CN110132935A - A kind of preparation method enhancing surface-enhanced raman scattering substrate - Google Patents
A kind of preparation method enhancing surface-enhanced raman scattering substrate Download PDFInfo
- Publication number
- CN110132935A CN110132935A CN201910417340.7A CN201910417340A CN110132935A CN 110132935 A CN110132935 A CN 110132935A CN 201910417340 A CN201910417340 A CN 201910417340A CN 110132935 A CN110132935 A CN 110132935A
- Authority
- CN
- China
- Prior art keywords
- flame
- carbon black
- preparation
- support substrates
- nanostructure
- 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
Landscapes
- Health & Medical Sciences (AREA)
- 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)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A kind of preparation method enhancing surface-enhanced raman scattering substrate, belongs to technical field of material.Enhancing surface-enhanced raman scattering substrate includes one layer of porous structure carbon black nano particle and noble metal (gold, silver etc.) nano particle for being attached to above-mentioned nano grain surface.Above-mentioned porous structure carbon black nano particle can be used various flammable non-toxic organic objects and deposit preparation by flame method on support substrates, and one layer of noble metal nano particles are deposited using physical gas phase deposition technology on its surface as template in porous structure carbon black nano particle, substrate is detected for SERS to construct porous carbon black/noble metal granule composite construction.High repeatability, low cost, property is stable, can be prepared on a large scale by can be obtained on support substrates by simple flame deposited and physical gas phase deposition technology by the present invention, and the SERS active-substrate of high sensitivity, a kind of easy new way is provided for the preparation and application scientific research of SERS substrate.
Description
Technical field
The invention belongs to technical field of material, be related to it is a kind of it is at low cost, homogeneity is good, it is repeated it is high, can be extensive
The preparation method of the surface enhanced Raman scattering substrate of preparation.
Background technique
Surface Raman enhancement (Surface enhanced Raman Scattering, SERS) technology, which utilizes, has Gao Ling
It is a kind of hypersensitive spectral technique suitable for low concentration detection to monomolecular detection that the active substrate of sensitivity, which is realized,.Cause
Its high sensitivity, it is easy to detect the advantages that become common point of the fields such as biology, diagnostics, environmental monitoring, medical diagnosis on disease
Analysis means.There are two aspects: Chemical enhancement and Electromagnetic enhancement for the enhancing mechanism of surface Raman enhancement scattering substrate；Chemical enhancement
Principle is: generating photoinduced charge transfer between noble metal nano particles and the probe molecule for being attracted to substrate surface, is formed
New surface metal compound polarizability increase, have under the irradiation of exciting light appropriate Raman enhance scattering effect.Electromagnetism
The principle of enhancing is: generating local electric field between noble metal nano particles and forms surface plasmon resonance, covibration causes
Local electric field enhanced strength is that Raman scattering strength is multiplied.Base is learnt according to the working principle that surface Raman enhancement scatters
Can bottom surface form be the important factor in order that SERS effect occur and determine SERS signal power, so SERS substrate is always
It is the research hotspot in the field.There is special nanostructure, the substrate of morphology controllable by preparation surface, reach highly sensitive inspection
The purpose of survey.
The current preparation method for commonly preparing SERS substrate mainly has: chemical vapour deposition technique, physical vaporous deposition,
Electrochemical redox method, chemical etching method, metal-sol method, oldered array printing technology etc..Common SERS substrate preparation
Method there is preparation process it is complicated, at high cost, experimental period is long the problems such as, largely limit the popularization of SERS technology
With application.
Therefore, a kind of function admirable is developed, is easy to large scale preparation, is low in cost, is easy to use, and testing result can
The high high-performance SERS substrate of repeatability becomes particularly important.
Summary of the invention
It is an object of the invention to solve preparation time, cost of material, sensitivity etc. in existing SERS substrate technology of preparing
Aspect is difficult to the problem of coordinating and unifying, provides a kind of quick, cheap, low consumption SERS substrate preparation method.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
A kind of preparation method enhancing surface-enhanced raman scattering substrate, enhancing surface-enhanced raman scattering substrate include one layer of porous knot
Structure carbon black nano particle and noble metal (gold, silver etc.) nano particle for being attached to above-mentioned nano grain surface.Preparation method packet
Include following steps:
The first step, using flame method, the porous carbon black nanostructure of deposition three-dimensional, realization are three-dimensional more on support substrates surface
The building of hole carbon black nanoparticle structure body, specifically:
Support substrates are placed in combustible organic upper horizontal and are aligned it with flame source center；Define substrate and flame
The distance in source is d, as shown in Fig. 1.Flame source is lighted, regulates and controls the relative altitude d of flame and support substrates, one layer can be deposited
Three-dimensional porous carbon black nanostructure.The thickness of the three-dimensional porous carbon black nanostructure according to sedimentation time and can support
The regulation of the relative position of substrate and flame；
Support substrates and mask plate can also be placed in combustible organic upper horizontal and be aligned it with flame source center,
Wherein, mask plate is placed in support substrates lower surface；Flame source is lighted, the relative altitude of flame and support substrates, Ji Kechen are regulated and controled
The three-dimensional porous carbon black nanostructure of one layer model of product.The thickness of the three-dimensional porous carbon black nanostructure of the medelling
Degree can regulate and control according to the relative position of sedimentation time and support substrates and flame.
Second step, the three-dimensional porous carbon black nano junction of three-dimensional porous carbon black nanostructure or medelling that the first step is obtained
Support membrane of the structure as SERS substrate, in your gold that its surface uses physical vaporous deposition to deposit a layer thickness as 10-500nm
Metal nano-particle layer, to construct out carbon black/metal nanoparticle composite S ERS substrate.The support membrane is also referred to as crucial lining
Bottom surface pattern manipulates layer.The noble metal nano particles size can be regulated and controled according to physical vapour deposition (PVD) relevant parameter.Root
According to SERS enhance characteristic, can size, pattern, grain spacing to metal nanoparticle be finely adjusted guarantee SERS signal enhancing reach
To suitable strength, the sensitivity for minimal feeding is promoted.
Further, combustable organic object described in the first step is any combustible organic that can produce carbon black nanostructure, packet
Include alcohol, kerosene, candle etc..
Further, support substrates described in the first step include quartz plate, silicon wafer, titanium dioxide silicon wafer, stainless steel and aluminium oxide
Substrate etc..
Further, the relative altitude of flame and support substrates described in the first step is 0 < d < 7cm；The sedimentation time is
10s-180s。
Further, noble metal described in second step is capable of forming active hot spot, including gold nanoparticle, Nano silver grain or
The composite nanoparticle of the two.
Further, the physical gas phase deposition technology described in second step for deposited metal film includes magnetron sputtering
Method, ion beam deposition, vapour deposition method, atomic force sedimentation, pulsed deposition method.
Compared with prior art, the invention has the benefit that the present invention on support substrates by passing through simple fire
Flame deposition and physical gas phase deposition technology can be obtained high repeatability, low cost, property stabilization, can be prepared on a large scale, and
The SERS active-substrate of high sensitivity provides a kind of easy new way for the preparation and application scientific research of SERS substrate.
Detailed description of the invention
Fig. 1 is carbon black manufacturing process schematic diagram in embodiment 1；
Fig. 2 is carbon black manufacturing process schematic diagram in embodiment 2；
Fig. 3 is the vertical view scanning electron microscope (SEM) photograph (SEM) of carbon black nanostructure in embodiment 1；
Fig. 4 is carbon black nanostructure cross section scanning electron microscope (SEM) photograph (SEM) in embodiment 1；
Fig. 5 is the vertical view scanning electron microscope (SEM) photograph (SEM) of the SERS substrate prepared in embodiment 1；
Fig. 6 is the cross section scanning electron microscope (SEM) photograph (SEM) of the SERS substrate prepared in embodiment 1；
Fig. 7 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 1；
Fig. 8 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 2；
Fig. 9 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 3；
Figure 10 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 4；
Figure 11 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 6；
Figure 12 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 10；
Figure 13 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 11；
Figure 14 is the Raman signal of R6G measured by the SERS substrate for preparing in embodiment 14.
Specific embodiment
As shown in Fig. 1, support substrates are placed in flame source (such as alcolhol burner) upper horizontal and makes itself and flame source center
Alignment, lights flame source, lights flame source and start to deposit, three-dimensional porous carbon black nano junction can be obtained in time 10s-180s
Hereafter support membrane of the structure as SERS substrate utilizes physical gas phase deposition technology deposition one on the carbon black structural body surface of preparation
Layer noble metal film finally obtains carbon black/metal nanoparticle composite S ERS substrate with a thickness of 10nm-500nm.
As shown in Fig. 2, support substrates and mask plate are placed in flame source (such as alcolhol burner) upper horizontal, and makes itself and fire
The alignment of flame source center, lights flame source, lights flame source and start to deposit, three-dimensional porous carbon can be obtained in time 10s-180s
Hereafter support membrane of the black nanostructure as SERS substrate utilizes physical vapour deposition (PVD) skill on the carbon black structural body surface of preparation
Art deposits one layer of noble metal film and finally obtains carbon black/metal nanoparticle composite S ERS base with a thickness of 10nm-500nm
Bottom.
The present invention can be more easily to understand by reference to the detailed description below to embodiment and attached drawing.However, this
Invention can have many different forms to implement, and should not be construed as limited to embodiment described in this paper.These embodiments
It is intended to keep the disclosure complete and informs those skilled in the art in the invention's the scope of the present invention.It is three-dimensional more
The macrostructure of hole carbon black nanostructure can be supported directly on silicon wafer using the porous carbon black nanostructure of flame source deposition three-dimensional
Body, the mask plate that also can use plurality of specifications are prepared into the three-dimensional porous carbon black nanostructure supporter of different mode.
Embodiment 1
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and it is to start to deposit at 3cm that support substrates, which are placed in flame kernel d value, and time 10s can be obtained three
Tie up porous carbon black nanostructure as SERS substrate support membrane (attached drawing 3 be this example in using flame method deposition three-dimensional it is more
The stereoscan photograph (SEM) of hole carbon black nano-particle layer, as shown, the distribution of carbon black nanostructure size dimension is more equal
One, and wherein have apparent hole configurations), silver nano-grain, setting are deposited using magnetic control sputtering device in carbon black nanostructure
Magnetic control sputtering device operating current is 60mA, operating voltage 40mV, operating power 20W, sedimentation time 30min is obtained
(attached drawing 4 is that this example sputters the SEM figure after silver nano-grain using magnetron sputtering to SERS substrate, as shown, silver nano-grain
Size and form is more uniform, and is similarly formed 3 D stereo hole configurations).
Attached drawing 7 is the SERS substrate that is prepared using this example to rhodamine (biological stain, R6G) various concentration aqueous solution
Raman spectrogram when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detectable concentration of this example preparation
The limit is lower than 10-11Mol/L shows excellent SERS feature.
Embodiment 2
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates and mask plate are placed in alcolhol burner upper horizontal as shown in Fig. 2 and make itself and fire
The alignment of flame source center, lights flame source, and it is to start to deposit at 3cm that support substrates, which are placed in flame kernel d value, time 10s, i.e.,
The three-dimensional porous carbon black nanostructure of medelling can be obtained as the support membrane of SERS substrate, and (attached drawing 3 is as shown in 2 illustration of attached drawing
Using the stereoscan photograph (SEM) of the three-dimensional porous carbon black nano-particle layer of flame method deposition in this example, as shown, carbon
Black nanostructure size dimension distribution is more uniform, and wherein has apparent hole configurations), magnetic is utilized in carbon black nanostructure
It controls sputter and deposits silver nano-grain, setting magnetic control sputtering device operating current is 60mA, operating voltage 40mV, operating power are
20W, sedimentation time 30min, obtaining SERS substrate, (attached drawing 4 is after this example sputters silver nano-grain using magnetron sputtering
SEM figure, as shown, silver nano-grain size and form is more uniform, and is similarly formed 3 D stereo hole configurations).
Attached drawing 8 is the SERS substrate that is prepared using this example to rhodamine (biological stain, R6G) various concentration aqueous solution
Raman spectrogram when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detectable concentration of this example preparation
The limit is lower than 10-11Mol/L shows excellent SERS feature.
Embodiment 3
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is burnt using kerosene
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and it is to start to deposit at 5cm that support substrates, which are placed in flame kernel d value, time 50s, it can be obtained
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate deposits silver using magnetic control sputtering device in carbon black nanostructure
Nano particle, setting magnetic control sputtering device operating current is 60mA, operating voltage 40mV, operating power 20W, and sedimentation time is
30min obtains SERS substrate, and silver nano-grain size and form is more uniform, forms 3 D stereo hole configurations.
Attached drawing 9 is that the SERS substrate prepared with this experiment exists to rhodamine (biological stain, R6G) various concentration aqueous solution
Raman spectrogram when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detectable concentration pole of this example preparation
Limit is lower than 10-11Mol/L shows very excellent SERS feature.
Embodiment 4
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize candle combustion
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 1cm, time 30s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, is received in carbon black nanostructure using magnetic control sputtering device deposition silver
Rice grain, setting magnetic control sputtering device operating current be 60mA, operating voltage 40mV, operating power 20W, sedimentation time is
30min obtains SERS substrate, and silver nano-grain size and form is more uniform, forms 3 D stereo hole configurations.
Attached drawing 10 is water-soluble to rhodamine (biological stain, R6G) various concentration for the SERS substrate prepared using this example
Raman spectrogram of the liquid when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detection of this example preparation are dense
It spends the limit and is lower than 10-11Mol/L, attached drawing 6 be the SERS substrate that is prepared using this example to rhodamine (biological stain, R6G) no
With Raman spectrogram of the concentration of aqueous solution when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS of this example preparation
The substrate detectable concentration limit is lower than 10-11Mol/L shows very excellent SERS feature.
Embodiment 5
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, ion beam depositing silver nanoparticle is utilized in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations, can express excellent SERS feature.
Embodiment 6
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is burnt using kerosene
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 150s be can be obtained
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate utilizes ion beam depositing silver nanoparticle in carbon black nanostructure
Particle obtains SERS substrate, forms 3 D stereo hole configurations.
Attached drawing 11 is water-soluble to rhodamine (biological stain, R6G) various concentration for the SERS substrate prepared using this example
Raman spectrogram of the liquid when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detection of this example preparation are dense
It spends the limit and is lower than 10-10Mol/L shows very excellent SERS feature.
Embodiment 7
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize candle combustion
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, ion beam depositing silver nanoparticle is utilized in carbon black nanostructure
Grain obtains SERS substrate, forms three-dimensional porous structure, can express very excellent SERS feature.
Embodiment 8
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, vapor deposition silver nanoparticle is utilized in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations, can express very excellent SERS feature.
Embodiment 9
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is burnt using kerosene
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, vapor deposition silver nanoparticle is utilized in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations, can express very excellent SERS feature.
Embodiment 10
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize candle combustion
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, vapor deposition silver nanoparticle is utilized in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations.
Attached drawing 12 is water-soluble to rhodamine (biological stain, R6G) various concentration for the SERS substrate prepared using this example
Raman spectrogram of the liquid when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detection of this example preparation are dense
It spends the limit and is lower than 10-10Mol/L shows very excellent SERS feature.
Embodiment 11
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 50s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, deposits silver nanoparticle using atomic force in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations.
Attached drawing 13 is water-soluble to rhodamine (biological stain, R6G) various concentration for the SERS substrate prepared using this example
Raman spectrogram of the liquid when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detection of this example preparation are dense
It spends the limit and is lower than 10-11Mol/L shows excellent SERS characteristic.
Embodiment 12
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is burnt using kerosene
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, deposits silver nanoparticle using atomic force in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations, can express excellent SERS characteristic.
Embodiment 13
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize candle combustion
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 100s be can be obtained
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate deposits silver nanoparticle using atomic force in carbon black nanostructure
Particle obtains SERS substrate, forms 3 D stereo hole configurations, can express excellent SERS characteristic.
Embodiment 14
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, deposits silver nanoparticle using impulse method in carbon black nanostructure
Grain obtains SERS substrate, forms 3 D stereo hole configurations.
Attached drawing 14 is water-soluble to rhodamine (biological stain, R6G) various concentration for the SERS substrate prepared using this example
Raman spectrogram of the liquid when Raman excitation optical wavelength is 532.8nm, as seen from the figure, the SERS substrate detection of this example preparation are dense
It spends the limit and is lower than 10-11Mol/L shows very excellent SERS feature.
Embodiment 15
Support dried for standby after quartz plate (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is fired using kerosene
The flame flame envelope of burning deposits carbon black.As shown in Fig. 1 flame source upper horizontal place support substrates and make its in flame source
Heart alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s be can be obtained
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate deposits silver nanoparticle using impulse method in carbon black nanostructure
Particle obtains SERS substrate, forms 3 D stereo hole configurations, can express excellent SERS feature.
Embodiment 16
Support dried for standby after titanium dioxide silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize wax
Burned flame flame envelope of lighting up deposits carbon black.Support substrates are placed in flame source upper horizontal as shown in Fig. 1 and make itself and flame
The alignment of source center, lights flame source, by support substrates as flame kernel d value to start to deposit at 3cm, time 10s
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate is obtained, deposits silver using impulse method in carbon black nanostructure
Nano particle obtains SERS substrate, forms 3 D stereo hole configurations, can express excellent SERS feature.
Embodiment 17
Support dried for standby after stainless steel (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.It is fired using alcohol
The flame flame envelope of burning deposits carbon black.As shown in Fig. 1 alcolhol burner upper horizontal place support substrates and make its in flame source
Heart alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s be can be obtained
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate deposits gold using magnetic control sputtering device in carbon black nanostructure
Nano particle, setting magnetic control sputtering device operating current be 60mA, operating voltage 40mV, operating power 20W, sedimentation time
For 20min, SERS substrate is obtained, can express excellent SERS feature.
Embodiment 18
Support dried for standby after aluminum oxide substrate (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize wine
Smart burned flame flame envelope deposits carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame
The alignment of source center, lights flame source, by support substrates as flame kernel d value to start to deposit at 3cm, time 10s
Support membrane of the three-dimensional porous carbon black nanostructure as SERS substrate is obtained, ion beam depositing gold is utilized in carbon black nanostructure
Nano particle obtains SERS substrate, can express excellent SERS feature.
Embodiment 19
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, vapor deposition gold nano is utilized in carbon black nanostructure
Grain, obtains SERS substrate, can express excellent SERS feature.
Embodiment 20
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, deposits gold nano using atomic force in carbon black nanostructure
Grain, obtains SERS substrate, can express excellent SERS feature.
Embodiment 21
Support dried for standby after silicon wafer (1cm*1cm) is cleaned with acetone, alcohol, deionized water respectively.Utilize alcohol burn
Flame flame envelope deposit carbon black.Support substrates are placed in alcolhol burner upper horizontal as shown in Fig. 1 and make itself and flame source center
Alignment, lights flame source, and by support substrates as flame kernel d value to start to deposit at 3cm, time 10s can be obtained three
Support membrane of the porous carbon black nanostructure as SERS substrate is tieed up, deposits gold nano using impulse method in carbon black nanostructure
Grain, obtains SERS substrate, can express excellent SERS feature.
Examples detailed above proves: simple and practical SERS substrate is synthesized using Technical Design proposed in this paper, it is significant to drop
Low experimental period, low consumption and high sensitivity.The above-mentioned description to example simultaneously is the ordinary skill for the ease of the technical field
Personnel can understand and apply the invention.Person skilled in the art obviously easily can make various repair to these examples
Change, and applies the general principles described here to other examples without having to go through creative labor.Therefore, of the invention
Examples of implementation here are not limited to, those skilled in the art's announcement according to the present invention for the improvement of the invention made and is repaired
Changing all should be within protection scope of the present invention.
Claims (10)
1. a kind of preparation method for enhancing surface-enhanced raman scattering substrate, which is characterized in that the preparation method includes following step
It is rapid:
The first step, using flame method on support substrates surface the porous carbon black nanostructure of deposition three-dimensional, realize three-dimensional porous carbon
The building of black nanoparticle structure body, specifically: support substrates are placed in combustible organic upper horizontal and make itself and flame source
Center alignment, defining substrate is d at a distance from flame source；Flame source is lighted, the relative altitude d of flame and support substrates is regulated and controled,
One layer of three-dimensional porous carbon black nanostructure can be deposited；The thickness of the three-dimensional porous carbon black nanostructure can be according to heavy
The relative position of product time and support substrates and flame regulates and controls；
The three-dimensional porous carbon black nanostructure of second step, the three-dimensional porous carbon black nanostructure that the first step is obtained or medelling is made
For the support membrane of SERS substrate, uses physical vaporous deposition to deposit a layer thickness on its surface and received for the noble metal of 10-500nm
Rice grain layer, to construct out carbon black/metal nanoparticle composite S ERS substrate；The noble metal nano particles size can root
Regulated and controled according to physical vapour deposition (PVD) relevant parameter.
2. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 1, which is characterized in that the first step
In, support substrates and mask plate can also be placed in combustible organic upper horizontal and be aligned it with flame source center, wherein
Mask plate is placed in support substrates lower surface；Flame source is lighted, regulates and controls the relative altitude of flame and support substrates, one layer can be deposited
The three-dimensional porous carbon black nanostructure of medelling；The thickness of the three-dimensional porous carbon black nanostructure of the medelling can root
Regulate and control according to the relative position of sedimentation time and support substrates and flame.
3. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 1 or 2, which is characterized in that institute
The relative altitude of the flame and support substrates stated is 0 < d < 7cm；The sedimentation time is 10s-180s.
4. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 1 or 2, which is characterized in that institute
The support substrates stated include quartz plate, silicon wafer, titanium dioxide silicon wafer, stainless steel and aluminum oxide substrate.
5. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 3, which is characterized in that described
Support substrates include quartz plate, silicon wafer, titanium dioxide silicon wafer, stainless steel and aluminum oxide substrate.
6. a kind of preparation method of enhancing surface-enhanced raman scattering substrate described according to claim 1 or 2 or 5, which is characterized in that
The noble metal includes the composite nanoparticle of gold nanoparticle, Nano silver grain or both.
7. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 3, which is characterized in that described
Noble metal includes the composite nanoparticle of gold nanoparticle, Nano silver grain or both.
8. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 4, which is characterized in that described
Noble metal includes the composite nanoparticle of gold nanoparticle, Nano silver grain or both.
9. a kind of preparation method of enhancing surface-enhanced raman scattering substrate described according to claim 1 or 2 or 5 or 7 or 8, special
Sign is, the physical gas phase deposition technology for deposited metal film include magnetron sputtering method, ion beam deposition,
Vapour deposition method, atomic force sedimentation, pulsed deposition method.
10. a kind of preparation method for enhancing surface-enhanced raman scattering substrate according to claim 3, which is characterized in that described
The physical gas phase deposition technology for deposited metal film include magnetron sputtering method, ion beam deposition, vapour deposition method, atom
Power sedimentation, pulsed deposition method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910417340.7A CN110132935B (en) | 2019-05-20 | 2019-05-20 | Preparation method of enhanced surface Raman scattering substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910417340.7A CN110132935B (en) | 2019-05-20 | 2019-05-20 | Preparation method of enhanced surface Raman scattering substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110132935A true CN110132935A (en) | 2019-08-16 |
| CN110132935B CN110132935B (en) | 2021-05-07 |
Family
ID=67571413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910417340.7A Active CN110132935B (en) | 2019-05-20 | 2019-05-20 | Preparation method of enhanced surface Raman scattering substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110132935B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865847A (en) * | 2010-06-18 | 2010-10-20 | 清华大学 | Preparation method of Raman scattering substrate |
| JP2011076948A (en) * | 2009-09-30 | 2011-04-14 | Toray Ind Inc | Conductive complex, and negative electrode for lithium ion battery |
| CN102759520A (en) * | 2012-05-14 | 2012-10-31 | 北京化工大学 | Preparation method of active radical with surface-enhanced Raman scattering (SERS) effect |
| WO2013065747A1 (en) * | 2011-10-31 | 2013-05-10 | 有限会社マイテック | Metal complex quantum crystals and surface enhanced raman scattering (sers) analysis method of biochemical substance using same |
| CN103924188A (en) * | 2014-05-07 | 2014-07-16 | 山东师范大学 | Method for graphene in-situ growth on insulation substrate through double-flame method under atmospheric environment |
| CN106986320A (en) * | 2017-03-29 | 2017-07-28 | 上海出入境检验检疫局工业品与原材料检测技术中心 | A kind of magnetic ordered mesoporous carbon composite material of metal oxide insertion and preparation method and application |
| TW201812851A (en) * | 2016-09-23 | 2018-04-01 | 國立成功大學 | Flexible raman substrate and method for manufacturing the same |
| CN108872189A (en) * | 2018-06-01 | 2018-11-23 | 徐州医科大学 | The titanium dioxide nanoplate array SERS base material and its preparation method and application of nanometer modified by silver |
| KR101932195B1 (en) * | 2017-10-27 | 2018-12-24 | 한국과학기술원 | Method of manufacturing surface enhanced raman spectroscopy substrates |
-
2019
- 2019-05-20 CN CN201910417340.7A patent/CN110132935B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011076948A (en) * | 2009-09-30 | 2011-04-14 | Toray Ind Inc | Conductive complex, and negative electrode for lithium ion battery |
| CN101865847A (en) * | 2010-06-18 | 2010-10-20 | 清华大学 | Preparation method of Raman scattering substrate |
| WO2013065747A1 (en) * | 2011-10-31 | 2013-05-10 | 有限会社マイテック | Metal complex quantum crystals and surface enhanced raman scattering (sers) analysis method of biochemical substance using same |
| CN102759520A (en) * | 2012-05-14 | 2012-10-31 | 北京化工大学 | Preparation method of active radical with surface-enhanced Raman scattering (SERS) effect |
| CN103924188A (en) * | 2014-05-07 | 2014-07-16 | 山东师范大学 | Method for graphene in-situ growth on insulation substrate through double-flame method under atmospheric environment |
| TW201812851A (en) * | 2016-09-23 | 2018-04-01 | 國立成功大學 | Flexible raman substrate and method for manufacturing the same |
| CN106986320A (en) * | 2017-03-29 | 2017-07-28 | 上海出入境检验检疫局工业品与原材料检测技术中心 | A kind of magnetic ordered mesoporous carbon composite material of metal oxide insertion and preparation method and application |
| KR101932195B1 (en) * | 2017-10-27 | 2018-12-24 | 한국과학기술원 | Method of manufacturing surface enhanced raman spectroscopy substrates |
| CN108872189A (en) * | 2018-06-01 | 2018-11-23 | 徐州医科大学 | The titanium dioxide nanoplate array SERS base material and its preparation method and application of nanometer modified by silver |
Non-Patent Citations (2)
| Title |
|---|
| L. B. HE ET AL: "Systematic investigation of the SERS efficiency and SERS hotspots in gas-phase deposited Ag nanoparticle assemblies", 《PHYS.CHEM.CHEM.PHYS》 * |
| 张朋月 等: "石墨烯/双金属纳米颗粒基底的制备及实验研究", 《中国激光》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110132935B (en) | 2021-05-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6198957B2 (en) | Surface enhanced Raman spectroscopic substrate and method for producing the same | |
| Chan et al. | Using patterned arrays of metal nanoparticles to probe plasmon enhanced luminescence of CdSe quantum dots | |
| Haes et al. | Solution-phase, triangular Ag nanotriangles fabricated by nanosphere lithography | |
| Zhang et al. | Spherical nanoparticle arrays with tunable nanogaps and their hydrophobicity enhanced rapid SERS detection by localized concentration of droplet evaporation | |
| Chattopadhyay et al. | Surface-enhanced Raman spectroscopy using self-assembled silver nanoparticles on silicon nanotips | |
| Tabatabaei et al. | Optical properties of silver and gold tetrahedral nanopyramid arrays prepared by nanosphere lithography | |
| Yang et al. | One-pot synthesis of monodispersed silver nanodecahedra with optimal SERS activities using seedless photo-assisted citrate reduction method | |
| Dong et al. | Simultaneous SEF and SERRS from silver fractal-like nanostructure | |
| Bhatnagar et al. | Fluorescence enhancement from nano-gap embedded plasmonic gratings by a novel fabrication technique with HD-DVD | |
| Weyher et al. | Relationship between the nano-structure of GaN surfaces and SERS efficiency: Chasing hot-spots | |
| Hao et al. | Modified Ag nanoparticles on the regular array structure to improve the optical properties | |
| CN109592635A (en) | A kind of method of controllable preparation composite nano figure line array | |
| Zhang et al. | Surface-enhanced Raman spectroscopy with Au-nanoparticle substrate fabricated by using femtosecond pulse | |
| Höflich et al. | Plasmonic dimer antennas for surface enhanced Raman scattering | |
| Zhang et al. | A study on a hybrid SERS substrates based on arrayed gold nanoparticle/graphene/copper cone cavities fabricated by a conical tip indentation | |
| Feofanov et al. | Nondisturbing and stable SERS-active substrates with increased contribution of long-range component of Raman enhancement created by high-temperature annealing of thick metal films | |
| Jin et al. | Lotus Seedpod Inspired SERS Substrates: A Novel Platform Consisting of 3D Sub‐10 nm Annular Hot Spots for Ultrasensitive SERS Detection | |
| Crouch et al. | Zero-mode waveguide nanophotonic structures for single molecule characterization | |
| Cao et al. | Surface-enhanced fluorescence and application study based on Ag-wheat leaves | |
| Zhu et al. | Increasing polarization-dependent SERS effects by optimizing the axial symmetry of plasmonic nanostructures | |
| Díaz-Núñez et al. | On the large near-field enhancement on nanocolumnar gold substrates | |
| Kato et al. | One-side metal-coated pyramidal cantilever tips for highly reproducible tip-enhanced Raman spectroscopy | |
| US20140293280A1 (en) | Nanosilica sintered glass substrate for spectroscopy | |
| Zhu et al. | Au nanocone array with 3D hotspots for biomarker chips | |
| Wang et al. | Facile synthesis of hybrid silver/porous carbon black substrate for surface-enhanced Raman scattering |
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 |