CN105241862B - A kind of surface has the surface-enhanced Raman effects substrate and preparation method of pin hole - Google Patents
A kind of surface has the surface-enhanced Raman effects substrate and preparation method of pin hole Download PDFInfo
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- CN105241862B CN105241862B CN201510608664.0A CN201510608664A CN105241862B CN 105241862 B CN105241862 B CN 105241862B CN 201510608664 A CN201510608664 A CN 201510608664A CN 105241862 B CN105241862 B CN 105241862B
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Abstract
The invention belongs to trace materials detection technique field, more particularly to a kind of surface has the surface-enhanced Raman effects substrate and preparation method of pin hole.The present invention prepares Silver nanorod array film using growth method is tilted, recycle low temperature ald technology that there is the aluminum oxide film of pin hole in one layer of its surface uniform deposition, obtain silver-colored alumina composite nanostructured of the surface with pin hole as surface-enhanced Raman effects substrate.The method can control the needle hole ratio of pellumina by adjusting the parameter of low temperature ald technology; its ultra-thin oxide layer ensures that substrate has good surface reinforced Raman active; and isolate internal Silver nanorod with external environment, significantly improve the chemical stability of substrate.Meanwhile the adsorbable specific detection molecules in the silver-colored top layer in pellumina and pin hole, the substrate can be used for the detection of a variety of chemical substances, extend the use scope of surface-enhanced Raman effects, be with a wide range of applications.
Description
Technical field
The invention belongs to trace materials detection technique field, more particularly to a kind of surface has the surface-enhanced Raman of pin hole
Effect substrate and preparation method.
Background technology
Surface-enhanced Raman effects are used for chemistry, the trace detection of biomolecule, have nondestructive analysis, high sensitivity, inspection
Survey the advantages that time is short, expense is low, strong applicability.This method needs to prepare with high sensitivity using noble metals such as gold, silver
Surface-enhanced Raman effects substrate, simultaneously because the poor chemical stability of metal Nano structure, the suction to some detection molecules
It is attached indifferent, it greatly limit the development of surface enhanced Raman technique.
The present invention deposits one layer of ultra-thin oxygen with pin hole on silver nanostructured surface by low temperature ald technology
Change aluminium film, and can control the needle hole ratio of pellumina, the base obtained by adjusting the parameter of low temperature ald technology
The chemical stability and applicability at bottom have very big lifting, extend the detection range of surface-enhanced Raman effects.Because of ultra-thin oxygen
Change layer will not strong attenuation Silver nanorod surface-enhanced Raman signals, substrate has good surface reinforced Raman active；Oxygen
Change layer also to isolate metal core with external environment, significantly improve the chemical stability of substrate；Meanwhile aoxidize aluminum surface layer and pin
The adsorbable specific detection molecules in silver-colored top layer in hole, the substrate can be used for the detection of a variety of chemical substances, extend surface
Strengthen the application range of Ramam effect.
The content of the invention
There is the surface enhanced drawing of silver-alumina composite nanostructured of pin hole the object of the present invention is to provide a kind of surface
Graceful effect substrate, and to prepare silver-aluminium oxide multiple using low temperature ald method (Atomic Layer Deposition, ALD)
The method for closing nanostructured substrate.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of surface has the surface-enhanced Raman effects substrate of pin hole：In Silver nanorod array film surface uniform deposition
One layer of aluminum oxide film with pin hole, and needle hole ratio is controllable, obtaining surface has silver-alumina composite nano junction of pin hole
Structure is as surface-enhanced Raman effects substrate.
Further, the Silver nanorod array film is oblique rod array film or the straight rod array film of cylinder, Yin Na
Rice rod length is 400nm~700nm, and there is pin hole, thickness to be less than 1nm on the surface of the aluminum oxide film.
Further, the needle hole ratio refers to that the silver-colored surface area of not oxidized aluminium film covering accounts for whole surface increasing
The ratio of strong Ramam effect substrate surface product；The scope of needle hole ratio is 16%~5%.
The preparation method of surface-enhanced Raman effects substrate as described above：Using growing method is tilted, sink on substrate
Product metallic silver, obtains Silver nanorod array film；It is equal on Silver nanorod array film surface using low temperature ald technology
Even one layer of aluminum oxide film with pin hole of deposition, obtains silver-alumina composite nanostructured of the surface with pin hole as table
Face strengthens Ramam effect substrate.
Further, it is using tilting the step of growing method prepares Silver nanorod array film：At room temperature, by substrate
It is fixed on the sample stage of electron beam evaporation deposition machine；Metallic silver is used as target, electron beam evaporation deposition machine cavity room is evacuated to
Vacuum is 3 × 10- 5Pa~8 × 10- 5Pa；It is 85 °~88 ° to adjust electron beam incident angle, and makes sample stage static or with 6rpm
The speed rotation of~10rpm, grows Silver nanorod array film on the substrate of sample stage.
Further, will be previously prepared when there is the aluminum oxide film of pin hole using low temperature ald technology deposition
Good Silver nanorod array film is put into the middle part of atomic layer deposition reaction cavity, and cavity temperature is 50 DEG C~70 DEG C；With trimethyl
Aluminium and water are passed through in reaction cavity as precursors, alternating, flow 20sccm, by varying being passed through for two kinds of presomas
Time adjusts the needle hole ratio of aluminum oxide film, and trimethyl aluminium and water each lead into 2~80ms and 1~40ms.
Further, as the amount for being passed through trimethyl aluminium and water increases, needle hole ratio declines, and the scope of needle hole ratio is
16%~5%.
The beneficial effects of the invention are as follows：Uniformly sunk on Silver nanorod array film surface by low temperature ald technology
One layer of product has the ultrathin alumina film of pin hole, and controls the pin hole of aluminum oxide film ratio by adjusting atomic layer deposition parameter
Example.Due to ultra-thin oxide layer will not strong attenuation Silver nanorod surface-enhanced Raman signals, substrate has good surface
Strengthen Raman active；Oxide layer also isolates metal core with external environment, significantly improves the chemical stability of substrate；Together
When, the adsorbable specific detection molecules in silver-colored top layer in aluminum surface layer and pin hole are aoxidized, which can be used for a variety of chemical substances
Detection, extend the application range of the surface enhanced Raman substrate.
Brief description of the drawings
In Fig. 1, Fig. 1 a are that the surface prepared in embodiment 1 has silver-alumina composite nanostructured substrate of pin hole
Scanning electron microscope (SEM) photograph, Fig. 1 b are the transmission electron microscope picture of single Silver nanorod, and Fig. 1 c are that the high-resolution for the aluminum oxide film for having pin hole is saturating
Electron microscope is penetrated, Fig. 1 d are silver-alumina composite nanometer that the surface prepared with the trimethyl aluminium and water of different content has pin hole
Structural substrates detection 1 × 10-2Raman spectrogram obtained by M acridines.
In Fig. 2, Fig. 2 a, 2c, 2e are respectively the oblique rod array film of silver nanoparticle that will be prepared in embodiment 2 in sodium chloride
(NaCl, 30mM), hydrogen peroxide (H2O2, 2.2%) and Cymag (NaCN, 50ppb) solution in soak 3h, 0.5h and 3h after
Scanning electron microscope (SEM) photograph；Fig. 2 b, 2d, 2f are respectively silver-alumina composite nano junction that the surface prepared in embodiment 2 is had pin hole
Structure substrate is in sodium chloride (NaCl, 30mM), hydrogen peroxide (H2O2, 2.2%) and Cymag (NaCN, 50ppb) solution in soak
Scanning electron microscope (SEM) photograph after 3h, 0.5h and 3h.
In Fig. 3, the surface prepared in embodiment 3 is had silver-alumina composite nano junction of pin hole by Fig. 3 a, Fig. 3 c respectively
Structure substrate is used to detect the Raman spectrum line chart obtained when trace Cymag and 2,6- pyridinedicarboxylic acid, and Fig. 3 b, Fig. 3 d are correspondingly
For the quantitative analysis figure to raman scattering intensity-molecular concentration relation.
Embodiment
Below in conjunction with the accompanying drawings 1~3 and embodiment the present invention is illustrated.Following embodiments be it is illustrative, no
It is limited, it is impossible to limit protection scope of the present invention with following embodiments.
Embodiment 1
1. silicon chip or glass substrate acetone, alcohol, deionized water order are cleaned by ultrasonic and dried；
2. pretreated substrate is fixed on the sample stage of electron beam evaporation deposition machine；
3. at room temperature, use metallic silver as target, by the chamber of electron beam evaporation deposition machine be evacuated to vacuum for 3 ×
10- 5Pa；
4. adjusting the incidence angle of electron beam to 85 °, and make sample stage static, in the substrate updip sideways growth nanometer of sample stage
Rod length is the oblique rod array film of silver nanoparticle of 700nm；
5. by low temperature ald method, to 70 DEG C, the flow for controlling trimethyl aluminium and water is heating cavity
20sccm, by adjusting being passed through the time and controlling the needle hole ratio of pellumina for trimethyl aluminium and water, trimethyl aluminium is passed through
Time is respectively 2ms, 5ms, 10ms, 20ms, 40ms, 80ms, water be passed through the time be correspondingly followed successively by 1ms, 2ms, 5ms,
10ms, 20ms, 40ms, in one layer of aluminum oxide film with pin hole of the oblique rod array film surface uniform deposition of silver nanoparticle, obtain
Surface has silver-alumina composite nanostructured of pin hole, as surface-enhanced Raman effects substrate.
Fig. 1 a are that the surface for the atomic layer deposition preparation for each leading into 20ms and 10ms with trimethyl aluminium and water has pin hole
Silver-alumina composite nanostructured substrate scanning electron microscope (SEM) photograph, Fig. 1 b are the transmission electron microscope picture of single Silver nanorod, and Fig. 1 c are
There is the high-resolution-ration transmission electric-lens figure of the aluminum oxide film of pin hole.Since the reaction temperature of atomic layer deposition is relatively low, Silver nanorod
Pattern is not destroyed, it can be seen that pellumina is very thin, and uniformly coats Silver nanorod, its thickness is about 0.7nm.
Fig. 1 d are silver-alumina composite nano junction that the surface prepared with the trimethyl aluminium and water of different content has pin hole
Structure substrate detection 1 × 10-2Raman spectrogram obtained by M acridines.Wherein uncoated Ag represent that the oblique rod array of fine silver nanometer is thin
Film, 2-1 expressions each led into trimethyl aluminium and water the surface prepared by the atomic layer deposition of 2ms and 1ms with pin hole silver-
Alumina composite nanostructured substrate, the atomic layer deposition that 5-2 expressions each lead into 5ms and 2ms with trimethyl aluminium and water are made
Standby surface has silver-alumina composite nanostructured substrate of pin hole, and 10-5 expressions are each led into trimethyl aluminium and water
Surface prepared by the atomic layer deposition of 10ms and 5ms has silver-alumina composite nanostructured substrate of pin hole, 20-10 tables
Show silver-aluminium oxide that there is pin hole with the surface prepared by trimethyl aluminium and water each lead into the atomic layer deposition of 20ms and 10ms
Composite nanostructure substrate, 40-20 expressions are each led into trimethyl aluminium and water prepared by the atomic layer deposition of 40ms and 20ms
Surface there is silver-alumina composite nanostructured substrate of pin hole, 80-40 expressions each lead into 80ms with trimethyl aluminium and water
There is silver-alumina composite nanostructured substrate of pin hole with the surface prepared by the atomic layer deposition of 40ms.
Since acridine only can be adsorbed on silver surface, without forming chemical bond, the oblique rod array of fine silver nanometer between aluminium oxide
The adsorbable more acridine of film, the Raman spectrum obtained are strong；The surface-enhanced Raman effects substrate that surface has pin hole passes through
The silver surface absorption acridine of exposure in pin hole, absorption point is less, and the Raman spectrum obtained is weak.It is oblique in fine silver nanometer according to acridine
Rod array film and surface have the 1043cm of the surface-enhanced Raman effects substrate of pin hole-1The intensity rate of raman characteristic peak,
It can show that (the silver-colored surface area of not oxidized aluminium film covering accounts for whole surface enhancing Ramam effect for the needle hole ratio of different base
The ratio of substrate surface product).As the amount for being passed through trimethyl aluminium and water increases, needle hole ratio declines, it can be achieved that to needle hole ratio
16%~5% adjusting.
Embodiment 2
1. silicon chip or glass substrate acetone, alcohol, deionized water order are cleaned by ultrasonic and dried；
2. pretreated substrate is fixed on the sample stage of electron beam evaporation deposition machine；
3. at room temperature, use metallic silver as target, by the chamber of electron beam evaporation deposition machine be evacuated to vacuum for 5 ×
10- 5Pa；
4. adjusting the incidence angle of electron beam to 86 °, and sample stage is set to be rotated with the speed of 6rpm, on the substrate of sample stage
Tilt the oblique rod array film of silver nanoparticle that growing nano-rod length is 600nm；
5. by low temperature ald method, to 60 DEG C, the flow for controlling trimethyl aluminium and water is heating cavity
20sccm, it is respectively 10ms and 5ms to be passed through the time, has pin hole for one layer in the oblique rod array film surface uniform deposition of silver nanoparticle
Aluminum oxide film, obtaining surface has silver-alumina composite nanostructured of pin hole, as surface-enhanced Raman effects substrate；
6. silver-alumina composite that the oblique rod array film of the silver nanoparticle prepared in step 4-5 and surface have pin hole is received
Rice structural substrates are in sodium chloride (NaCl, 30mM), hydrogen peroxide (H2O2, 2.2%) and Cymag (NaCN, 50ppb) solution in point
Not Jin Pao 3h, 0.5h and 3h, and observe its pattern change.
In Fig. 2, Fig. 2 a, 2c, 2e are respectively the oblique rod array film of silver nanoparticle that will be prepared in embodiment 2 in sodium chloride
(NaCl, 30mM), hydrogen peroxide (H2O2, 2.2%) and Cymag (NaCN, 50ppb) solution in soak 3h, 0.5h and 3h after
Scanning electron microscope (SEM) photograph；Fig. 2 b, 2d, 2f are respectively silver-alumina composite nano junction that the surface prepared in embodiment 2 is had pin hole
Structure substrate is in sodium chloride (NaCl, 30mM), hydrogen peroxide (H2O2, 2.2%) and Cymag (NaCN, 50ppb) solution in soak
Scanning electron microscope (SEM) photograph after 3h, 0.5h and 3h.Wherein uncoated Ag NRs represent the oblique rod array film of fine silver nanometer, Ag NRs@
Al2O3Represent that surface has silver-alumina composite nanostructured substrate of pin hole.
Since sodium chloride, hydrogen peroxide and sodium cyanide solution are respectively provided with corrosivity, the oblique rod array film of silver nanoparticle quickly by
Corrosion, for pattern there occurs great variety (Fig. 2 a, 2c, 2e), substrate stability is poor, is unfavorable for surface-enhanced Raman detection；And table
Face has silver-alumina composite nanostructured substrate of pin hole, and the aluminum oxide film on its surface uniformly coats Silver nanorod, and pin
Hole number is few, can effectively isolate internal Silver nanorod with extraneous bad border, make its nanostructured holding stabilization (Fig. 2 b,
2d, 2f).
Embodiment 3
1. silicon chip substrate or glass substrate acetone, alcohol, deionized water order are cleaned by ultrasonic and dried；
2. pretreated substrate is fixed on the sample stage of electron beam evaporation deposition machine；
3. at room temperature, using metallic silver as target, the chamber of electron beam evaporation deposition machine is evacuated to 8 × 10- 5The height of Pa
Vacuum；
4. adjusting the incidence angle of electron beam to 88 °, and sample stage is set to be rotated with the speed of 10rpm, in the substrate of sample stage
Updip sideways growth nanorod length is the straight rod array film of silver nanoparticle cylinder of 400nm；
5. by low temperature ald method, to 50 DEG C, the flow for controlling trimethyl aluminium and water is heating cavity
20sccm, it is respectively 80ms and 40ms to be passed through the time, is had for one layer in the straight rod array film surface uniform deposition of silver nanoparticle cylinder
The aluminum oxide film of pin hole, obtaining surface has silver-alumina composite nanostructured of pin hole；
6. silver prepared by step 5-alumina composite nanostructured substrate is different as surface enhanced Raman substrate, detection
The sodium cyanide solution (1ppb-100ppb) and 2,6- pyridinedicarboxylic acids solution (1 × 10 of concentration-8M-1×10-4M)。
In Fig. 3, the surface prepared in embodiment 3 is had silver-alumina composite nano junction of pin hole by Fig. 3 a, Fig. 3 c respectively
Structure substrate is used to detect the Raman spectrum line chart obtained when trace Cymag and 2,6- pyridinedicarboxylic acid, and Fig. 3 b, Fig. 3 d are correspondingly
For the quantitative analysis figure to raman scattering intensity-molecular concentration relation.
Cymag only can be adsorbed on silver surface, and chemical bond cannot be formed between aluminium oxide, and silver of the surface with pin hole-
Alumina composite nanostructured substrate adsorbs nacn by the silver surface of exposure in pin hole, obtains Surface enhanced Raman spectroscopy,
And available for the quantitative analysis of raman scattering intensity-sodium cyanide concentration relation；2,6- pyridinedicarboxylic acids not only can be adsorbed on silver surface,
Chemical bond can be formed with aluminium oxide, therefore surface has silver-alumina composite nanostructured substrate of pin hole can be by pin hole
Exposed silver surface, aluminum oxide film film surface while absorption 2,6- pyridinedicarboxylic acids, obtains Surface enhanced Raman spectroscopy, detection is dense
The degree limit is low, and available for the quantitative analysis of raman scattering intensity -2,6- pyridinedicarboxylic acid concentration relationship.
Claims (5)
1. a kind of surface has the surface-enhanced Raman effects substrate of pin hole, it is characterised in that in Silver nanorod array film table
One layer of aluminum oxide film with pin hole of face uniform deposition, and needle hole ratio is controllable, obtaining surface has silver-aluminium oxide of pin hole
Composite nanostructure, as surface-enhanced Raman effects substrate；
The Silver nanorod array film is oblique rod array film or the straight rod array film of cylinder, Silver nanorod length are
There is pin hole, thickness to be less than 1nm for 400nm~700nm, the surface of the aluminum oxide film；
The needle hole ratio refers to that the silver-colored surface area of not oxidized aluminium film covering accounts for whole surface enhancing Ramam effect base
The ratio of bottom surface area；The scope of needle hole ratio is 16%~5%.
2. a kind of preparation method of surface-enhanced Raman effects substrate according to claim 1, it is characterised in that using inclining
Sideways growth method, in deposition on substrate metallic silver, obtains Silver nanorod array film；Using low temperature ald technology in silver
One layer of aluminum oxide film with pin hole of nano-stick array thin film surface uniform deposition, obtaining surface has silver-oxidation of pin hole
Aluminium composite nanostructure, as surface-enhanced Raman effects substrate.
3. preparation method according to claim 2, it is characterised in that prepare Silver nanorod array using growing method is tilted
The step of film is：At room temperature, substrate is fixed on the sample stage of electron beam evaporation deposition machine；Metallic silver is used as target
Material, vacuum is evacuated to as 3 × 10 by electron beam evaporation deposition machine cavity room- 5Pa~8 × 10- 5Pa；Adjusting electron beam incident angle is
85 °~88 °, and make sample stage static or rotated with the speed of 6rpm~10rpm, grow Silver nanorod on the substrate of sample stage
Array film.
4. preparation method according to claim 2, it is characterised in that there is pin using low temperature ald technology deposition
During the aluminum oxide film in hole, Silver nanorod array film well prepared in advance is put into the middle part of atomic layer deposition reaction cavity, chamber
Temperature is 50 DEG C~70 DEG C；It is passed through using trimethyl aluminium and water as precursors, alternating in reaction cavity, flow is
20sccm, being passed through the time and adjust the needle hole ratio of aluminum oxide film, trimethyl aluminium and moisture by varying two kinds of presomas
2~80ms and 1~40ms are not passed through it.
5. preparation method according to claim 4, it is characterised in that as the amount for being passed through trimethyl aluminium and water increases, pin
Boring ratio example declines, and the scope of needle hole ratio is 16%~5%.
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| CN108680556A (en) * | 2018-05-14 | 2018-10-19 | 清华大学 | A kind of silver aluminium solid solution nanorod surfaces enhancing Raman substrate and preparation method thereof |
| CN109161849B (en) * | 2018-07-19 | 2019-10-11 | 西安交通大学 | A kind of ordered porous array and preparation method thereof of silver tantalum composite material building |
| CN111896521A (en) * | 2020-08-06 | 2020-11-06 | 中国电子科技集团公司第四十六研究所 | Method for detecting coverage rate of large-area continuous thin film of transition metal sulfide |
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