CN107761053A - Preparation method of large area Raman enhancing substrate and products thereof and application - Google Patents
Preparation method of large area Raman enhancing substrate and products thereof and application Download PDFInfo
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- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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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
- G01N21/65—Raman scattering
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Abstract
The present invention, which provides a kind of preparation method of large area Raman enhancing substrate and products thereof and application, methods described, to be included:One layer of Ag nano thin-film is prepared using magnetron sputtering cosputtering in smooth glass or monocrystalline silicon piece substrate, and prepares one layer of Al using ald on this basis2O3Nano thin-film, recycle magnetron sputtering to prepare one layer of Ag nano thin-film on this technology, then carry out short annealing processing under nitrogen protection, finally prepare one layer of Al using ald on this basis again2O3Nano thin-film.Preparation technology of the present invention is simple, and the Raman enhancing effect of its product is excellent, and is suitable for large area preparation.
Description
Technical field
Field, more particularly to a kind of large area Raman enhancing substrate are prepared and tested and analyzed the invention belongs to nano thin-film
Preparation method and products thereof and application.
Background technology
Raman scattering is a kind of scattering phenomenon of light, is photon and testing molecule interaction, hair when monochromatic incident light
Raw inelastic collision, occurs energy exchange between photon and molecule, photon changes the scattering that the direction of motion and frequency are occurred and drawn
Graceful scattering spectrum turns into the powerful molecular detection technology of One function due to its specificity to molecule and chemical bond oscillations peak.
Due to the very small scattering cross section of Raman scattering, Raman scattering is a very weak process, and is unfavorable for determining for micro substance
Property analysis.Can it be the practical key of raman scattering spectrum Detection Techniques that scattering enhancing be made.Fleischman observations in 1974
It can be increased substantially to the Raman diffused light spectral intensity for being attached to textured metal micro-nano structure surface molecular, be referred to as surface enhanced
Raman scattering(Surface-enhanced Raman Scattering, abbreviation SERS).SERS(SERS)It is
A kind of enhancement effect with surface selectivity, the Raman signal adsorbed in the molecule of material surface can be amplified several quantity
Level, overdelicate detection can be reached in the fields such as analysis, environment and catalysis.Common SERS includes thick
Rough silverskin, golden nanometer particle, Nano silver grain, golden contracted payment nano-particle etc..Using nanogold, Ag colloid particle, exist emphatically
Renaturation is poor, it is impossible to the shortcomings of prepared by large area.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at:A kind of preparation of large area Raman enhancing substrate is provided
Method.
Another object of the present invention is:Large area Raman enhancing substrate product obtained above is provided.
A further object of the present invention is:The application of the said goods is provided.
The object of the invention is achieved through the following technical solutions:A kind of preparation method of large area Raman enhancing substrate, is utilized
Magnetron sputtering and technique for atomic layer deposition are combined, and are comprised the steps of:
(1)The thick Ag nano thin-films of 60-100nm are prepared in smooth glass or monocrystalline silicon piece substrate using magnetron sputtering;
(2)One layer of 2-8nm thickness Al is further prepared in above-mentioned substrate using ald2O3Nano thin-film;
(3)Again further 40-60nm thickness Ag nano thin-films are prepared in above-mentioned substrate using magnetron sputtering;
(4)By above-mentioned substrate under nitrogen atmosphere, short annealing is carried out;
(5)1-5nm thickness Al is further prepared in the substrate after the return of goods using ald2O3Nano thin-film.
The present invention is combined using magnetron sputtering and technique for atomic layer deposition, it is ensured that large area is processed, and is had
Good stability and repeatability.
On the basis of such scheme, step(1)With(3)Described in magnetron sputtering, target used is metal Ag targets, sputter gas
Atmosphere is argon gas.
Step(2)With(5)Described in ald, forerunner source used is trimethyl aluminium and water, depositing temperature 150
℃。
Step(4)Described in short annealing, annealing temperature be 800 DEG C, annealing time 30-60s.
The present invention provides a kind of large area Raman enhancing substrate, is prepared according to method described above.
The present invention also provides a kind of application of large area Raman enhancing substrate in Raman detection.
The present invention provides a kind of preparation method of large area Raman enhancing substrate, on the one hand thin by two layers of Ag nano particle
The structure of film, Raman-enhancing energy is significantly improved compared to individual layer Ag nanometer particle films;Meanwhile pass through ald table
Face covers Al2O3Passivation layer, stability is improved, improve service life.The present invention all of be suitable for large area preparation
Magnetron sputtering and technique for atomic layer deposition, it is ensured that substrate can be processed with large area, and ensure that the good weight of substrate
Renaturation.
Brief description of the drawings
Fig. 1 is that nano thin-film substrate prepared by embodiment 1 can be schemed to the Raman-enhancing of 5cb.
Embodiment
A kind of preparation of large area Raman enhancing substrate:
1st, using magnetron sputtering in smooth glass or monocrystalline silicon piece substrate Ag nano thin-films processed;
2nd, one layer of Al is further prepared in above-mentioned substrate using ald2O3Nano thin-film;
3rd, Ag nano thin-films further are prepared using magnetron sputtering in above-mentioned substrate again;
4th, by above-mentioned substrate under nitrogen atmosphere, short annealing is carried out;
5th, Al is further prepared in substrate after the return of goods using ald2O3Nano thin-film.
Magnetron sputtering Ag nano thin-films described in step 1, its thickness are 60-100nm;
Al described in step 22O3Nano thin-film, its thickness are 2-8nm;
Magnetron sputtering Ag nano thin-films described in step 3, its thickness are 40-60nm;
Short annealing described in step 4, its annealing temperature are 800 DEG C, annealing time 30-60s;
Al described in step 52O3Nano thin-film, its thickness are 1-5nm;
Step 1 and 3 magnetron sputterings, target used are metal Ag targets, and sputtering atmosphere is argon gas;
Step 2 and 5 alds, forerunner source used are trimethyl aluminium and water, and depositing temperature is 150 DEG C, Al2O3Thickness
Degree control, is controlled, single cycle Al by number of deposition cycles2O3Thickness be about 0.1nm.
Embodiment 1
1st, using magnetron sputtering in smooth glass or monocrystalline silicon piece substrate 60nmAg nano thin-films processed;
2nd, one layer of 2nmAl is further prepared in above-mentioned substrate using ald2O3Nano thin-film;
3rd, 40nmAg nano thin-films further are prepared using magnetron sputtering in above-mentioned substrate again;
4th, by above-mentioned substrate under nitrogen atmosphere, short annealing is carried out, its annealing temperature is 800 DEG C, annealing time 30s;
5th, 1nm Al are further prepared in substrate after the return of goods using ald2O3Nano thin-film.
Embodiment 2
1st, using magnetron sputtering in smooth glass or monocrystalline silicon piece substrate 100nmAg nano thin-films processed;
2nd, one layer of 8nmAl is further prepared in above-mentioned substrate using ald2O3Nano thin-film;
3rd, 60nmAg nano thin-films further are prepared using magnetron sputtering in above-mentioned substrate again;
4th, by above-mentioned substrate under nitrogen atmosphere, short annealing is carried out, its annealing temperature is 800 DEG C, annealing time 60s;
5th, 5nm Al are further prepared in substrate after the return of goods using ald2O3Nano thin-film.
Embodiment 3
1st, using magnetron sputtering in smooth glass or monocrystalline silicon piece substrate 70nmAg nano thin-films processed;
2nd, one layer of 3nmAl is further prepared in above-mentioned substrate using ald2O3Nano thin-film;
3rd, 50nmAg nano thin-films further are prepared using magnetron sputtering in above-mentioned substrate again;
4th, by above-mentioned substrate under nitrogen atmosphere, short annealing is carried out, its annealing temperature is 800 DEG C, annealing time 40s;
5th, 3nm Al are further prepared in substrate after the return of goods using ald2O3Nano thin-film.
Above-described embodiment prepare Raman enhanced film substrate, preparation technology is simple, can large area prepare, function admirable,
It is stability, reproducible, there is good practicality.
Claims (7)
1. a kind of preparation method of large area Raman enhancing substrate, it is characterised in that comprise the steps of:
(1)The thick Ag nano thin-films of 60-100nm are prepared in smooth glass or monocrystalline silicon piece substrate using magnetron sputtering;
(2)One layer of 2-8nm thickness Al is further prepared in above-mentioned substrate using atomic layer deposition method2O3Nano thin-film;
(3)Again further 40-60nm thickness Ag nano thin-films are prepared in above-mentioned substrate using magnetron sputtering;
(4)By above-mentioned substrate under nitrogen atmosphere, short annealing is carried out;
(5)1-5nm thickness Al is prepared using further in the substrate of atomic layer deposition method after annealing2O3Nano thin-film.
2. the preparation method of large area Raman enhancing substrate according to claim 1, it is characterised in that step(1)With(3)
Described in magnetron sputtering, by the use of metal Ag targets as target, sputtering atmosphere is argon gas.
3. the preparation method of large area Raman enhancing substrate according to claim 1, it is characterised in that step(2)With(5)
Described in atomic layer deposition method, trimethyl aluminium and water as forerunner source, depositing temperature is 150 DEG C.
4. the preparation method of the large area Raman enhancing substrate according to claim 1 and 3, it is characterised in that pass through deposition
Cycle-index is controlled Al2O3Thickness control, single cycle Al2O3Thickness be about 0.1nm.
5. the preparation method of large area Raman enhancing substrate according to claim 1, it is characterised in that step(4)Middle institute
The short annealing stated, annealing temperature are 800 DEG C, annealing time 30-60s.
6. a kind of large area Raman strengthens substrate, it is characterised in that is prepared into according to claim 1-5 any one methods described
Arrive.
A kind of 7. application of the Raman of large area according to claim 6 enhancing substrate in Raman detection.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN109267023A (en) * | 2018-08-29 | 2019-01-25 | 江苏理工学院 | A kind of antibacterial active carbon fiber material and preparation method thereof |
CN109365831A (en) * | 2018-12-19 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of new infrared photodetection substrate based on tip deposition Pd/Ag gold nano double cone structure |
CN109434128A (en) * | 2018-10-25 | 2019-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Au loads preparation method of tin dioxide nanometer material and products thereof and application |
CN109520992A (en) * | 2018-11-08 | 2019-03-26 | 南京光声超构材料研究院有限公司 | A kind of SERS substrate of bromination silver nanowires and preparation method thereof |
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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CN104746049A (en) * | 2015-04-07 | 2015-07-01 | 南京大学 | Method for preparing surface-enhanced Raman scattering base with metal nanometer gaps by utilizing ALD (atomic layer deposition) |
CN105651756A (en) * | 2016-01-04 | 2016-06-08 | 山东师范大学 | Raman enhanced base for amplifying raman signal, and preparation method and application thereof |
CN205484061U (en) * | 2016-01-21 | 2016-08-17 | 中国人民公安大学 | Raman reinforcing basement |
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CN104746049A (en) * | 2015-04-07 | 2015-07-01 | 南京大学 | Method for preparing surface-enhanced Raman scattering base with metal nanometer gaps by utilizing ALD (atomic layer deposition) |
CN105651756A (en) * | 2016-01-04 | 2016-06-08 | 山东师范大学 | Raman enhanced base for amplifying raman signal, and preparation method and application thereof |
CN205484061U (en) * | 2016-01-21 | 2016-08-17 | 中国人民公安大学 | Raman reinforcing basement |
Cited By (8)
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CN109267023A (en) * | 2018-08-29 | 2019-01-25 | 江苏理工学院 | A kind of antibacterial active carbon fiber material and preparation method thereof |
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 |
CN109434128A (en) * | 2018-10-25 | 2019-03-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Au loads preparation method of tin dioxide nanometer material and products thereof and application |
CN109520992A (en) * | 2018-11-08 | 2019-03-26 | 南京光声超构材料研究院有限公司 | A kind of SERS substrate of bromination silver nanowires and preparation method thereof |
CN109520992B (en) * | 2018-11-08 | 2021-02-05 | 南京光声超构材料研究院有限公司 | SERS substrate of silver bromide nanowire and preparation method thereof |
CN109365831A (en) * | 2018-12-19 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of new infrared photodetection substrate based on tip deposition Pd/Ag gold nano double cone structure |
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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