CN103600082B - Silver nano-particle layer and preparation method thereof and application - Google Patents
Silver nano-particle layer and preparation method thereof and application Download PDFInfo
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- CN103600082B CN103600082B CN201310610671.5A CN201310610671A CN103600082B CN 103600082 B CN103600082 B CN 103600082B CN 201310610671 A CN201310610671 A CN 201310610671A CN 103600082 B CN103600082 B CN 103600082B
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 73
- 239000004332 silver Substances 0.000 title claims abstract description 73
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000012528 membrane Substances 0.000 claims abstract description 54
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract 1
- 101000674278 Homo sapiens Serine-tRNA ligase, cytoplasmic Proteins 0.000 description 22
- 101000674040 Homo sapiens Serine-tRNA ligase, mitochondrial Proteins 0.000 description 22
- 102100040516 Serine-tRNA ligase, cytoplasmic Human genes 0.000 description 22
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 description 13
- 238000001069 Raman spectroscopy Methods 0.000 description 12
- 229920000877 Melamine resin Polymers 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 150000003378 silver Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000001530 Raman microscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- -1 argon ion Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of Silver nano-particle layer and preparation method thereof and application.The method, comprises the steps: 1) the silver nanoparticle colloidal sol be made up of silver nano-grain and water is carried out centrifugal, after collecting precipitation washes with water, ultrasonic disperse, in water, obtains the silver nanoparticle colloidal sol after centrifugal enrichment again; 2) the silver nanoparticle colloidal sol filter membrane after step 1) gained centrifugal enrichment is filtered, described filter membrane forms Silver nano-particle layer, dry, obtain the Silver nano-particle layer of load on described filter membrane.The filter membrane substrate utilizing method of the present invention to prepare has excellent SERS performance and comprises homogeneity, repeatability, high sensitivity and long-term stability; In preparation method provided by the invention, raw material is inexpensive, technique is simple, effectively reduces product cost, is suitable for industrialization, has very high application prospect and practical value.
Description
Technical field
The present invention relates to a kind of Silver nano-particle layer and preparation method thereof and application.
Background technology
The preparation of SERS (referred to as SERS) substrate is mainly divided into two kinds: physical method and chemical method.Substrate prepared by physical method strictly can control the size of parameter as base particle of substrate, shape, distribution, can well strengthen the uniformity of Raman scattering signal and repeatability by control surface, but all too complicated and high cost of the equipment needed for these class methods and technology; Chemical method is then obviously simple, and convenient, cost is low, and the substrate that usually prepared by these class methods has stronger strengthening the property, but the usual reappearance of these class methods and homogeneity poor.Current most of process is also difficult to the advantage simultaneously with these two class methods, and most method all cannot have the longer shelf-life under the high prerequisite of strengthening the property of guarantee, can reach the effect of this for SERS technology practical application.
Summary of the invention
The object of this invention is to provide a kind of Silver nano-particle layer and preparation method thereof and application.
The method preparing Silver nano-particle layer provided by the invention, comprises the steps:
1) undertaken centrifugal by the silver nanoparticle colloidal sol be made up of silver nano-grain and water, after collecting precipitation washes with water, ultrasonic disperse, in water, obtains the silver nanoparticle colloidal sol after centrifugal enrichment again;
2) the silver nanoparticle colloidal sol filter membrane after step 1) gained centrifugal enrichment is filtered, described filter membrane forms Silver nano-particle layer, dry, obtain the Silver nano-particle layer of load on described filter membrane.
In the step 1) of said method, in the silver nanoparticle colloidal sol be made up of silver nano-grain and water, the mass ratio of silver nano-grain and water is 10-100mg:200mL, is specially 50mg:200mL;
The particle diameter 20-120nm of silver nano-grain, concrete 50-100nm;
In silver nanoparticle colloidal sol after described centrifugal enrichment, the mass ratio of silver nano-grain and water is 0.1-0.5:100, is specially 0.125:100.
In centrifugation step, centrifugal rotational speed is 5000-12000rmp, is specially 12000rpm; Centrifugal force is 1816-10464g, is specially 10464g; Time is 5-20min, is specially 10min;
In described ultrasonic step, the time is 5-20 minute, is specially 10 minutes; Ultrasonic power is 30-100W, is specially 30W.
Described step 2) in, the aperture of filter membrane used is less than 3 times of described silver nano-grain particle diameter; The aperture of filter membrane used is specially 2.2 times of described silver nano-grain particle diameter.
In filtration step, filtering rate is 0.25 ~ 1ml/min, is specially 0.5ml/min;
Filtration pressure is 2-10.3bar, is specially 5.2bar;
In drying steps, temperature is 25-40 DEG C, is specially 30 DEG C; Time is 10-30min, is specially 15min.
In addition, the Silver nano-particle layer prepared according to the method described above, and the application using this Silver nano-particle layer as substrate in surface-enhanced raman scattering, also belong to protection scope of the present invention.
The present invention utilizes a kind of simple filter method, obtain fine and close, homogeneous, can repeat, excellent stability, to a certain extent quantitatively and the surface enhanced Raman scattering substrate of practical application, prior art can be solved and prepare the problem that ubiquitous sensitivity in SERS substrate is low, complicated process of preparation, cost are high, homogeneity is poor, the shelf-life is short.The method utilizes to filter to be separated with water by the nano particle in noble metal nano colloidal sol, the nano particle be adsorbed on filter membrane evenly, is densely combined by the high pressure produced in filter process, thus obtains uniform compact repeatably surface enhanced Raman scattering substrate.Wherein applied filter sizes and prepared nanoparticle size extremely important, corresponding filter membrane to be selected when selecting different size nano particle to filter, forming the object of nano-grain array to reach at filter membrane surface.In concrete preparation technology, the nano particle of different size and the filter membrane of respective aperture can be selected to mate different excitation wavelengths and applied environment, to strengthen the application of SERS technology.
Utilize the method gained surface enhanced Raman scattering substrate to have splendid repeatability, its relative standard deviation reaches 10%; Signal homogeneity reaches 9%; Enhancer can reach 10 simultaneously
8the order of magnitude, can reach 10 respectively to the detectability of rhodamine 6G and melamine
-14m and 10
-8the M order of magnitude; The shelf-life of prepared substrate is extremely long, can reach two months.In preparation method provided by the invention, raw material is inexpensive, technique is simple, effectively reduces product cost, is suitable for industrialization, has very high application prospect and practical value.
Accompanying drawing explanation
Fig. 1 is the FE-SEM figure of filter membrane substrate prepared by embodiment 1.
Fig. 2 is that the Raman mapping of filter membrane substrate prepared by embodiment 1 schemes.
Fig. 3 is that filter membrane substrate prepared by embodiment 1 is schemed the SERS of rhodamine 6G detectability.
Fig. 4 is that filter membrane substrate prepared by embodiment 1 is schemed the SERS of melamine detectability.
Fig. 5 is the SERS figure of different time in the filter membrane substrate three months prepared of embodiment 1.
Fig. 6 is the XPS figure of different time in the filter membrane substrate three months prepared of embodiment 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.Described raw material all can obtain from open commercial sources if no special instructions.
Following embodiment silver nanoparticle colloidal sol used is all prepared as follows and obtains:
Get 100mg and there is the weak reductant glucose of aldehyde radical and 200mg protective agent PVP is dissolved in 150mL deionized water, ultrasonicly it is made to dissolve completely, after the membrane filtration process twice in 450nm aperture, under stirring at room temperature state, adding the 1MNaOH aqueous solution 180 μ L to the pH value of system is after 9, add Jin Jing's kind (concentration that Jin Jing plants is 65 μ g/mL) that 200 μ L particle diameters are 5nm again, the silver ammino solution 50mL that concentration is 1mg/mL is added again with the drop rate of 0.5mL/min, the silver-colored ammonia react of planting based on Jin Jing is carried out at 20 DEG C, react complete after 100 minutes, obtain the colloidal sol containing particle diameter 100nm silver nano-grain, wherein, the mass ratio of silver nano-grain and water is 1.25mg:5mL.
Embodiment 1,
1) by 5mL by particle diameter be the silver nanoparticle colloidal sol that forms of the silver nano-grain 1.25mg of 100nm and water 5mL rotating speed be 12000rmp, centrifugal force be the condition of 10464g under centrifugal 10min, to remove the supernatant that unreacted surfactant is contained on upper strata, collecting precipitation after spending deionized water 2 times again under power is the condition of 30W ultrasonic 10min be scattered in 1mL deionized water, obtain the silver nanoparticle colloidal sol after centrifugal enrichment, the mass ratio of silver nano-grain and water is 0.125:100;
2) the silver nanoparticle colloidal sol after step 1) gained centrifugal enrichment is loaded in the syringe of 5mL capacity, filter with the filter membrane in 0.22 μm of aperture, filtering rate is 0.5mL/min, filtration pressure is 5.2bar, on filter membrane, Silver nano-particle layer is formed after filtration, the film be attached on miillpore filter is placed on dry 15min in the baking oven of 30 DEG C, obtains the Silver nano-particle layer of load on filter membrane (also i.e. filter membrane substrate).
The morphology characterization of this Silver nano-particle layer carries out (voltage 10kV) on German LEO-1530 type field emission scanning electron microscope (FE-SEM), and its FE-SEM image as shown in Figure 1.
As shown in Figure 1, after filtering, the hole on filter membrane is covered by the silver nano-grain of size uniformity.The color of filter membrane also becomes the bright silver with metallic luster from white.Filtering under the high pressure that produces, nearly all silver nano-grain all to have got lodged in the hole of filter membrane itself thus has defined one deck densification, homogeneous, repeatably silver nano-grain array.This nano-array not only achieves the repeatability of preparation condition, simultaneously due to its three-dimensional fine and close array structure, defines more " focus ", which ensure that the excellent SERS of this substrate strengthens the property in same area.
The SERS signal homogeneity of this embodiment gained filter membrane substrate is evaluated:
With rhodamine 6G (R6G) as probe molecule, be 1 × 10 by 100 μ L concentration
-5the R6G solution of mol/l joins in 900 μ l silver nanoparticle colloidal sols, with membrane filtration after mix and blend 1h, then uses Raman spectrum (HoribaJYHR800 Raman spectrometer) to investigate the SERS performance of this Silver nano-particle layer substrate.Raman spectrum light source adopts 514nm argon ion laser, and power is 0.05mW, and camera lens is 50 times of telephoto lenses.
Table 1 is that Silver nano-particle layer substrate repeats ten batches under identical preparation and test condition, and test gained R6G is at 614cm
-1raman peak area contrast.
The R6G of table 1, the substrate of Silver nano-particle layer filter membrane is at 614cm
-1raman peak area contrast
| Batch | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Peak area | 25693 | 31430 | 28271 | 27990 | 31665 | 28165 | 24647 | 27477 | 22876 | 24533 |
As seen from table, the repeatable relative standard deviation of ten different batches filter membranes substrate is approximately 10%.Illustrate that filter membrane substrate has very excellent SERS test repeatability.
Fig. 2 is that the R6G of filter membrane substrate mensuration is at 614cm
-1the Raman Surface scan mapping image at place, is of a size of 50 × 50 μm
2, step-length is 2 μm, and the little figure in Fig. 2 is the normal distribution of SERS intensity.
As seen from the figure, in whole scanning area, SERS signal intensity is minimum.According to Gauss curve fitting, the relative standard deviation of SERS intensity reaches 9%.Raman Surface scan is a kind of mode of stricter inspection substrate homogeneity, this also illustrates homogeneous the strengthening the property of filter membrane substrate excellence.
Fig. 3 is the R6G detectability mensuration figure carried out in filter membrane substrate.Being respectively concentration is from top to bottom 1 × 10
-6, 1 × 10
-8, 1 × 10
-10, 1 × 10
-12, 1 × 10
-13, 5 × 10
-14the R6G of M, and the filter membrane substrate of blank.
As seen from the figure, compared with the Raman spectrogram of blank filter membrane, 5 × 10
-14613 can be positioned at, 1363,1509 by the clear R6G of seeing, 1572 and 1650cm in the Raman spectrogram of M
-1raman peaks.Which illustrate this three-dimensional fine and close filter membrane substrate and have extraordinary strengthening the property, the sensitivity that SERS detects can be improved well.
Fig. 4 is melamine detectability mensuration figure in filter membrane substrate.Being respectively concentration is from top to bottom 1 × 10
-3, 1 × 10
-4, 1 × 10
-5, 1 × 10
-6, 1 × 10
-7, 1 × 10
-8the Melamine of M, and the filter membrane substrate of blank.
As seen from the figure, compared with the Raman spectrogram of blank filter membrane, 1 × 10
-8clearly can see that melamine is positioned at 686cm in the Raman spectrogram of M
-1raman peaks.This illustrates that filter membrane substrate is except the sensitivity had conventional probe molecule in SERS detection, also has extraordinary universality to the material in practical application.
Fig. 5 be filter membrane substrate in three months different time sections measure 10
-6the R6G Raman spectrum of M.
As seen from the figure, filter membrane maintains very high SERS performance within the time of the first two months, is respectively the Raman spectrum of the R6G that same filter membrane substrate gathered at the 1st, 5,10,20,30,45,60 day from top to bottom.In the time of the first two months substrate in intensity almost without any change.After two months, obviously reducing appears in the SERS intensity of filter membrane, but still has SERS activity.This illustrates that filter membrane is very low to the susceptibility of time, has the shelf-life all more excellent than existing most of SERS substrate.
Fig. 6 is the XPS spectrum figure of the different time corresponding with filter membrane substrate in Fig. 5.Be respectively fresh filter membrane substrate and placed the filter membrane substrate after 80 days XPS contrast.
As seen from the figure, the silver element valence state of filter membrane substrate surface there occurs and obviously changes, and this demonstrate that the change of substrate SERS performance is caused by the oxidation of silver surface.
Claims (12)
1. prepare a method for Silver nano-particle layer, comprise the steps:
1) undertaken centrifugal by the silver nanoparticle colloidal sol be made up of silver nano-grain and water, after collecting precipitation washes with water, ultrasonic disperse, in water, obtains the silver nanoparticle colloidal sol after centrifugal enrichment again;
Described step 1) in, in the silver nanoparticle colloidal sol be made up of silver nano-grain and water, the mass ratio of silver nano-grain and water is 10-100mg:200mL;
The particle diameter of silver nano-grain is 20-120nm;
In silver nanoparticle colloidal sol after described centrifugal enrichment, the mass ratio of silver nano-grain and water is 0.1-0.5:100;
2) by step 1) silver nanoparticle colloidal sol filter membrane after gained centrifugal enrichment filters, and described filter membrane forms Silver nano-particle layer, dry, obtains the Silver nano-particle layer of load on described filter membrane.
2. method according to claim 1, is characterized in that: described step 1) in, in the silver nanoparticle colloidal sol be made up of silver nano-grain and water, the mass ratio of silver nano-grain and water is 50mg:200mL;
The particle diameter of silver nano-grain is 50-100nm;
In silver nanoparticle colloidal sol after described centrifugal enrichment, the mass ratio of silver nano-grain and water is 0.125:100.
3. method according to claim 1, is characterized in that: described step 1) in centrifugation step, centrifugal rotational speed is 5000-12000rmp;
Centrifugal force is 1816-10464g; Time is 5-20min;
In described ultrasonic step, the time is 5-20 minute;
Ultrasonic power is 30-100W.
4. method according to claim 3, is characterized in that: described step 1) in centrifugation step, centrifugal rotational speed is 12000rmp;
Centrifugal force is 10464g; Time is 10min;
In described ultrasonic step, the time is 10 minutes;
Ultrasonic power is 30W.
5. method according to claim 1, is characterized in that: described step 2) in, the aperture of filter membrane used is less than 3 times of described silver nano-grain particle diameter.
6. method according to claim 5, is characterized in that: the aperture of filter membrane used is 2.2 times of described silver nano-grain particle diameter.
7. method according to claim 1, is characterized in that: described step 2) in filtration step, filtering rate is 0.25 ~ 1ml/min;
Filtration pressure is 2-10.3bar.
8. method according to claim 7, is characterized in that: described step 2) in filtration step, filtering rate is 0.5ml/min;
Filtration pressure is 5.2bar.
9., according to described method arbitrary in claim 1-8, it is characterized in that: described step 2) in drying steps, temperature is 25-40 DEG C; Time is 10-30min.
10. method according to claim 9, is characterized in that: described step 2) in drying steps, temperature is 30 DEG C; Time is 15min.
The Silver nano-particle layer that the arbitrary described method of 11. claim 1-10 prepares.
12. application using Silver nano-particle layer described in claim 11 as substrate in surface-enhanced raman scattering.
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| CN105022103B (en) * | 2015-07-06 | 2017-01-18 | 上海大学 | Preparation method for silver nano film for magnetofluid distorting lens |
| CN105710386B (en) * | 2016-02-25 | 2018-04-03 | 天津工业大学 | One-dimensional silver-colored chain nanostructured, self-assembly preparation method thereof and SERS applications |
| CN106770171A (en) * | 2016-12-29 | 2017-05-31 | 中国科学院城市环境研究所 | The preparation method of Raman spectrum base and sample |
| CN107064101B (en) * | 2017-03-15 | 2020-03-31 | 东南大学 | Enhanced Raman substrate for detecting streptomyces hyphae and preparation and use methods thereof |
| CN109187489B (en) * | 2018-10-19 | 2021-01-05 | 福建师范大学 | Preparation and application of bimolecular recognition dopamine surface-enhanced Raman sensor |
| CN113324969A (en) * | 2021-04-06 | 2021-08-31 | 金陵科技学院 | Metal/carbon nanotube composite filter membrane, and manufacturing method and application thereof |
| CN113834804B (en) * | 2021-09-23 | 2023-01-24 | 中国农业大学 | Construction method and application of flexible surface enhanced Raman substrate |
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