CN107356584A - One kind oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver - Google Patents
One kind oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver Download PDFInfo
- Publication number
- CN107356584A CN107356584A CN201710800337.4A CN201710800337A CN107356584A CN 107356584 A CN107356584 A CN 107356584A CN 201710800337 A CN201710800337 A CN 201710800337A CN 107356584 A CN107356584 A CN 107356584A
- Authority
- CN
- China
- Prior art keywords
- zinc
- silver
- zinc oxide
- enhanced raman
- compound micro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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 discloses one kind to aoxidize the compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver, high-quality ZnO micron bars are prepared using Vapor Transport, the zinc oxide micron rods with perfect Echo Wall cavity body structure are chosen as optical microcavity, particle diameter, density distribution gradient, pattern, the metal silver nano-grain that Density Distribution is controllable, optical property is tunable are modified along the zinc oxide micron rods direction of growth using ion sputtering process, constructs oxidation compound micro-cavity structure surface-enhanced Raman (SERS) substrate of zinc-silver.The present invention provides a kind of effective method to build new hypersensitive SERS substrates, solve a series of problems such as traditional SERS substrates preparation process is complicated, Raman signal sensitivity is low simultaneously, the present invention has huge potential application in the detection of future biological medical science, environmental monitoring and life science.
Description
Technical field
The present invention relates to one kind to aoxidize zinc-silver (ZnO-Ag) compound micro-cavity structure surface enhanced Raman substrate preparation method,
Belong to Raman detection field.
Background technology
Due to the light field confinement effect of optical microcavity height, it is passed in optical communication, photodetection, chemical/biological in recent years
The application in the fields such as sense, laser gets most of the attention.Especially, the echo wall type resonator of high-quality how is obtained by the wide of people
General concern.Light wave carries out multiple total reflection in Whispering-gallery-mode (WGM) resonance cavity wall, reduces the energy damage that mirror-reflection is brought
Consumption, so as to obtain high-quality-factor and ultralow thresholding microcavity.ZnO is a kind of direct band gap semiconductor material with wide forbidden band, has height
Up to 60meV exciton bind energy.Compared to other semi-conducting materials, ZnO is that one kind is more suitable at room temperature or higher temperature
The lower ultraviolet light photo semi-conducting material used.In recent years, the UV photoelectric properties of ZnO semi-conducting materials, enjoy always both at home and abroad
The concern of researcher.The ZnO micron bars of section hexagonal structure are the optical microcavities of a natural Whispering-gallery-mode, are utilized
Cavity WGM effects are visited to the interphase interaction by strengthening exciting light and probe molecule so as to obtain ultrasensitive biological signal
Survey.
In addition, metal surface phasmon, is that the collective oscillation of metal surface free electron forms spatially height local
Electronic ripple, have height spatial locality and near field enhancing characteristic, the unique advantage of this spatially height local
Exactly suit the demand for development that modern science and technology integrates to element height, attract global numerous scientists to pay high attention to；And its
Near field enhancing characteristic has widely in fields such as plasmon, surface-enhanced Raman (Raman) and Fluorescence Increasings
Application.Therefore, with reference to argent (Ag) nano particle local surface phasmon (LSPs), optical microcavity WGM effects are utilized
With the synergy of metal nanoparticle LSPs effects, light and molecular detection interphase interaction can be greatly enhanced, lifting is drawn
Graceful signal sensitivity, and ZnO material higher isoelectric point advantage is utilized, can be with the organic material molecule of the low isoelectric point of Electrostatic Absorption, greatly
It is big to simplify conventional surface enhancing Raman scattering (SERS) substrate preparation process.In consideration of it, the present invention is by introducing argent local
Surface plasma bulk effect, construct the hypersensitive SERS substrates of new more compound micro-cavity structures of gradient ZnO-Ag, this invention
Possess huge application prospect in fields such as biomedical detection, environmental monitoring and the life sciences in future.
The content of the invention
Technical problem：Present invention aims at provide a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate of zinc-silver
Preparation method, with reference to ZnO microcavity echo wall die effects and metal Ag local surface phasmon effects, enhance light and detection point
Sub- interphase interaction, lift Raman signal detection sensitivity.
Technical scheme：The invention provides the compound micro-cavity structure surface enhanced Raman substrate preparation side of one kind oxidation zinc-silver
Method, this method comprise the following steps：
Step 1, in mass ratio 1:0.8~1.2 weighs Zinc oxide powder and powdered graphite progress mixed grinding, after grinding
Powder insert in container, as reaction source；
Step 2, Wafer Cleaning drying are used as substrate, and the polishing of silicon chip is covered on the container equipped with reaction source down
And do not contacted with reaction source, the container equipped with reaction source and silicon chip are placed in quartz ampoule one end of both ends open afterwards, and will be whole
Root quartz ampoule is placed in horizontal pipe furnace, is passed through argon gas simultaneously into horizontal pipe furnace and oxygen is reacted, after reaction terminates
Zinc oxide micron rods array is obtained on silicon chip, room temperature is cooled to and takes out；
Step 3, the zinc oxide micron rods with perfect Echo Wall cavity body structure are selected from zinc oxide micron rods array；
Step 4, the zinc oxide micron rods with perfect Echo Wall cavity body structure for choosing step 3 are perpendicularly fixed at new
In silicon chip substrate, the silicon chip substrate is vertically arranged on ion sputtering instrument sample stage afterwards, sputtered on zinc oxide micron rods surface
Metal silver nano-grain, obtain aoxidizing the compound micro-cavity structure surface enhanced Raman substrate of zinc-silver.
Wherein：
Container described in step 1 is quartz boat or corundum boat.
The purity of Zinc oxide powder described in step 1 is 98.00~99.99% by percentage by volume, during described grinding
Between be 10~30min.
Described in step 2 is the step of Wafer Cleaning is dried up：Under conditions of supersonic frequency is 20~60KHz, by silicon
Piece with acetone, absolute ethyl alcohol and deionized water difference 10~15min of ultrasound, is dried up with nitrogen afterwards successively.
Be passed through into horizontal pipe furnace argon gas described in step 2 and oxygen carry out reaction and refer to be in horizontal tube furnace temperature
30~60min is reacted under the conditions of 950~1150 DEG C, the flow that is passed through of wherein argon gas and oxygen is respectively 130~180sccm and 13
~18sccm.
A diameter of 1~20 μm with perfect Echo Wall cavity body structure zinc oxide micron rods described in step 3, length are
0.1~1cm.
The zinc oxide micron rods with perfect Echo Wall cavity body structure that will choose described in step 4 are perpendicularly fixed at new silicon
Refer to one end of zinc oxide micron rods is fixed in new silicon chip substrate with conducting resinl on piece substrate, the other end is located at silicon chip lining
The outside at bottom.
Parallel be fixed in silicon chip substrate of the zinc oxide micron rods for choosing step 3 described in step 4 refers to use conducting resinl
Zinc oxide micron rods are fixed in silicon chip substrate.
Particle diameter, the metal silver nano-grain of density distribution gradient are sputtered on zinc oxide micron rods surface described in step 4
Refer to there is the metal silver nanoparticle along zinc oxide micron rods direction of growth distribution gradient in the sputtering sputtering of zinc oxide micron rods surface
Particle, concrete operation step are as follows：
1), the silicon chip substrate for being fixed with zinc oxide micron rods is disposed vertically on sample stage, while ensures that zinc oxide is micro-
The rice one end of rod away from silicon chip substrate upward and is located at sample stage position, and target position is adjusted to metallic silver target, sample cavity is taken out
Vacuum, air pressure is passed through in protective gas adjusting cavity body afterwards to 30~50Pa；
2), 10~60s of sputtering time is set, sputtering current is 8~20mA, and metal silver nanoparticle is carried out to zinc oxide micron rods
Particle sputters, after the completion of, vacuum breaker takes out sample, obtains aoxidizing the compound micro-cavity structure surface enhanced Raman substrate of zinc-silver.
The crystal growth direction of described silicon chip is<100>.
Beneficial effect：Compared with prior art, the present invention has advantages below：
Firstth, the present invention is prepared for the compound micro-cavity structure surface enhanced Raman substrate of more gradients, hypersensitive ZnO-Ag；
Secondth, the present invention utilize echo wall die and metal local surface phasmon cooperative effect, greatly strengthen light and
Molecular detection interphase interaction, lift Raman signal detection sensitivity；
3rd, the present invention utilizes zinc oxide material higher isoelectric point advantage, the organic material molecule of the low isoelectric point of Electrostatic Absorption
And biomolecule, it enormously simplify traditional SERS substrates preparation process.
Brief description of the drawings
Fig. 1 is ZnO micron bar array scanning electron microscope pictures prepared by the embodiment of the present invention 1：Wherein the upper right corner is inserted
Figure is the scanning electron microscope diagram piece for the ZnO micron bars that embodiment 1 is selected；
Fig. 2 is stimulated radiation spectrum of the compound micro-cavity structures of ZnO-Ag of the preparation of the embodiment of the present invention 1 under the conditions of optical pumping；
Fig. 3 is that particle diameter, the metal Ag nano particles ultraviolet-visible of density gradient distribution prepared by the embodiment of the present invention 1 is inhaled
Spectrum is received, wherein illustration is the optical photograph that sputtering has metal silver nano-grain in quartz substrate；
Fig. 4 is the same concentrations Luo Dan of the compound micro-cavity structure diverse location collections of ZnO-Ag prepared by the embodiment of the present invention 1
Bright 6G (R6G) Raman signal spectrum, wherein illustration are the zinc oxide micron rods optical photographs that sputtering has metal silver nano-grain；
Fig. 5 is the various concentrations Luo Dan of the compound micro-cavity structure same position collections of ZnO-Ag prepared by the embodiment of the present invention 1
Bright 6G (R6G) Raman signal spectrum；Wherein illustration is the dense of the compound micro-cavity structure same position collections of ZnO-Ag prepared by embodiment 1
Spend for 5 × 10-11Mol/L rhodamine 6G (R6G) Raman signal spectrum enlarged drawing；
Fig. 6 is the structural representation of the compound microcavity of oxidation zinc-silver prepared by the embodiment of the present invention 1, and the wherein upper right corner is oxygen
The concentration for changing the compound micro-cavity structure same position collection of zinc-silver is 5 × 10-11Mol/L rhodamine 6G (R6G) Raman signal is put
Big spectrogram.
Embodiment
Further explanation is done to the present invention with reference to embodiment and accompanying drawing.Example below is merely to illustrate this hair
It is bright, but it is not used to limit the practical range of the present invention.
Embodiment 1
1. ZnO powder and graphite powder that selection purity is 99.99% are 1 in mass ratio:0.8 mixed grinding 30min, afterwards
0.8g is taken to insert in quartz boat in the mixture after grinding, as reaction source；
2. by 3cm × 3cm silicon chip (100) through acetone, absolute ethyl alcohol and deionized water successively in supersonic frequency 40KHz bars
15min is respectively washed under part, after being dried up with nitrogen, polishing is covered on the quartz boat equipped with mixed-powder source is placed in down
Both ends open, diameter and length are respectively 4cm and 15cm quartz ampoule one end, and the quartz ampoule for being then equipped with powder source and substrate is put
It is placed in the horizontal quartz tube stove that temperature is 1150 DEG C, argon gas and oxygen is passed through into quartz tube furnace, flow is respectively
150sccm and 15sccm, reacts 60min, and reaction is cooled to room temperature after terminating and takes out sample；
3. selected using light microscope from ZnO micron bar arrays with perfect Echo Wall cavity body structure ZnO micron bars,
Diameter and length are respectively 18 μm and 0.8cm；
4. there is perfect Echo Wall cavity body structure ZnO micron bars to be perpendicularly fixed at 2cm × 2cm selection using conducting resinl
On silicon chip, the silicon chip substrate is disposed vertically on small ion sputter sample stage afterwards, and keep ZnO micron bars away from silicon
One end of piece substrate then sputters particle diameter, density upward and on small ion sputter sample stage on ZnO micron bars surface
Along the metal Ag nano particles of zinc oxide micron rods direction of growth distribution gradient, obtain aoxidizing the compound micro-cavity structure table of zinc-silver
Face strengthens Raman substrate, wherein sputtering parameter：Sputtering current is 14mA, and cavity air pressure is 40Pa, sputtering time 20s.
The compound micro-cavity structures of ZnO-Ag built in the embodiment of the present invention 1 are entered using Raman spectrometer and XRF
Row optical performance test：Result of study shows：The SERS substrates have reached 10 to R6G molecule minimum detection limits-11Magnitude, it draws
Graceful enhancer is up to 1.2 × 1010, this hypersensitive signal detection performance is not only attributable simply to metal Ag nano particle light and excites
Enhancing of the local surface plasma to Raman signal caused by lower, at the same it is relevant with the architectural feature of substrate rule, its
The hexagonal structure of rule for exciting light, propagate by the confinement in cavity, strengthens between 514.5nm exciting lights and R6G probe molecules mutually
Effect, while excited the Ag local surface plasmas on other several faces of cavity to provide important physics advantage.
Embodiment 2
1. ZnO powder and graphite powder that selection purity is 99.00% are 1 in mass ratio:1 mixed grinding 25min, afterwards will
Mixture after grinding takes 0.7g to insert in quartz boat, as reaction source；
2. by 3cm × 3cm silicon chip (100) through acetone, absolute ethyl alcohol and deionized water successively in supersonic frequency 30KHz bars
10min is cleaned under part, after being dried up with nitrogen, polishing is covered on the quartz boat equipped with mixed-powder source is placed in both ends down
Opening, diameter and length are respectively 4cm and 15cm quartz ampoule one end, and the quartz ampoule for being then equipped with powder source and substrate is positioned over
Temperature is in 1100 DEG C of horizontal quartz tube stove, argon gas and oxygen is passed through into quartz tube furnace, flow is respectively 130sccm
And 13sccm, 30min is reacted, reaction is cooled to room temperature after terminating and takes out sample；
3. the ZnO microns with perfect Echo Wall cavity body structure are selected from ZnO micron bar arrays using light microscope
Rod, diameter and length are respectively 1 μm and 0.1cm；
4. there is perfect Echo Wall cavity body structure ZnO micron bars to be perpendicularly fixed at 2cm × 2cm selection using conducting resinl
On silicon chip, the silicon chip substrate is disposed vertically on small ion sputter sample stage afterwards, and keep ZnO micron bars away from silicon
One end of piece substrate then sputters particle diameter, density upward and on small ion sputter sample stage on ZnO micron bars surface
Along the metal Ag nano particles of zinc oxide micron rods direction of growth distribution gradient, obtain aoxidizing the compound micro-cavity structure table of zinc-silver
Face strengthens Raman substrate, wherein sputtering parameter：Sputtering current is 8mA, and cavity air pressure is 30Pa, sputtering time 60s.
Embodiment 3
1. ZnO powder and graphite powder that selection purity is 99.90% are 1 in mass ratio:1 mixed grinding 28min, afterwards will
Mixture after grinding takes 0.75g to insert in quartz boat, as reaction source；
2. by 3cm × 3cm silicon chip (100) through acetone, absolute ethyl alcohol and deionized water successively in supersonic frequency 20KHz bars
10min is cleaned under part, after being dried up with nitrogen, polishing is covered on the quartz boat equipped with mixed-powder source is placed in both ends down
Opening, diameter and length are respectively 4cm and 15cm quartz ampoule one end, and the quartz ampoule for being then equipped with powder source and substrate is positioned over
Temperature is in 950 DEG C of horizontal quartz tube stove, argon gas and oxygen is passed through into quartz tube furnace, flow is respectively 180sccm
And 18sccm, 40min is reacted, reaction is cooled to room temperature after terminating and takes out sample；
3. selected using light microscope from ZnO micron bar arrays micro- with the perfect single ZnO of Echo Wall cavity body structure
Rice rod, diameter and length are respectively 14 μm and 0.6cm；
4. there is perfect Echo Wall cavity body structure ZnO micron bars to be perpendicularly fixed at 2cm × 2cm selection using conducting resinl
On silicon chip, the silicon chip substrate is disposed vertically on small ion sputter sample stage afterwards, and keep ZnO micron bars away from silicon
One end of piece substrate then sputters particle diameter, density upward and on small ion sputter sample stage on ZnO micron bars surface
Along the metal Ag nano particles of zinc oxide micron rods direction of growth distribution gradient, obtain aoxidizing the compound micro-cavity structure table of zinc-silver
Face strengthens Raman substrate, wherein sputtering parameter：Sputtering current is 12mA, and cavity air pressure is 36Pa, sputtering time 40s.
Embodiment 4
1. ZnO powder and graphite powder that selection purity is 99.5% are 1 in mass ratio:1 mixed grinding 20min, afterwards will
Mixture after grinding takes 0.6g to insert in quartz boat, as reaction source；
2. by 3cm × 3cm silicon chip (100) through acetone, absolute ethyl alcohol and deionized water successively in supersonic frequency 60KHz bars
13min is cleaned under part, after being dried up with nitrogen, polishing is covered on the quartz boat equipped with mixed-powder source is placed in both ends down
Opening, diameter and length are respectively 4cm and 15cm quartz ampoule one end, and the quartz ampoule for being then equipped with powder source and substrate is positioned over
Temperature is in 1050 DEG C of horizontal quartz tube stove, argon gas and oxygen is passed through into quartz tube furnace, flow is respectively 165sccm
And 16sccm, 50min is reacted, reaction is cooled to room temperature after terminating and takes out sample；
3. selected using light microscope from ZnO micron bar arrays micro- with the perfect single ZnO of Echo Wall cavity body structure
Rice rod, diameter and length are respectively 7 μm and 0.7cm；
4. there is perfect Echo Wall cavity body structure ZnO micron bars to be perpendicularly fixed at 2cm × 2cm selection using conducting resinl
On silicon chip, the silicon chip substrate is disposed vertically on small ion sputter sample stage afterwards, and keep ZnO micron bars away from silicon
One end of piece substrate then sputters particle diameter, density upward and on small ion sputter sample stage on ZnO micron bars surface
Along the metal Ag nano particles of zinc oxide micron rods direction of growth distribution gradient, obtain aoxidizing the compound micro-cavity structure table of zinc-silver
Face strengthens Raman substrate, wherein sputtering parameter：Sputtering current is 20mA, and cavity air pressure is 50Pa, sputtering time 10s.
Embodiment 5
1. ZnO powder and graphite powder that selection purity is 98.50% are 1 in mass ratio:1 mixed grinding 26min, afterwards will
Mixture after grinding takes 0.45g to insert in quartz boat, as reaction source；
2. by 3cm × 3cm silicon chip (100) through acetone, absolute ethyl alcohol and deionized water successively in supersonic frequency 10KHz bars
11min is cleaned under part, after being dried up with nitrogen, polishing is covered on the quartz boat equipped with mixed-powder source is placed in both ends down
Opening, diameter and length are respectively 4cm and 15cm quartz ampoule one end, and the quartz ampoule for being then equipped with powder source and substrate is positioned over
Temperature is in 980 DEG C of horizontal quartz tube stove, argon gas and oxygen is passed through into quartz tube furnace, flow is respectively 140sccm
And 14sccm, 35min is reacted, reaction is cooled to room temperature after terminating and takes out sample；
3. selected using light microscope from ZnO micron bar arrays micro- with the perfect single ZnO of Echo Wall cavity body structure
Rice rod, diameter and length are respectively 20 μm and 1cm；
4. there is perfect Echo Wall cavity body structure ZnO micron bars to be perpendicularly fixed at 2cm × 2cm selection using conducting resinl
On silicon chip, the silicon chip substrate is disposed vertically on small ion sputter sample stage afterwards, and keep ZnO micron bars away from silicon
One end of piece substrate then sputters particle diameter, density upward and on small ion sputter sample stage on ZnO micron bars surface
The metal Ag nano particles of distribution gradient along the z-axis direction, obtain aoxidizing the compound micro-cavity structure surface-enhanced Raman base of zinc-silver
Bottom, wherein sputtering parameter：Sputtering current is 16mA, and cavity air pressure is 48Pa, sputtering time 15s.
Claims (9)
1. one kind oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver, it is characterised in that：This method includes
Following steps：
Step 1, in mass ratio 1:0.8~1.2 weighs Zinc oxide powder and powdered graphite progress mixed grinding, by the powder after grinding
End is inserted in container, as reaction source；
Step 2, regard Wafer Cleaning drying as substrate, by the polishing of silicon chip it is face-down be covered on the container equipped with reaction source and
Do not contacted with reaction source, the container and silicon chip be placed in one end of the quartz ampoule of both ends open afterwards, and by whole quartz ampoule
It is placed in horizontal pipe furnace, is passed through argon gas simultaneously into horizontal pipe furnace and oxygen is reacted, reacts after terminating on silicon chip
Zinc oxide micron rods array is obtained, room temperature is cooled to and takes out；
Step 3, the zinc oxide micron rods with perfect Echo Wall cavity body structure are selected from zinc oxide micron rods array；
Step 4, the zinc oxide micron rods with perfect Echo Wall cavity body structure for choosing step 3 are perpendicularly fixed at new silicon chip
On substrate, the silicon chip substrate is vertically arranged on ion sputtering instrument sample stage afterwards, in zinc oxide micron rods surface splash-proofing sputtering metal
Silver nano-grain, obtain aoxidizing the compound micro-cavity structure surface enhanced Raman substrate of zinc-silver.
2. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：Container described in step 1 is quartz boat or corundum boat.
3. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：The purity of Zinc oxide powder described in step 1 by percentage by volume be 98.00~99.99%, the grinding when
Between be 10~30min.
4. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：Described in step 2 is the step of Wafer Cleaning is dried up：Under conditions of supersonic frequency is 20~60KHz, by silicon
Piece with acetone, absolute ethyl alcohol and deionized water difference 10~15min of ultrasound, is dried up with nitrogen afterwards successively.
5. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：Argon gas is passed through into horizontal pipe furnace simultaneously and oxygen carries out reaction and referred in horizontal tube furnace temperature described in step 2
Spend under the conditions of 950~1150 DEG C, while be passed through 30~60min of argon gas and oxygen reaction, wherein argon gas and oxygen is passed through stream
Amount is respectively 130~180sccm and 13~18sccm.
6. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：A diameter of 1~20 μm with perfect Echo Wall cavity body structure zinc oxide micron rods described in step 3, length are
0.1~1cm.
7. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：It is new that there are will choose described in step 4 zinc oxide micron rods of perfect Echo Wall cavity body structure to be perpendicularly fixed at
Refer to one end of zinc oxide micron rods is fixed in new silicon chip substrate with conducting resinl in silicon chip substrate, the other end is located at silicon chip
The outside of substrate.
8. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 1, its
It is characterised by：The concrete operation step in zinc oxide micron rods surface splash-proofing sputtering metal silver nano-grain described in step 4 is as follows：
1), the silicon chip substrate for being fixed with zinc oxide micron rods is disposed vertically on ion sputtering instrument sample stage, while ensures oxygen
Change the one end of zinc micron bar away from silicon chip substrate upward and be located at sample stage position, target position is adjusted to metallic silver target, to sample
Product chamber vacuumizes, and is passed through in protective gas adjusting cavity body air pressure afterwards to 30~50Pa；
2), 10~60s of sputtering time is set, sputtering current is 8~20mA, and metal silver nano-grain is carried out to zinc oxide micron rods
Sputtering, after the completion of, vacuum breaker takes out sample, obtains aoxidizing the compound micro-cavity structure surface enhanced Raman substrate of zinc-silver.
9. a kind of oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver as claimed in claim 8, its
It is characterised by：Described protective gas is argon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710800337.4A CN107356584B (en) | 2017-09-07 | 2017-09-07 | Preparation method of zinc oxide-silver composite microcavity structure surface enhanced Raman substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710800337.4A CN107356584B (en) | 2017-09-07 | 2017-09-07 | Preparation method of zinc oxide-silver composite microcavity structure surface enhanced Raman substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107356584A true CN107356584A (en) | 2017-11-17 |
| CN107356584B CN107356584B (en) | 2020-08-11 |
Family
ID=60291402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710800337.4A Active CN107356584B (en) | 2017-09-07 | 2017-09-07 | Preparation method of zinc oxide-silver composite microcavity structure surface enhanced Raman substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107356584B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456848A (en) * | 2018-03-28 | 2018-08-28 | 吉林师范大学 | A kind of Ag/FeS composite stratified materials SERS substrates and preparation method thereof |
| CN110261366A (en) * | 2019-07-09 | 2019-09-20 | 吉林师范大学 | Have both the preparation method of the difunctional micro-composites of detection and degrading pesticide |
| CN115184339A (en) * | 2022-09-08 | 2022-10-14 | 海澳华(黑龙江)生物医药技术有限公司 | Method for rapidly detecting viruses based on portable Raman spectrometer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045548A (en) * | 2007-03-12 | 2007-10-03 | 东南大学 | Preparation method of echo wall die laser cavity based on zinc oxide single crystal micronano dish |
| CN102798624A (en) * | 2012-08-08 | 2012-11-28 | 中国科学院长春光学精密机械与物理研究所 | Near-field Raman biosensor based on echo wall mode |
| CN103311803A (en) * | 2013-06-13 | 2013-09-18 | 东南大学 | Graphene-enhancing zinc oxide ultraviolet laser microcavity and preparation method thereof |
-
2017
- 2017-09-07 CN CN201710800337.4A patent/CN107356584B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045548A (en) * | 2007-03-12 | 2007-10-03 | 东南大学 | Preparation method of echo wall die laser cavity based on zinc oxide single crystal micronano dish |
| CN102798624A (en) * | 2012-08-08 | 2012-11-28 | 中国科学院长春光学精密机械与物理研究所 | Near-field Raman biosensor based on echo wall mode |
| CN103311803A (en) * | 2013-06-13 | 2013-09-18 | 东南大学 | Graphene-enhancing zinc oxide ultraviolet laser microcavity and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JUNFENG LU等: "SERS-active ZnO/Ag hybrid WGM microcavity for ultrasensitive dopamine detection", 《APPLIED PHYSICS LETTERS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456848A (en) * | 2018-03-28 | 2018-08-28 | 吉林师范大学 | A kind of Ag/FeS composite stratified materials SERS substrates and preparation method thereof |
| CN110261366A (en) * | 2019-07-09 | 2019-09-20 | 吉林师范大学 | Have both the preparation method of the difunctional micro-composites of detection and degrading pesticide |
| CN115184339A (en) * | 2022-09-08 | 2022-10-14 | 海澳华(黑龙江)生物医药技术有限公司 | Method for rapidly detecting viruses based on portable Raman spectrometer |
| CN115184339B (en) * | 2022-09-08 | 2022-12-23 | 海澳华(黑龙江)生物医药技术有限公司 | Method for rapidly detecting viruses based on portable Raman spectrometer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107356584B (en) | 2020-08-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107356584A (en) | One kind oxidation compound micro-cavity structure surface enhanced Raman substrate preparation method of zinc-silver | |
| Yin et al. | Plasmon-enhanced upconversion luminescence on vertically aligned gold nanorod monolayer supercrystals | |
| Yin et al. | Remarkable enhancement of upconversion fluorescence and confocal imaging of PMMA Opal/NaYF4: Yb 3+, Tm 3+/Er 3+ nanocrystals | |
| Jiang et al. | A sensitive, uniform, reproducible and stable SERS substrate has been presented based on MoS 2@ Ag nanoparticles@ pyramidal silicon | |
| CN102180438A (en) | Manufacturing method of tunable triangular metal nano particle array structure | |
| CN102212790A (en) | Preparation method of noble metal/submicron spherical shell arrays | |
| CN108827938A (en) | Surface enhanced Raman scattering substrate based on dielectric grating-metallic film Yu metal nanoparticle composite construction | |
| CN106757372A (en) | A kind of methylamine lead iodine perovskite monocrystalline microcavity and preparation method thereof | |
| Zhou et al. | Ag loaded TiO2 nanotube photonic crystals self-doped Ti3+ periodically by anodization process and their performance of surface enhanced Raman scattering | |
| CN110044866A (en) | A kind of transverse direction nano-cavity array structure SERS substrate and preparation method thereof | |
| Shin et al. | Giant enhancement of the Raman response due to one-dimensional ZnO nanostructures | |
| CN108956574A (en) | Dual wavelength metal Fano resonant structure for two-photon fluorescence enhancing | |
| CN108333166A (en) | The surface enhanced Raman scattering substrate and preparation method of induced with laser | |
| Gao et al. | Single-layer gold nanoparticle film enhances the upconversion luminescence of a single NaYbF4: 2% Er3+ microdisk | |
| CN103756671B (en) | A kind of sandwich structure and preparation method strengthening light-emitting film photoluminescence luminous intensity | |
| CN106770162A (en) | A kind of substrate of SERS for detecting sweetener and its preparation method and application | |
| CN103149194B (en) | A kind of preparation method of Surface enhanced raman spectroscopy matrix | |
| CN112563874B (en) | Room temperature light-excited zinc oxide phonon vibration terahertz laser | |
| Piard et al. | Photoswitching in diarylethene nanoparticles, a trade-off between bulk solid and solution: towards balanced photochromic and fluorescent properties | |
| Zhang et al. | Generalized green synthesis of diverse LnF 3–Ag hybrid architectures and their shape-dependent SERS performances | |
| CN107359217B (en) | A kind of quick response ultraviolet light detector and preparation method | |
| CN109540791A (en) | A kind of liquid core light guide reactor and the method for preparing SERS chip using it | |
| JP2002277397A (en) | Molecular sensor, and raman spectroscopy | |
| Vančo et al. | Interference enhancement in SERS spectra of rhodamine 6G: Relation to reflectance | |
| CN107328750A (en) | A kind of high activity, surface enhanced Raman scattering substrate of high homogeneity and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |