CN107012428A - A kind of preparation of surface enhanced substrate and the method for demarcation performance - Google Patents
A kind of preparation of surface enhanced substrate and the method for demarcation performance Download PDFInfo
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
The invention discloses a kind of preparation of surface enhanced substrate and the method for demarcation performance, pass through dynamic shadow deposition technique, utilize electron beam evaporation film depositing system, the Silver nanorod array of uniform pitch arrangement is grown on clean sheet glass under the conditions of condition of high vacuum degree, surface enhanced substrate prepared by this method has special Silver nanorod array structure, this causes it to have high sensitivity and superior stability, the surface enhanced substrate multiplicity that this method is produced is high, the SERS Strength Changes of same batch different surfaces enhancing substrate are less than 10%, the SERS Strength Changes of different batches substrate are less than 15%, it is strong compared to other Fabrication Techniques of Nano-Structure controllabilitys, cost is low, multiplicity is high, and it is adapted to large-scale production.
Description
Technical field
The present invention relates to a kind of preparation of surface enhanced substrate and the method for demarcation performance.
Background technology
For many years, people are adjusted to be managed by different methods to features such as nanostructure size, gaps
The SERS active-substrate thought.At present, noble metal sol-gel process, nanometer bead arrangement method, electrochemical erosion method, electronics are utilized
The method of some special preparation nano materials such as beam photoetching process, template and dynamic shadow deposition technique can be met bar
The SERS active-substrate of part, the defect such as its generally existing preparation process is complicated, high, the repeatable difference of cost.
The content of the invention
To solve the above problems, the present invention provides preparation and the method for demarcation performance of a kind of surface enhanced substrate, the party
Surface enhanced substrate prepared by method has special Silver nanorod array structure, and this causes it to have high sensitivity and superior
Stability, the surface enhanced substrate multiplicity that this method is produced is high, and same batch different surfaces strengthen the SERS intensity of substrate
Change is less than 10%, and the SERS Strength Changes of different batches substrate are controllable compared to other Fabrication Techniques of Nano-Structure less than 15%
The strong, cost of property is low, multiplicity is high, and is adapted to large-scale production.
To achieve the above object, the present invention uses following technological means：
The present invention provides a kind of preparation method of surface enhanced substrate, by dynamic shadow deposition technique, utilizes electron beam
Thin evaporated film depositing system, grows the Silver nanorod battle array of uniform pitch arrangement under the conditions of condition of high vacuum degree on clean sheet glass
Row, are concretely comprised the following steps：
(1) sheet glass is cut into the square of 1 × 1cm2 sizes, is soaked in mixing, washing liquid and boils 20min, is taken out
Rinsed three times, be put into after nitrogen drying in settling chamber with secondary deionized water afterwards；
(2) confirm whether the volume of deposition material silver and titanium in crucible accounts for the 70% of crucible volume, confirm film thickness sensor
Life-span whether be more than 30%, check complete machine cooling water circulation it is whether normal, sample stage rotate it is whether normal；
(3) automatic vacuum is selected in the vacuum interface of switch board system operatio, vacuum reaches 5 after about 1.5 hours
After × 10-7Torr, the preparation of substrate is carried out；
(4) material parameter, thickness, speed and selection sensor are set, speed is deposited with 0.2nm/s using an electron gun
Rate at the uniform velocity deposits the thick Ti films of 20nm, then thin with the thick Ag of 0.3nm/s speed deposition 200nm using No. two electron guns
Film.Sample stage angle is then set, sample stage relative steam source incident direction is rotated 86 °, be continuing with No. two electron guns with
0.3nm/s speed at the uniform velocity deposit thickness is 2000nm silver layer.
Further, step (1) the mixing, washing liquid is that the portion rate of the concentrated sulfuric acid and hydrogen peroxide is 8：2.
The present invention also provides a kind of method for demarcating a kind of surface enhanced substrate performance prepared by this method, including by 2uL
Concentration is added drop-wise to for 10-5mol/L BPE solution in a kind of surface enhanced substrate of the inventive method preparation, after natural air drying,
Its SERS signal is detected, same process is repeated and prepares 20 groups of substrates, enhancer has been carried out to randomly selecting 6 in every group of substrate
Test and calculating, to verify the repeatability of substrate.
Further, when detecting SERS signal, the time of integration is 1s, and laser power is 30mW
Beneficial effects of the present invention：
Surface enhanced substrate prepared by this method has special Silver nanorod array structure, and this causes it has highly sensitive
Degree and superior stability, the surface enhanced substrate multiplicity that this method is produced are high, and same batch different surfaces strengthen base
The SERS Strength Changes at bottom are less than 10%, and the SERS Strength Changes of different batches substrate are less than 15%, compared to other nanostructureds
Technology of preparing controllability is strong, cost is low, multiplicity is high, and is adapted to large-scale production.
Brief description of the drawings
Fig. 1 prepares schematic diagram for Silver nanorod array substrate；
Fig. 2 schemes for Silver nanorod array section SEM；
Fig. 3 schemes for the SEM of Silver nanorod array；
Fig. 4 is that Silver nanorod array substrate prepares control flow chart；
Fig. 5 is SERS signal of the BPE solution on Silver nanorod array.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention will be further described.
Embodiment 1：This implementation provides preparation and the method for demarcation performance that the present invention provides a kind of surface enhanced substrate, leads to
Dynamic shadow deposition technique is crossed, using electron beam evaporation film depositing system, in clean sheet glass under the conditions of condition of high vacuum degree
The Silver nanorod array of upper growth uniform pitch arrangement, specifically includes following steps：
(1) sheet glass is cut into the square of 1 × 1cm2 sizes, is soaked in mixing, washing liquid and boils 20min, is taken out
Rinsed three times, be put into after nitrogen drying in settling chamber with secondary deionized water afterwards；
(2) confirm whether the volume of deposition material silver and titanium in crucible accounts for the 70% of crucible volume, confirm film thickness sensor
Life-span whether be more than 30%, check complete machine cooling water circulation it is whether normal, sample stage rotate it is whether normal；
(3) automatic vacuum is selected in the vacuum interface of switch board system operatio, vacuum reaches 5 after about 1.5 hours
After × 10-7Torr, the preparation of substrate is carried out；
(4) material parameter, thickness, speed and selection sensor are set, speed is deposited with 0.2nm/s using an electron gun
Rate at the uniform velocity deposits the thick Ti films of 20nm, then thin with the thick Ag of 0.3nm/s speed deposition 200nm using No. two electron guns
Film.Sample stage angle is then set, sample stage relative steam source incident direction is rotated 86 °, be continuing with No. two electron guns with
0.3nm/s speed at the uniform velocity deposit thickness is 2000nm silver layer.
Step (1) the mixing, washing liquid is that the portion rate of the concentrated sulfuric acid and hydrogen peroxide is 8：2.
Control flow chart prepared by specific Silver nanorod array substrate is as shown in Figure 4.
Dynamic shadow deposition technique mainly relies on traditional physical vapour deposition (PVD), and the atom of the raw material of fusing, which is combined, meets
To the surface of solids of low temperature, extend deposition and the condensation of these atoms, form smooth, flat film；However, in deposition process
Huge inclination angle between middle incident flow and substrate can form shadow effect on surface, and initially these are used as nanostructure growth
Core；Further after deposition, core starts to obtain different anisotropic structures, and final substrate surface formation matter is close, discrete, uniform
Coarse nanostructured, specific works schematic diagram is as shown in Figure 1.
SERS active-substrate prepared by dynamic shadow deposition technique has special Silver nanorod array structure, the silver nanoparticle
Array substrate oblique arrangement, as shown in Figure 2；Its surface uniformity is good, and growth is fine and close, as shown in Figure 3.Pass through Image J softwares
Statistical analysis is carried out to the length of nanometer rods, diameter and angle of inclination, as a result shown, Silver nanorod is relative to sheet glass normal
74.2 ± 1.1 degree of the inclination angle in direction, length about 1030.7 ± 53.4nm, diameter about 66.8 ± 5.2nm, this causes it to have height
Sensitivity and superior stability.
Demarcate substrate performance：
In the substrate that 2uL concentration is added drop-wise to the inventive method preparation for 10-5mol/L BPE solution, the time of integration is
1s, laser power is 30mW, and the Raman spectrum for obtaining BPE is as shown in Figure 5.
The SERS enhancers of silver nanoparticle array substrate are calculated by below equation：
Formula (a) is that the surface-enhanced Raman of the calculation formula of enhancer, i.e. individual molecule strengthens signal intensity and its
Body Raman signal intensity is contrasted；Formula (b) calculates the number of the lower BPE molecules of laser irradiation in Silver nanorod array substrate；Formula (c) is counted
Calculate the molecule sum of the lower BPE powder of laser irradiation.Wherein, ISERSRefer to SERS letter of the BPE solution in silver nanoparticle array substrate
Number intensity, IRamanRefer to the Raman signal of BPE powder under the same conditions, NSERS is total molecular number of tested BPE solution；
SLaserAnd SSubIt is laser facula area and area of base.NRamanRefer to total molecular number in tested BPE powder.BPE powder
Area SPowder, m and M are respectively the quality of BPE powder and BPE molal weight, and NA is Avgadro constant.
By measuring and analyzing, SERS signal intensity of the BPE solution in silver nanoparticle array substrate is 5 × 103, BPE powder
The Raman signal of end under the same conditions is 3.5 × 102.Area of base is 1cm2, the area of BPE powder is 1mm2, BPE powder
Quality and BPE molal weight be respectively 1.5mg and 316mg/mol. Avgadro constants be 6.02 × 1023It is computed,
The SERS enhancers of Silver nanorod array are about 3.4 × 108, relative error is 2.86%, illustrates that substrate meets input detection
The basic demand used.
Repeat same process and be prepared for 20 groups of substrates, enhancer test has been carried out to randomly selecting 6 in every group of substrate
And calculating, to verify the repeatability of substrate.
It is demonstrated experimentally that the SERS substrates multiplicity that this method is produced is high, the SERS intensity of same batch different base becomes
Change less than 10%, the SERS Strength Changes of different batches substrate are less than 15%.Dynamic shadow deposition technique compares other nano junctions
Structure is standby, and technological controllability is strong, cost is low, multiplicity is high, and is adapted to large-scale production.
Claims (4)
1. a kind of preparation method of surface enhanced substrate, it is characterised in that by dynamic shadow deposition technique, steamed using electron beam
Thin film deposition system is sent out, the Silver nanorod battle array of uniform pitch arrangement is grown on clean sheet glass under the conditions of condition of high vacuum degree
Row, are concretely comprised the following steps：
(1) sheet glass is cut into the square of 1 × 1cm2 sizes, is soaked in mixing, washing liquid and boils 20min, is used after taking-up
Secondary deionized water is rinsed three times, is put into after nitrogen drying in settling chamber；
(2) confirm whether the volume of deposition material silver and titanium in crucible accounts for the 70% of crucible volume, confirm the longevity of film thickness sensor
Whether life is more than 30%, checks whether complete machine cooling water circulation is normal, whether normal sample stage rotates；
(3) automatic vacuum is selected in the vacuum interface of switch board system operatio, vacuum reaches 5 × 10- after about 1.5 hours
After 7Torr, the preparation of substrate is carried out；
(4) material parameter, thickness, speed and selection sensor are set, it is even with 0.2nm/s evaporation rates using an electron gun
Ti films thick speed deposition 20nm, then using No. two electron guns with Ag films thick 0.3nm/s speed deposition 200nm.Connect
Setting sample stage angle, sample stage relative steam source incident direction is rotated 86 °, is continuing with No. two electron guns with 0.3nm/
S speed at the uniform velocity deposit thickness is 2000nm silver layer.
2. the preparation method of a kind of surface enhanced substrate according to claim 1, it is characterised in that described in step (1)
Mixing, washing liquid is that the portion rate of the concentrated sulfuric acid and hydrogen peroxide is 8：2.
3. a kind of method for demarcating a kind of surface enhanced substrate performance prepared according to claim 1, it is characterised in that by 2uL
Concentration is added drop-wise in a kind of surface enhanced substrate prepared according to claim 1 for 10-5mol/L BPE solution, natural air drying
Afterwards, its SERS signal is detected, the method for repeating a kind of surface enhanced substrate performance described in claim 1 prepares 20 groups of substrates,
Enhancer test and calculating are carried out to randomly selecting 6 in every group of substrate, to verify the repeatability of substrate.
4. a kind of side for demarcating a kind of surface enhanced substrate performance prepared according to claim 1 according to claim 3
Method, it is characterised in that during detection SERS signal, the time of integration is 1s, and laser power is 30mW.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051424A (en) * | 2017-11-30 | 2018-05-18 | 暨南大学 | SERS substrates, preparation method and applications based on shell surface |
| CN109939750A (en) * | 2017-12-20 | 2019-06-28 | 浙江大学自贡创新中心 | A kind of microchannel plate of functionalization and bimolecular sensors comprising the microchannel plate |
| CN110231326A (en) * | 2018-03-06 | 2019-09-13 | 江苏师范大学 | The residual detection qualitative-and-quantitative method of Amitraz agriculture in a kind of efficiently honey |
| CN110468376A (en) * | 2019-08-27 | 2019-11-19 | 吉林大学 | A kind of carbon-coated Silver nanorod array and its preparation method and application |
| CN111879754A (en) * | 2020-08-05 | 2020-11-03 | 山东寿光检测集团有限公司 | Use method of precious metal nanocone SERS substrate for detecting novel coronavirus |
| CN114990494A (en) * | 2022-05-27 | 2022-09-02 | 江苏师范大学 | Gold nano-layer-coated silver nano-rod array-based surface-enhanced Raman scattering (SERS) substrate with pine cone structure and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108051424A (en) * | 2017-11-30 | 2018-05-18 | 暨南大学 | SERS substrates, preparation method and applications based on shell surface |
| CN109939750A (en) * | 2017-12-20 | 2019-06-28 | 浙江大学自贡创新中心 | A kind of microchannel plate of functionalization and bimolecular sensors comprising the microchannel plate |
| CN110231326A (en) * | 2018-03-06 | 2019-09-13 | 江苏师范大学 | The residual detection qualitative-and-quantitative method of Amitraz agriculture in a kind of efficiently honey |
| CN110468376A (en) * | 2019-08-27 | 2019-11-19 | 吉林大学 | A kind of carbon-coated Silver nanorod array and its preparation method and application |
| CN111879754A (en) * | 2020-08-05 | 2020-11-03 | 山东寿光检测集团有限公司 | Use method of precious metal nanocone SERS substrate for detecting novel coronavirus |
| CN114990494A (en) * | 2022-05-27 | 2022-09-02 | 江苏师范大学 | Gold nano-layer-coated silver nano-rod array-based surface-enhanced Raman scattering (SERS) substrate with pine cone structure and preparation method thereof |
| CN114990494B (en) * | 2022-05-27 | 2024-02-09 | 江苏师范大学 | Pine cone structure SERS substrate with gold nano layer coated with silver nano rod array and preparation method thereof |
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