using growing method is tilted
The co-deposition growth of existing silver and silica on silicon chip.
3) incident angle for setting electron beam is 88 °, and chip bench rotary speed is 100r/s.
4) set respectively silver deposition velocity beThe deposition velocity of silica isSedimentation time is 600s, is obtained
To the uniform one-dimensional silver of growth and silica composite nanorod of certain length (ESEM result is shown in Fig. 2A).
5) taken out after the silver and silica composite substrate of preparation being immersed in into 10 μM of R6G solution 30min, be placed in hand-held
Raman detector tested, laser power 150mW, time of integration 10s, obtained SERS collection of illustrative plates are shown in Fig. 5.
Embodiment 2
1) quartz plate of single-sided polishing is immersed in cleaning agent, carrying out ultrasonic wave to quartz plate cleans 30 minutes, Ran Houyong
Processing is dried in quartz plate after the cleaning of deionized water rinsing ultrasonic wave, then the quartz plate to rinsing well；
2) silver and silica are respectively placed in 4cm two crucibles, silver and oxygen is realized using growing method is tilted
Co-deposition growth of the SiClx on quartz plate；
3) incident angle for setting electron beam is 87 °, and it is 30r/s to control chip bench rotary speed；
4) set respectively silver deposition velocity beThe deposition velocity of silica isSedimentation time is 600s, is obtained
To the uniform one-dimensional silver of growth and silica composite nanorod of certain length (ESEM result is shown in Fig. 2 B)；
5) taken out after the silver and silica composite substrate of preparation being immersed in into 10 μM of R6G solution 30min, be placed in hand-held
Raman detector tested, laser power 150mW, time of integration 10s, obtained SERS collection of illustrative plates are shown in Fig. 5.
6) silver and silica composite substrate prepared are placed in OPA-1200 type Analysis of optical power instrument, sample is from 50 DEG C
400 DEG C are begun heat to, the rate of heat addition is 60 DEG C/min, obtained substrate reflectivity variation with temperature relation such as Fig. 4.From figure
In as can be seen that the reflectivity of substrate is little in 50-400 DEG C of change, illustrate that the pattern of substrate does not change, and the base of fine silver
Bottom reflectivity at about 100 DEG C changes.
7) silver and silica composite substrate of preparation are placed 1 day, 10 days and 20 days in atmosphere, respectively will in atmosphere
The SERS substrates for placing different time are immersed in 30min in 10 μM of R6G solution, take out, and are placed in the Raman detector of hand-held
Tested, laser power 150mW, time of integration 10s.Obtained SERS collection of illustrative plates is shown in Fig. 6.
Embodiment 3
1) silicon chip of single-sided polishing is immersed in cleaning agent, carrying out ultrasonic wave to silicon chip cleans 30 minutes, then spend from
Processing is dried in the silicon chip that sub- water is rinsed after ultrasonic wave cleaning, then the silicon chip to rinsing well.
2) silver and silica are respectively placed in 4cm two crucibles, silver and oxygen is realized using growing method is tilted
Co-deposition growth of the SiClx on silicon chip.
3) incident angle for setting electron beam is 87 °, and chip bench rotary speed is 30r/s.
4) set respectively silver deposition velocity beThe deposition velocity of silica isSedimentation time is 480s, is obtained
To the uniform one-dimensional silver of growth and silica composite nanorod of certain length (ESEM result is shown in Fig. 2 C).
5) silver and the transmissioning electric mirror test result of silica composite substrate prepared as shown in Figure 3A, can be seen that by Fig. 3 A
Silver nano-grain is evenly distributed in silica matrices, and the diameter of Argent grain is about 3nm-8nm.
6) silver and silica composite substrate prepared are placed in OPA-1200 type Analysis of optical power instrument, sample is from 50 DEG C
400 DEG C are begun heat to, the rate of heat addition is 20 DEG C/min, obtained substrate reflectivity variation with temperature relation such as Fig. 4.From figure
In as can be seen that the reflectivity of substrate is little in 50-400 DEG C of change, illustrate that the pattern of substrate does not change, and the base of fine silver
Bottom reflectivity at about 100 DEG C changes.
7) taken out after the silver and silica composite substrate of preparation being immersed in into 10 μM of R6G solution 30min, be placed in hand-held
Raman detector tested, laser power 150mW, time of integration 10s, obtained SERS collection of illustrative plates are shown in Fig. 5.
Embodiment 4
1) silicon chip of single-sided polishing is immersed in cleaning agent, carrying out ultrasonic wave to silicon chip cleans 30 minutes, then spend from
Processing is dried in the silicon chip that sub- water is rinsed after ultrasonic wave cleaning, then the silicon chip to rinsing well.
2) silver and silica are respectively placed in 4cm two crucibles, silver and oxygen is realized using growing method is tilted
Co-deposition growth of the SiClx on silicon chip.
3) incident angle for setting electron beam is 86 °, and about 20 DEG C of the temperature of chip bench is controlled using liquid nitrogen.
4) set respectively silver deposition velocity beThe deposition velocity of silica isSedimentation time is 12min,
Obtain the uniform one-dimensional silver of growth and silica composite nanorod of certain length (ESEM result is shown in Fig. 2 D).
5) silver and the transmissioning electric mirror test result of silica composite substrate prepared as shown in Figure 3 B, can be seen that by Fig. 3 B
Silver nano-grain is evenly distributed in silica matrices, and the diameter of Argent grain is about 3nm-8nm.
6) taken out after the silver and silica composite substrate of preparation being immersed in into 10 μM of R6G solution 30min, be placed in hand-held
Raman detector tested, laser power 150mW, time of integration 20s, obtained SERS collection of illustrative plates are shown in Fig. 5.
Claims (5)
- A kind of 1. surface enhanced Raman substrate that silver and silica are mutually inlayed, it is characterised in that：The surface enhanced Raman substrate It is made up of nanometer stick array, the silver in the nanometer stick array exists with nano level particle form, and the silicon oxide layer of amorphous is uniform Ground is coated on Argent grain surface, forms the structure that silver and silica are mutually inlayed.
- 2. the surface enhanced Raman substrate that a kind of silver according to claim 1 and silica are mutually inlayed, it is characterised in that institute Argent grain is discrete in the nanometer stick array stated, a diameter of 3-8nm of Argent grain.
- 3. the preparation method for the surface enhanced Raman substrate that a kind of silver as claimed in claim 1 or 2 and silica are mutually inlayed, its It is characterised by that this method comprises the following steps：1) substrate of single-sided polishing is immersed in cleaning agent, is cleared up and carry out drying process, be then placed within chip bench；2) use twin-cathode ray beam deposition system, in the system two evaporation source centre distances controls utilize and tilt growth in 3-6cm Method, set electron beam incident angle degree between 86 ° -88 °, on substrate simultaneously deposition of silver and silica；3) control silver sedimentation rate beThe rotary speed of chip bench is 0-100r/s, and the speed of deposition of silver is with sinking The speed ratio of product silica is 5:1-1:1, the surface enhanced for obtaining being made up of the nanometer stick array that silver and silica are mutually inlayed is drawn Graceful substrate.
- 4. the preparation method for the surface enhanced Raman substrate that a kind of silver according to claim 3 and silica are mutually inlayed, its It is characterised by, the sedimentation time of silver and silica is 8min-12min in step 3).
- 5. the preparation method for the surface enhanced Raman substrate that a kind of silver according to claim 3 and silica are mutually inlayed, its It is characterised by, the substrate described in step 1) uses silicon chip, quartz plate or optical glass.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109898057A (en) * | 2019-03-25 | 2019-06-18 | 中国科学院物理研究所 | Glassy metal film, preparation method and application with surface Raman enhancement effect |
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| US20130293884A1 (en) * | 2012-05-01 | 2013-11-07 | University Of Maryland, College Park | Nanoparticle array with tunable nanoparticle size and separation |
| CN104280376A (en) * | 2013-07-10 | 2015-01-14 | 任贻均 | Surface enhanced Raman spectroscopy (SERS) sensing substrate and manufacturing method thereof |
| CN104404512A (en) * | 2014-10-10 | 2015-03-11 | 清华大学 | High-stability recyclable surface-enhanced Raman substrate and preparation method |
| CN104692827A (en) * | 2015-02-02 | 2015-06-10 | 华南师范大学 | Preparation method of Ag-SiO2-Ag nanosphere array |
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- 2017-07-20 CN CN201710596278.3A patent/CN107449768B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130293884A1 (en) * | 2012-05-01 | 2013-11-07 | University Of Maryland, College Park | Nanoparticle array with tunable nanoparticle size and separation |
| CN104280376A (en) * | 2013-07-10 | 2015-01-14 | 任贻均 | Surface enhanced Raman spectroscopy (SERS) sensing substrate and manufacturing method thereof |
| CN104404512A (en) * | 2014-10-10 | 2015-03-11 | 清华大学 | High-stability recyclable surface-enhanced Raman substrate and preparation method |
| CN104692827A (en) * | 2015-02-02 | 2015-06-10 | 华南师范大学 | Preparation method of Ag-SiO2-Ag nanosphere array |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109898057A (en) * | 2019-03-25 | 2019-06-18 | 中国科学院物理研究所 | Glassy metal film, preparation method and application with surface Raman enhancement effect |
| CN109898057B (en) * | 2019-03-25 | 2020-12-29 | 中国科学院物理研究所 | Metallic glass film with surface Raman enhancement effect, preparation method and application thereof |
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