CN109520992B - SERS substrate of silver bromide nanowire and preparation method thereof - Google Patents
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- 239000000758 substrate Substances 0.000 title claims abstract description 51
- 239000002070 nanowire Substances 0.000 title claims abstract description 41
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 title claims abstract description 37
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 40
- 239000004332 silver Substances 0.000 claims abstract description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 39
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 10
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 9
- 238000004544 sputter deposition Methods 0.000 claims abstract description 9
- 230000035484 reaction time Effects 0.000 claims 1
- LMJXSOYPAOSIPZ-UHFFFAOYSA-N 4-sulfanylbenzoic acid Chemical compound OC(=O)C1=CC=C(S)C=C1 LMJXSOYPAOSIPZ-UHFFFAOYSA-N 0.000 description 15
- 238000001069 Raman spectroscopy Methods 0.000 description 13
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000010703 silicon Substances 0.000 description 10
- 239000002086 nanomaterial Substances 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003550 marker Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004001 molecular interaction Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- -1 silver halides Chemical class 0.000 description 1
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- 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
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- 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)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses an SERS substrate of silver bromide nanowires and a preparation method thereof. The SERS substrate comprises a substrate, a silver film and silver bromide nanowires, wherein the silver film is located on the substrate, and the silver bromide nanowires are located on the silver film. The preparation method comprises the following steps: (1) sputtering a silver film on a substrate by adopting a magnetron sputtering method; (2) and (2) soaking the silver film obtained in the step (1) in 1mL of mixed solution consisting of 50mM/L ferric nitrate nonahydrate, 40mM/L sodium bromide and 50mM/L polyvinylpyrrolidone for reaction for a certain time by adopting an in-situ silver oxide film method, and obtaining a product, namely the SERS substrate of the silver bromide nanowire. The SERS substrate can generate uniform SERS signals with high intensity and good stability.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a SERS substrate based on silver bromide nanowires and a preparation method thereof.
Background
Raman spectroscopy is an analytical technique for non-contact non-destructive testing that allows analysis of the chemical structure, crystalline phase and molecular interactions of a sample. However, the raman spectrum has very weak signal intensity, which limits its application range. The Surface Enhanced Raman Scattering (SERS) technology overcomes the defect of weak Raman spectrum signals, can greatly amplify the Raman signals of the analytes on the surface of the plasma metal nano structure, and has the advantages of high sensitivity and nondestructive detection. Therefore, the technology has wide application prospect in the fields of chemistry, biology, environment and the like.
The SERS substrate mostly adopts a noble metal nano rough surface or nano structure to enhance the intensity of raman scattering signals, which greatly limits the application of the SERS technology. In recent years, with the intensive research on nanomaterials, the research on SERS characteristics of metal oxides, silver halides, semiconductors and their mixed structures has become an important branch of SERS. The interface of the mixed nano structure of the noble metal and the semiconductor material generates strong charge transfer and electromagnetic field due to the plasma effect and excellent conductivity of the noble metal nano particles, and the result shows that the nano structures have excellent SERS activity and can be applied to high-sensitivity detection of various molecules.
Disclosure of Invention
Therefore, the invention provides the SERS substrate of the silver bromide nanowire, which has higher SERS performance. It is another object of the present invention to provide a method for preparing the substrate.
The substrate of the invention adopts the technical scheme that:
the SERS substrate of the silver bromide nanowire comprises a substrate, a silver film and the silver bromide nanowire, wherein the silver film is located on the substrate, and the silver bromide nanowire is located on the silver film.
Preferably, the thickness of the silver film is 100-400 nm.
Preferably, the silver bromide nanowires have the length of 0.6-6 mu m and the diameter of 30-150 nm.
Preferably, the substrate is a silicon wafer polished on a single surface, and the silicon wafer is a monocrystalline silicon wafer or a polycrystalline silicon wafer.
The invention relates to a preparation method of an SERS substrate of silver bromide nanowires, which comprises the following steps:
(1) preparing a silver film: sputtering a silver film with the thickness of 100-400 nm on a substrate by adopting a magnetron sputtering method;
(2) preparing silver bromide nanowires: and (2) soaking the silver film obtained in the step (1) in 1mL of mixed solution consisting of 50mM/L ferric nitrate nonahydrate, 40mM/L sodium bromide and 50mM/L polyvinylpyrrolidone for reaction for 0.5-8 h by adopting an in-situ silver oxide film method, wherein the obtained product is the SERS substrate of the silver bromide nanowire.
The invention provides a preparation method of an SERS substrate with a noble metal silver and semiconductor silver bromide nano mixed structure and an in-situ silver oxide film, aiming at the defects of non-uniformity and instability of the conventional SERS substrate. The noble metal silver nanoparticles have the plasma effect and excellent conductivity, so that the semiconductor material silver bromide can stably exist under visible light, and meanwhile, the interface between the noble metal silver and the semiconductor has strong charge transfer (chemical enhancement) and electromagnetic field (physical enhancement), thereby being beneficial to the substrate to generate uniform SERS signals with high strength and good stability.
Drawings
FIG. 1 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 1, taken after 0.5h of reaction.
FIG. 2 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 2, taken after reaction for 1 hour.
FIG. 3 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 3, reacted for 2 h.
FIG. 4 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 4 after reaction for 4 hours.
FIG. 5 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 5 after reaction for 6 hours.
FIG. 6 is a scanning electron micrograph of the Ag-AgBr structure obtained in example 6 after reaction for 8 hours.
FIG. 7 is an XRD of the Ag-AgBr structure obtained in example 3.
FIG. 8 is a SERS spectrum of Raman labeled molecule 4MBA structurally linked with Ag-AgBr prepared in examples 1-6.
FIG. 9 is a SERS spectrum of Ag-AgBr prepared in examples 1-6, wherein different Raman labeling molecules (a) Me, CV (b) RhB, R6G are structurally linked.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
The SERS substrate of the embodiment comprises a silicon wafer with a polished single surface, a silver film on the polished surface of the silicon wafer and a silver bromide nanowire, wherein the chemical formula is Ag-AgBr, and the silver bromide nanowire is positioned on the silver film.
Example 1
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP, K-30, 50mM/L) for reaction for 0.5h by adopting an in-situ silver oxide film method to obtain an Ag-AgBr product.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 1, the size of the nanowire bar is: the longitudinal length is 2 + -0.1 μm and the transverse diameter is 30 + -2 nm.
Example 2
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP 50mM/L) for reaction for 1h by adopting an in-situ silver oxide film method, and obtaining a product, namely Ag-AgBr.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 2, the size of the nanowire bar is: the longitudinal length is 3 + -0.2 μm and the transverse diameter is 40 + -5 nm.
Example 3
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP, 50mM/L) for reaction for 2 hours by adopting an in-situ silver oxide film method, and obtaining the product, namely Ag-AgBr.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 3, the size of the nanowire bar is: the longitudinal length is 2 + -0.02 μm and the transverse diameter is 150 + -10 nm. The corresponding XRD pattern of the substrate is shown in fig. 7.
Example 4
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP, 50mM/L) for reaction for 4 hours by adopting an in-situ silver oxide film method, and obtaining the product, namely Ag-AgBr.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 4, the size of the nanowire bar is: the longitudinal length is 6 + -0.5 μm and the transverse diameter is 70 + -5 nm.
Example 5
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP, 50mM/L) for reaction for 6h by adopting an in-situ silver oxide film method, and obtaining the product, namely Ag-AgBr.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 5, the size of the nanowire bar is: the longitudinal length is 4 + -0.3 μm and the transverse diameter is 40 + -4 nm.
Example 6
(1) Preparing a silver film, and sputtering a layer of silver film with the thickness of 200nm on a silicon wafer by adopting magnetron sputtering.
(2) And (2) preparing silver bromide nanowires, namely soaking the silver film obtained in the step (1) in 1mL of mixed solution of ferric nitrate nonahydrate (50mM/L), sodium bromide (40mM/L) and polyvinylpyrrolidone (PVP, 50mM/L) for reaction for 8 hours by adopting an in-situ silver oxide film method, and obtaining the product, namely Ag-AgBr.
The silver bromide nanowire structure on the substrate prepared by this example, as shown in fig. 6, the size of the nanowire bar is: the longitudinal length is 0.6 + -0.05 μm and the transverse diameter is 50 + -3 nm.
Example 7
This example provides an implementation process for linking the Ag-AgBr substrate prepared in examples 1 to 6 to a raman labeled molecule and detecting its SERS spectrum. The method comprises the following specific steps:
(1) p-mercaptobenzoic acid (4MBA) was used as a Raman labeling molecule to prepare a solution of p-mercaptobenzoic acid (4MBA) at a concentration of 10 mM.
(2) And (3) soaking the Ag-AgBr substrate prepared in the embodiment 1-6 in a 4MBA solution drop, placing the solution at room temperature for 3 hours, after full linkage, washing the 4MBA labeled molecules which are not linked to the substrate with deionized water, washing for 2-3 times, and then placing the substrate at room temperature for natural drying.
(3) Measuring the SERS spectrum of the 4 MBA-labeled molecules linked from the Ag-AgBr substrate prepared in step (2). For detection, a small raman spectrometer (BWS415, B & W Tek Inc.) was used, and the characteristic SERS spectrum of the 4 MBA-labeled molecule recorded by the raman spectrometer is shown in fig. 8. The integration time for collecting the SERS spectrum is 10s, the power of the irradiation laser is 26mw, and the laser wavelength is 785 nm.
As can be seen from FIG. 8, the substrates prepared in examples 1 to 6 have excellent SERS characteristics. Among them, the substrate prepared in example 4 has the optimal SERS activity.
Example 8
This example shows an implementation of linking the Ag-AgBr substrate prepared in example 4 with raman labeled molecules of different concentrations and detecting its SERS spectrum. The method comprises the following specific steps:
(1) p-mercaptobenzoic acid (4MBA) is used as a Raman marker molecule, and the preparation concentration is 10-2M～10-7M in p-mercaptobenzoic acid (4 MBA).
(2) And (3) soaking a plurality of Ag-AgBr substrates prepared in the embodiment 4 in 4MBA solutions with different concentrations, placing the substrates at room temperature for 3 hours, after full linking, washing the 4MBA labeled molecules which are not linked to the substrates by using deionized water, washing for 2-3 times, and then placing the substrates at room temperature for natural drying.
(3) Measuring the SERS spectrum of the Ag-AgBr substrate-linked 4MBA labeled molecule prepared in the step (2). For detection, a small raman spectrometer (BWS415, B & W Tek Inc.) was used, and the characteristic SERS spectrum of the 4 MBA-labeled molecule recorded by the raman spectrometer is shown in fig. 9. The integration time for collecting the SERS spectrum is 10s, the power of the irradiation laser is 26mw, and the laser wavelength is 785 nm.
As can be seen from FIG. 9, the SERS spectrum intensity decreases with the decrease of the 4MBA concentration, and when the 4MBA concentration is 10-71078 and 1560cm of labeled molecule can be still clearly seen at M-1Characteristic peak of (2). The Ag-AgBr substrate has excellent sensitivity and can be used for molecular detection.
The above description is only a preferred embodiment of the present invention, and it should be noted that any simple modification and modification of the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention for those skilled in the art without departing from the content of the technical solution of the present invention.
Claims (3)
1. A preparation method of an SERS substrate of silver bromide nanowires is characterized by comprising the following steps:
(1) preparing a silver film: sputtering a silver film on a substrate by adopting a magnetron sputtering method;
(2) preparing silver bromide nanowires: soaking the silver film obtained in the step (1) in 1mL of mixed solution consisting of 50mmol/L ferric nitrate nonahydrate, 40mmol/L sodium bromide and 50mmol/L polyvinylpyrrolidone for reacting for a certain time by adopting an in-situ silver oxide film method to obtain a product of the silver bromide nanowire positioned on the silver film, namely the SERS substrate of the silver bromide nanowire.
2. The method for preparing the SERS substrate of silver bromide nanowires as claimed in claim 1, wherein in the step (1), the thickness of the silver film is 100-400 nm.
3. The method for preparing the SERS substrate of silver bromide nanowires as claimed in claim 1, wherein in the step (2), the reaction time is 0.5-8 h.
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