CN104897638B - Silver-colored germanium copper compound structure device and its production and use - Google Patents
Silver-colored germanium copper compound structure device and its production and use Download PDFInfo
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- CN104897638B CN104897638B CN201510203493.3A CN201510203493A CN104897638B CN 104897638 B CN104897638 B CN 104897638B CN 201510203493 A CN201510203493 A CN 201510203493A CN 104897638 B CN104897638 B CN 104897638B
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Abstract
The invention discloses a kind of silver-colored germanium copper compound structure device and its production and use.Device for copper mesh surface and mesh wall on construct the Ge nanoline for being modified with silver nano-grain thereon, wherein, the mesh diameter of copper mesh is 35~45 μm, and the linear diameter of Ge nanoline is that 100~150nm, line length are 5~15 μm, and the particle diameter of silver nano-grain is 15~35nm；Method is that first copper mesh is placed at 1.5~2.5cm of gold target in sputter, in 1.5~2.5min of sputtering under 15~25mA of sputtering current, obtaining evaporation on its surface and mesh wall has the copper mesh of gold nano grain, reuse chemical gas-phase method growing Ge nanoline thereon, obtain constructing the copper mesh of Ge nanoline on its surface and mesh wall, afterwards, silver nano-grain is sputtered thereon using sputter, purpose product is made.It can as SERS active substrate, be widely used for the content for measuring the rhodamine 6G adhered to thereon or parathion-methyl or adenine or 6 aminopenicillanic acids or novocillin.
Description
Technical field
The present invention relates to a kind of complex structural device and preparation method and purposes, especially a kind of silver-germanium-copper compound structure
Device and its production and use.
Background technology
In existing SERS (SERS) base material, precious metal material Au, Ag, Cu etc. can pass through thing
Reason enhancing reach preferable Raman enhancing effect, so noble metal substrate use it is the most extensive.Simultaneously, although semi-conducting material
Si、ZnO、TiO2, that NiO etc. acts on the enhancing effect that can be provided by Chemical enhancement is limited, but is due to that it has that cost is low, give birth to
Thing and chemical affinity are good and the features such as the complicated nanostructured of high SERS activity is easily generated thereon, are often used as
Skeleton, prepares together with precious metal material and has noble metal physics enhancing compound SERS substrates enhanced with semiconductor active concurrently.
As people deepen continuously to compound SERS substrates research work, gradually recognize to enter with SERS technologies
During row detection, in addition to the SERS base materials for needing high activity, by substrate in itself or extraneous means are to be measured
Thing realizes that the even specific capture of enrichment is also highly important.Such as entitled " Label-free and highly
sensitive biomolecular detection using SERS and electrokinetic
Preconcentration ", Lab on a Chip, 2009,9 (23), 3360. (" are enriched with by surface-enhanced Raman and electric field
Technology is detected to the unmarked high activity of biomolecule ",《Chip lab》The 23rd phase page 3360 of volume 9 in 2009) text
Chapter.The compound SERS substrates referred in this article are that one layer of gold nano is deposited on the polysilicon nanometer post being equipped with a silicon substrate
After grain, sample cell bottom is placed on, while also connecting voltage in detection as electrode, the richness to testing molecule is realized
Collection.Though this SERS substrates can be detected to biomolecule, but also there is weak point, first, exciting light must during detection
It must can be just applied in the substrate of bottom through solution to be measured, can so cause exciting light and the energy of outgoing signal to damage
Lose；Secondly, detectable species is on the low side.
The content of the invention
There is provided a kind of rational in infrastructure, real to overcome weak point of the prior art for the technical problem to be solved in the present invention
With the more silver-germanium-copper compound structure device of detectable species.
The invention solves the problems that another technical problem to provide a kind of preparation of above-mentioned silver-germanium-copper compound structure device
Method.
The invention solves the problems that another technical problem to provide a kind of purposes of above-mentioned silver-germanium-copper compound structure device.
For solve the present invention technical problem, the technical scheme used for：Silver-germanium-copper compound structure device includes lining
Bottom, particularly,
The substrate is to have been constructed on copper mesh, the surface of the copper mesh and mesh wall on Ge nanoline, the Ge nanoline
It is modified with silver nano-grain；
The mesh diameter of the copper mesh is 35~45 μm；
The linear diameter of the Ge nanoline is that 100~150nm, line length are 5~15 μm；
The particle diameter of the silver nano-grain is 15~35nm.
For solve the present invention another technical problem, another technical scheme used for：Above-mentioned silver-germanium-copper is multiple
The preparation method for closing structure devices is as follows including chemical vapour deposition technique, particularly key step：
Step 1, first copper mesh is placed at 1.5~2.5cm of gold target in sputter, in sputtering under 15~25mA of sputtering current
1.5~2.5min, obtaining evaporation on its surface and mesh wall has the copper mesh of gold nano grain, reuses chemical gas-phase method in its table
Evaporation has growing Ge nanoline on the copper mesh of gold nano grain on face and mesh wall, obtains having constructed germanium on its surface and mesh wall
The copper mesh of nano wire；
Step 2, using sputter in sputtering silver nanoparticle on the copper mesh that Ge nanoline is constructed on its surface and mesh wall
Grain, is made silver-germanium-copper compound structure device.
It is used as the further improvement of the preparation method of silver-germanium-copper compound structure device：
Preferably, in being sputtered on copper mesh before gold nano grain, first it is cleaned by ultrasonic using ethanol and deionized water successively.
Preferably, it is that evaporation on its surface and mesh wall is had into gold using the process of chemical gas-phase method growing Ge nanoline
The copper mesh of nano particle is placed in the mixed atmosphere of germane and argon gas, is incubated at least 30min at 310~350 DEG C, wherein, germane with
Germane and the mixed gas of 60mL/min argon gas that the mixed atmosphere of argon gas is 3.5~4.5mL/min of flow.
Preferably, the process of sputtering silver nano-grain is the copper mesh of Ge nanoline will to be constructed on its surface and mesh wall
It is placed at silver-colored 1.5~2.5cm of target in sputter, in 7~8min of sputtering under 15~25mA of sputtering current.
For solve the present invention another technical problem, another technical scheme used for：Above-mentioned silver-germanium-copper is multiple
Close structure devices purposes be,
Using silver-germanium-copper compound structure device as the active substrate of SERS, laser Raman spectroscopy is used
The instrument rhodamine 6G that adheres to thereon of measurement or parathion-methyl or adenine or 6-amino-penicillanic acid or novocillin contain
Amount.
It is used as the further improvement of the purposes of silver-germanium-copper compound structure device：
Preferably, silver-germanium-copper compound structure device is placed in 10-5~10-9Mol/L adenine solution or 6- amino is blue or green
The surface of mould alkanoic acid molecular solution or novocillin solution, and in adenine solution or 6-amino-penicillanic acid molecular solution
Copper mesh of the positive electrode with being connected silver-germanium-copper compound structure device negative electricity interpolar application -1V voltage or in novocillin
What the voltage that the negative electricity interpolar of copper mesh of the positive electrode with being connected silver-germanium-copper compound structure device in solution applies 1V was constituted
Component as SERS active substrate；Beneficial to its enrichment to testing molecule, so as to be greatly enhanced detection
Sensitivity.
Preferably, the excitation wavelength of laser Raman spectrometer is that 532nm, power output are 0.2~0.4mW, the time of integration
For 3~7s.
Beneficial effect relative to prior art is：
First, obtained purpose product is characterized using ESEM and its subsidiary power spectrum tester respectively, by
Its result understands that purpose product is modified with the germanium nanometer of silver nano-grain to be constructed on the surface of copper mesh and mesh wall thereon
Line；Wherein, the mesh diameter of copper mesh is 35~45 μm, and the linear diameter of Ge nanoline is that 100~150nm, line length are 5~15 μm,
The particle diameter of silver nano-grain is 15~35nm.This purpose product being assembled into by copper mesh, Ge nanoline and silver nano-grain, both
Due to the hierarchy that semiconductor Germanium and noble silver are constituted, and incorporate the Chemical enhancement of semiconductor Germanium and the thing of noble silver
Reason enhancing SERS effects, make it have higher SERS activity；The regular hole having again by copper mesh is in Raman spectrum mirror
Remain to clearly to be differentiated under head, and make it be easy to contact with solution in exciting light alignment holes when carrying out SERS detections
The Ge nanoline of sparse modified by silver nanoparticles is to realize detection；Due also to copper mesh is electrically connected upper powered with testing molecule institute
After the opposite voltage of lotus, the enrichment to testing molecule is realized, so as to greatly increase the sensitivity of detection；More because in enrichment
During, purpose product is in the top of solution to be measured, without by muddy opaque solution to exciting light and outgoing
The adverse effect of signal, thus easily enrichment process can be monitored in real time.
Second, using obtained purpose product as SERS active-substrate, through respectively to rhodamine 6G, parathion-methyl, gland
Purine, 6-amino-penicillanic acid and novocillin carry out the test of multiple many batches under various concentrations, and it can be low by concentration
To 10-6Mol/L above-mentioned determinand is all detected, and its detection uniformity and repeatability in the multiple spot in purpose product and
Any point is all very good.Drawn after purpose product is placed in corresponding solution and applies voltage constituent components as surface enhanced
During the active substrate of graceful scattering, its sensitivity detected is greatly improved.
Third, preparation method is simple, science, efficiently.Rational in infrastructure, practicality has not only been made, species has been can detect more
Purpose product --- silver-germanium-copper compound structure device, also makes it have detection trace rhodamine 6G or parathion-methyl or gland
The performance of purine or 6-amino-penicillanic acid or novocillin, more there is the characteristics of preparation process is simple and direct, cost is low；And then make
Purpose product is extremely easy to be widely used in the real-time analysis to pollutant, it is had extensively in fields such as environment, chemistry, biologies
General application prospect.
Brief description of the drawings
Fig. 1 is to copper mesh, intermediate product --- copper mesh, the purpose product of Ge nanoline are constructed on its surface and mesh wall
One of ESEM (SEM) and the result for being characterized its subsidiary power spectrum (EDS) tester are used respectively.Wherein, Fig. 1 a
For the SEM image of copper mesh；Fig. 1 b are the SEM image of intermediate product；Fig. 1 c are the part of intermediate product Blocked portion shown in Fig. 1 b
The SEM image being exaggerated；The SEM image that Fig. 1 d have been the partial enlargement of intermediate product Blocked portion shown in Fig. 1 c；Fig. 1 e are mesh
Product SEM image, the illustration in its upper right corner is its high magnification SEM image；Fig. 1 f are intermediate product and the EDS of purpose product
Spectrogram.
Fig. 2 is that purpose product is placed in into 10-6In mol/L adenine solution and apply conduct after -1V voltage constituent components
During the active substrate of SERS, one of result characterized using laser Raman spectrometer to it.Wherein, scheme
2a is the SERS spectrograms that measure under different time；Fig. 2 b are adenine in 735cm-1Place's feature peak intensity prolongs with electric field enrichment time
Long change curve.
Fig. 3 is that purpose product is enriched with after 6-amino-penicillanic acid and novocillin respectively, uses laser Raman spectrometer
One of result characterized to it.Wherein, Fig. 3 a are that purpose product is placed in into 10-7Mol/L 6-amino-penicillanic acid solution
In and apply after -1V voltage constituent components, be used as the SERS spectral lines pair before and after the active substrate 30min of SERS
Than figure；Fig. 3 b are that purpose product is placed in into 10-7In mol/L novocillin solution and apply after 1V voltage constituent components, as
SERS spectral line comparison diagrams before and after the active substrate 30min of SERS.
Embodiment
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Buy or be voluntarily made from market first：
Mesh diameter is 35~45 μm of copper mesh；Germane；Argon gas.
Then,
Embodiment 1
What is prepared concretely comprises the following steps：
Step 1, after being first cleaned by ultrasonic successively using ethanol and deionized water for 35 μm of copper mesh to mesh diameter, put
At gold target 1.5cm in sputter, in sputtering 1.5min under sputtering current 25mA, obtaining being deposited on its surface and mesh wall has
The copper mesh of gold nano grain.The copper mesh that has gold nano grain will be deposited on its surface and mesh wall again and is placed in the mixed of germane and argon gas
Close atmosphere, be incubated 35min at 310 DEG C, wherein, the mixed atmosphere of germane and argon gas is flow 3.5mL/min germane and 60mL/
The mixed gas of min argon gas, obtains being similar to having constructed Ge nanoline on its surface shown in Fig. 1 b~Fig. 1 d and mesh wall
Copper mesh.
Step 2, the silver-colored target 1.5cm copper mesh that Ge nanoline is constructed on its surface and mesh wall being placed in sputter
Place, in sputtering 7min under sputtering current 25mA, is made and is similar to shown in Fig. 1 e, and silver-germanium as shown in the curve in Fig. 1 f-
Copper compound structure device.
Embodiment 2
What is prepared concretely comprises the following steps：
Step 1, after being first cleaned by ultrasonic successively using ethanol and deionized water for 38 μm of copper mesh to mesh diameter, put
At gold target 1.8cm in sputter, in sputtering 1.8min under sputtering current 23mA, obtaining being deposited on its surface and mesh wall has
The copper mesh of gold nano grain.The copper mesh that has gold nano grain will be deposited on its surface and mesh wall again and is placed in the mixed of germane and argon gas
Close atmosphere, be incubated 34min at 320 DEG C, wherein, the mixed atmosphere of germane and argon gas is flow 3.8mL/min germane and 60mL/
The mixed gas of min argon gas, obtains being similar to having constructed Ge nanoline on its surface shown in Fig. 1 b~Fig. 1 d and mesh wall
Copper mesh.
Step 2, the silver-colored target 1.8cm copper mesh that Ge nanoline is constructed on its surface and mesh wall being placed in sputter
Place, in sputtering 7.3min under sputtering current 23mA, be made be similar to silver shown in Fig. 1 e, and as shown in the curve in Fig. 1 f-
Germanium-copper compound structure device.
Embodiment 3
What is prepared concretely comprises the following steps：
Step 1, after being first cleaned by ultrasonic successively using ethanol and deionized water for 40 μm of copper mesh to mesh diameter, put
At gold target 2cm in sputter, in sputtering 2min under sputtering current 20mA, obtaining evaporation on its surface and mesh wall has Jenner
The copper mesh of rice grain.The copper mesh that evaporation has gold nano grain on its surface and mesh wall is placed in the gaseous mixture of germane and argon gas again
Atmosphere, be incubated 33min at 330 DEG C, wherein, the mixed atmosphere of germane and argon gas for flow 4mL/min germane and 60mL/min
The mixed gas of argon gas, obtains constructing the copper mesh of Ge nanoline on its surface as shown in Fig. 1 b~Fig. 1 d and mesh wall.
Step 2, the copper mesh that Ge nanoline is constructed on its surface and mesh wall is placed at the silver-colored target 2cm in sputter,
In sputtering 7.5min under sputtering current 20mA, it is made as shown in fig. le, and silver-germanium-copper as shown in the curve in Fig. 1 f is multiple
Close structure devices.
Embodiment 4
What is prepared concretely comprises the following steps：
Step 1, after being first cleaned by ultrasonic successively using ethanol and deionized water for 43 μm of copper mesh to mesh diameter, put
At gold target 2.3cm in sputter, in sputtering 2.3min under sputtering current 18mA, obtaining being deposited on its surface and mesh wall has
The copper mesh of gold nano grain.The copper mesh that has gold nano grain will be deposited on its surface and mesh wall again and is placed in the mixed of germane and argon gas
Close atmosphere, be incubated 31min at 340 DEG C, wherein, the mixed atmosphere of germane and argon gas is flow 4.3mL/min germane and 60mL/
The mixed gas of min argon gas, obtains being similar to having constructed Ge nanoline on its surface shown in Fig. 1 b~Fig. 1 d and mesh wall
Copper mesh.
Step 2, the silver-colored target 2.3cm copper mesh that Ge nanoline is constructed on its surface and mesh wall being placed in sputter
Place, in sputtering 7.8min under sputtering current 18mA, be made be similar to silver shown in Fig. 1 e, and as shown in the curve in Fig. 1 f-
Germanium-copper compound structure device.
Embodiment 5
What is prepared concretely comprises the following steps：
Step 1, after being first cleaned by ultrasonic successively using ethanol and deionized water for 45 μm of copper mesh to mesh diameter, put
At gold target 2.5cm in sputter, in sputtering 2.5min under sputtering current 15mA, obtaining being deposited on its surface and mesh wall has
The copper mesh of gold nano grain.The copper mesh that has gold nano grain will be deposited on its surface and mesh wall again and is placed in the mixed of germane and argon gas
Close atmosphere, be incubated 30min at 350 DEG C, wherein, the mixed atmosphere of germane and argon gas is flow 4.5mL/min germane and 60mL/
The mixed gas of min argon gas, obtains being similar to having constructed Ge nanoline on its surface shown in Fig. 1 b~Fig. 1 d and mesh wall
Copper mesh.
Step 2, the silver-colored target 2.5cm copper mesh that Ge nanoline is constructed on its surface and mesh wall being placed in sputter
Place, in sputtering 8min under sputtering current 15mA, is made and is similar to shown in Fig. 1 e, and silver-germanium as shown in the curve in Fig. 1 f-
Copper compound structure device.
The purposes of silver-germanium-copper compound structure device is,
Using silver-germanium-copper compound structure device as SERS active substrate, it is or silver-germanium-copper is multiple
Close structure devices and be placed in 10-5~10-9Mol/L adenine solution or 6-amino-penicillanic acid molecular solution or novocillin is molten
The surface of liquid, and positive electrode in adenine solution or 6-amino-penicillanic acid molecular solution is with being connected silver-germanium-copper composite junction
The negative electricity interpolar application -1V of the copper mesh of structure device voltage or the positive electrode in novocillin solution are with being connected silver-germanium-copper
The component that the voltage that the negative electricity interpolar of the copper mesh of complex structural device applies 1V is constituted as SERS work
Property substrate, measure the rhodamine 6G that adheres to thereon or parathion-methyl or adenine using laser Raman spectrometer or 6- amino be blue or green
The content of mould alkanoic acid or novocillin, obtain as be similar to Fig. 2 or Fig. 3 shown in result；Wherein, laser Raman spectrometer
Excitation wavelength be 532nm, power output be 0.2~0.4mW, the time of integration be 3~7s.
Obviously, those skilled in the art can to silver-germanium-copper compound structure device and preparation method thereof of the present invention and
Purposes carries out various changes and modification without departing from the spirit and scope of the present invention.So, if to these modifications of the invention
Belong to modification within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to comprising these changes and become
Including type.
Claims (8)
1. a kind of silver-germanium-copper compound structure device, including substrate, it is characterised in that：
The substrate is to have constructed on Ge nanoline, the Ge nanoline to modify on copper mesh, the surface of the copper mesh and mesh wall
There is silver nano-grain；
The mesh diameter of the copper mesh is 35~45 μm；
The linear diameter of the Ge nanoline is that 100~150nm, line length are 5~15 μm；
The particle diameter of the silver nano-grain is 15~35nm.
2. the preparation method of silver-germanium-copper compound structure device described in a kind of claim 1, including chemical vapour deposition technique, it is special
Levy and be that key step is as follows：
Step 1, first copper mesh is placed at 1.5~2.5cm of gold target in sputter, in sputtering 1.5 under 15~25mA of sputtering current
~2.5min, obtaining evaporation on its surface and mesh wall has the copper mesh of gold nano grain, reuses chemical gas-phase method in its surface
There is growing Ge nanoline on the copper mesh of gold nano grain with evaporation on mesh wall, obtain having constructed germanium on its surface and mesh wall and receive
The copper mesh of rice noodles；
Step 2, made using sputter in sputtering silver nano-grain on the copper mesh for constructing Ge nanoline on its surface and mesh wall
Get Yin-germanium-copper compound structure device.
3. the preparation method of silver-germanium-copper compound structure device according to claim 2, it is characterized in that in sputtering on copper mesh
Before gold nano grain, first it is cleaned by ultrasonic using ethanol and deionized water successively.
4. the preparation method of silver-germanium-copper compound structure device according to claim 3, it is characterized in that using chemical gaseous phase
The process of method growing Ge nanoline is that the copper mesh that evaporation has gold nano grain on its surface and mesh wall is placed in into germane and argon gas
Mixed atmosphere, be incubated at least 30min at 310~350 DEG C, wherein, the mixed atmosphere of germane and argon gas for flow 3.5~
The mixed gas of 4.5mL/min germane and 60mL/min argon gas.
5. the preparation method of silver-germanium-copper compound structure device according to claim 3, it is characterized in that sputtering silver nanoparticle
Grain process be, silver-colored 1.5~2.5cm of target that the copper mesh that Ge nanoline is constructed on its surface and mesh wall is placed in sputter
Place, in 7~8min of sputtering under 15~25mA of sputtering current.
6. the purposes of silver-germanium-copper compound structure device described in a kind of claim 1, it is characterised in that：
Using silver-germanium-copper compound structure device as the active substrate of SERS, surveyed using laser Raman spectrometer
Measure the content of the rhodamine 6G adhered to thereon or parathion-methyl or adenine or 6-amino-penicillanic acid or novocillin.
7. the purposes of silver-germanium-copper compound structure device according to claim 6, it is characterized in that by silver-germanium-copper composite junction
Structure device is placed in 10-5~10-9Mol/L adenine solution or 6-amino-penicillanic acid molecular solution or novocillin solution
Surface, and positive electrode in adenine solution or 6-amino-penicillanic acid molecular solution is with being connected silver-germanium-copper compound structure device
The negative electricity interpolar application -1V voltage or the positive electrode in novocillin solution of the copper mesh of part are combined with being connected silver-germanium-copper
The component that the voltage that the negative electricity interpolar of the copper mesh of structure devices applies 1V is constituted as SERS active group
Bottom.
8. the purposes of silver-germanium-copper compound structure device according to claim 6 or 7, it is characterized in that laser Raman spectrometer
Excitation wavelength be 532nm, power output be 0.2~0.4mW, the time of integration be 3~7s.
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| CN108802004B (en) * | 2018-06-01 | 2020-12-01 | 徐州医科大学 | Gold nanowire modified titanium dioxide nanorod array SERS substrate material and preparation method and application thereof |
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