CN105403551A - Preparation method of thin film with Raman enhancing performance - Google Patents
Preparation method of thin film with Raman enhancing performance Download PDFInfo
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- CN105403551A CN105403551A CN201510721659.0A CN201510721659A CN105403551A CN 105403551 A CN105403551 A CN 105403551A CN 201510721659 A CN201510721659 A CN 201510721659A CN 105403551 A CN105403551 A CN 105403551A
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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
Abstract
The invention provides a preparation method of a thin film with a Raman enhancing performance. A silver and silicon dioxide nano composite thin film with the size of 100nm-150nm is prepared on a smooth quartz or mono-crystalline silicon substrate by using magnetron sputtering co-sputtering; one layer of nano silver thin film with the size of 30nm-50nm is continually sputtered on the surface of the composite thin film; the thin film is put into an annealing furnace and is heated to 900-940 DEG C under a protective atmosphere to be annealed for 1-3 hours; and then the thin film is cooled to a room temperature to obtain the thin film with the Raman enhancing performance. The preparation method has a simple preparation process, good repeatability and good stability.
Description
Technical field
The invention belongs to nano thin-film preparation and detect analysis field, relating to a kind of method that magnetron sputtering prepares the substrate of Raman enhanced film.
Background technology
Raman scattering is a kind of scattering phenomenon of light, when the photon of monochromatic incident light and testing molecule interact, there is inelastic collision, energy exchange is there is between photon and molecule, photon changes scattering raman scattering spectrum that direction of motion and frequency occur because it is to the specificity at molecule and chemical bond oscillations peak, becomes a powerful molecular detection technology.Due to the scattering xsect that Raman scattering is very little, Raman scattering is a very weak process, and is unfavorable for the qualitative analysis of micro substance.Can scattering be made to strengthen be the practical keys of raman scattering spectrum Detection Techniques.Fleischman in 1974 observes the Raman diffused light spectral intensity being attached to textured metal micro-nano structure surface molecular and can increase substantially, and is called as Surface enhanced raman spectroscopy (Surface-enhancedRamanScattering is called for short SERS).Surface enhanced raman spectroscopy (SERS) is that one has surface optionally enhancement effect, the Raman signal of the molecule being adsorbed on material surface can be amplified several order of magnitude, can reach overdelicate detection in the fields such as analysis, environment and catalysis.Common Surface enhanced raman spectroscopy comprises coarse silverskin, golden nanometer particle, Nano silver grain, golden contracted payment nano particle etc.Utilize nm of gold, Ag colloid particle, there is the shortcomings such as repeatability and poor stability, utilize Ag films to have good repeatability, but it is stable not to there is chemical property, the shortcoming of easy sulfidation-oxidation.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method with Raman-enhancing energy film.
There is a preparation method for Raman-enhancing energy film, it is characterized in that, comprise following steps:
(1) utilize magnetron sputtering cosputtering on smooth quartz or monocrystal silicon substrate, prepare silver and the silica nanometer laminated film of 100nm-150nm;
(2) sputtering one deck 30-50nm nano silver film is continued on laminated film surface;
(3) above-mentioned film is put into annealing furnace, under protective atmosphere, be heated to 900 DEG C-940 DEG C carry out annealing 1-3 hour, be cooled to room temperature, namely obtain one and there is Raman-enhancing energy film.
Magnetron sputtering cosputtering described in step (1) is silver-colored target and silicon dioxide target co-sputtering.
Silver described in step (1) and silica nanometer laminated film, silver-colored mass percent is 30%-70%.
Protective atmosphere described in step (3) is argon gas atmosphere.
The present invention utilized the method for magnetron sputtering cosputtering to prepare silver and silicon dioxide laminated film, laminated film deposited the silver nanoparticle film of the very thin dispersion of one deck again, by the high temperature long term annealing close to silver point, the inner silver nano-grain of film is made fully to spread fusion, the silver nano-grain part that film shows simultaneously diffuses into film inside, be connected with inner nano-Ag particles, form the distribution of three-dimensional composite space, the protection that nano particle in film effectively can either be subject to silicon dioxide prevents oxidation of sulfureted, therefore stability is very good, still there is spatial distribution structure simultaneously, there is good Raman and strengthen effect.The invention provides a kind of preparation method with Raman-enhancing energy film, prepared a kind of membrane structure of silver nano-grain space distribution, solved the problem that the stability of nano silver film existence is bad, there is higher sensitivity, preparation technology is simple, reproducible, and good stability.
Accompanying drawing explanation
The SEM figure of the nano thin-film of Fig. 1 prepared by embodiment 1.
Nano thin-film substrate can figure to the Raman-enhancing of 5cb prepared by embodiment 1-3 for Fig. 2.
Embodiment
Embodiment 1:
1, utilize magnetron sputtering cosputtering in smooth substrate, prepare silver and the silica nanometer laminated film of 150nm, thin film composition, by the power adjustments of silver-colored target and titanium dioxide silicon target, guarantees that the mass percent of Ag is 30%;
2, sputtering one deck 30nm nano silver film is continued on laminated film surface;
3, above-mentioned film is put into annealing furnace, under protective atmosphere, be heated to 920 DEG C carry out annealing in process, keep 3 hours, be cooled to room temperature.
Fig. 1 is the SEM figure of prepared nano thin-film, and as can be seen from the figure film surface is dispersed with nano-Ag particles.
Embodiment 2:
1, utilize magnetron sputtering cosputtering in smooth substrate, prepare silver and the silica nanometer laminated film of 100nm, sputter target used and be respectively silver-colored target and titanium dioxide silicon target, work atmosphere is argon gas, sputtering pressure is 0.8Pa, regulate the power of silver-colored target and titanium dioxide silicon target, guarantee that the mass percent of Ag is 70%;
2, sputtering one deck 40nm nano silver film is continued on laminated film surface;
3, above-mentioned film is put into annealing furnace, under protective atmosphere, be heated to 900 DEG C carry out annealing in process, keep 3 hours, be cooled to room temperature.
By prepared film substrate, for the detection of 5cb liquid crystal molecule.
Embodiment 3:
1, utilize magnetron sputtering cosputtering in smooth substrate, prepare silver and the silica nanometer laminated film of 130nm, sputter target used and be respectively silver-colored target and titanium dioxide silicon target, work atmosphere is argon gas, sputtering pressure is 0.8Pa, thin film composition, by the power adjustments of silver-colored target and titanium dioxide silicon target, guarantees that the mass percent of Ag is 50%;
2, sputtering one deck 50nm nano silver film is continued on laminated film surface;
3, above-mentioned film is put into annealing furnace, under protective atmosphere, be heated to 940 DEG C carry out annealing in process, keep 1 hours, be cooled to room temperature.
By prepared film substrate, for the detection of 5cb liquid crystal molecule.
Raman enhanced film substrate prepared by above-described embodiment, preparation technology is simple, reproducible, and the film performance of preparation is stablized, and can meet many-sided detection application demand.
Claims (4)
1. there is a preparation method for Raman-enhancing energy film, it is characterized in that, comprise following steps:
(1) utilize magnetron sputtering cosputtering on smooth quartz or monocrystal silicon substrate, prepare silver and the silica nanometer laminated film of 100nm-150nm;
(2) sputtering one deck 30-50nm nano silver film is continued on laminated film surface;
(3) above-mentioned film is put into annealing furnace, under protective atmosphere, be heated to 900 DEG C-940 DEG C carry out annealing 1-3 hour, be cooled to room temperature, namely obtain one and there is Raman-enhancing energy film.
2. a kind of preparation method with Raman-enhancing energy film according to claim 1, it is characterized in that, magnetron sputtering cosputtering described in step (1) is silver-colored target and silicon dioxide target co-sputtering.
3. a kind of preparation method with Raman-enhancing energy film according to claim 1, it is characterized in that, the silver described in step (1) and silica nanometer laminated film, silver-colored mass percent is 30%-70%.
4. a kind of preparation method with Raman-enhancing energy film according to claim 1, it is characterized in that, the protective atmosphere described in step (3) is argon gas atmosphere.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105839062A (en) * | 2016-04-05 | 2016-08-10 | 吉林师范大学 | Compound type multilayer film structure silver nanowire and preparation method thereof |
| CN106544788A (en) * | 2016-11-03 | 2017-03-29 | 苏州科技大学 | The synthetic method of nanometer silver/silicon dioxide Raman surface enhanced film and application |
| CN109136860A (en) * | 2018-09-18 | 2019-01-04 | 北京科技大学 | A kind of surface enhanced Raman substrate and preparation method thereof |
| CN111364092A (en) * | 2020-03-26 | 2020-07-03 | 新疆艾旗斯德检测科技有限公司 | Preparation method of silver-porous silicon-based surface enhanced Raman scattering biological detection chip |
| CN113981371A (en) * | 2021-10-20 | 2022-01-28 | 杭州电子科技大学 | Ag/SiO with high SERS strength2Preparation method of co-sputtering single-layer film |
| CN114231930A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Method for preparing ultra-dense hot spot space structure |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105839062A (en) * | 2016-04-05 | 2016-08-10 | 吉林师范大学 | Compound type multilayer film structure silver nanowire and preparation method thereof |
| CN106544788A (en) * | 2016-11-03 | 2017-03-29 | 苏州科技大学 | The synthetic method of nanometer silver/silicon dioxide Raman surface enhanced film and application |
| CN106544788B (en) * | 2016-11-03 | 2018-12-25 | 苏州科技大学 | The synthetic method and application of nanometer silver/silicon dioxide Raman surface enhanced film |
| CN109136860A (en) * | 2018-09-18 | 2019-01-04 | 北京科技大学 | A kind of surface enhanced Raman substrate and preparation method thereof |
| CN111364092A (en) * | 2020-03-26 | 2020-07-03 | 新疆艾旗斯德检测科技有限公司 | Preparation method of silver-porous silicon-based surface enhanced Raman scattering biological detection chip |
| CN111364092B (en) * | 2020-03-26 | 2021-06-08 | 新疆艾旗斯德检测科技有限公司 | Preparation method of silver-porous silicon-based surface enhanced Raman scattering biological detection chip |
| CN113981371A (en) * | 2021-10-20 | 2022-01-28 | 杭州电子科技大学 | Ag/SiO with high SERS strength2Preparation method of co-sputtering single-layer film |
| CN113981371B (en) * | 2021-10-20 | 2024-03-15 | 杭州电子科技大学 | Ag/SiO with high SERS intensity 2 Co-sputtering single-layer film preparation method |
| CN114231930A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Method for preparing ultra-dense hot spot space structure |
| CN114231930B (en) * | 2021-12-22 | 2023-10-17 | 杭州电子科技大学 | Method for preparing ultra-dense hot spot space structure |
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