CN109187486A - A kind of Nano silver piece and preparation method thereof and purposes - Google Patents
A kind of Nano silver piece and preparation method thereof and purposes Download PDFInfo
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- CN109187486A CN109187486A CN201811099213.9A CN201811099213A CN109187486A CN 109187486 A CN109187486 A CN 109187486A CN 201811099213 A CN201811099213 A CN 201811099213A CN 109187486 A CN109187486 A CN 109187486A
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- 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
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Abstract
The present invention provides a kind of preparation method of Nano silver piece, include the following steps: that (1) configures electrolyte；(2) using electrochemical method in deposition on substrate Nano silver piece；(3) it anneals.Wherein, it is 30-40 DEG C that sedimentary condition described in step (2), which is electrolyte temperature, sedimentation time 4-6min.The present invention also provides one kind Nano silver piece as made from method made above and its applications in Raman spectrum base.The invention has preparation method simple process, reproducible, at low cost, can produce in batches；Porous Nano silver piece obtained can effectively inhibit to reunite, and have porous pattern, uniformity is preferable, forms a large amount of Raman active sites, has many advantages, such as lower SERS detectable limit.
Description
Background technique
Surface Enhanced Raman Scattering Spectrum (Surface Enhanced Raman Scattering, SERS) is a kind of fast
Fast, highly sensitive, lossless detection technique, so far in fields such as the researchs such as Surface Science, electrochemistry, analytical chemistry and biology
Show huge application prospect.
For most of molecules, Raman scattering effect is very weak, and scattered light intensity is about the 10 of incident intensity-6-10-9, significantly limit the application and development of Raman spectrum.1977, Jeanmaire and VanDuyne discovery when point
Son is placed on coarse precious metal surface or nearby rear Raman signal can be significantly enhanced, and this effect was referred to as later
Surface enhanced Raman scattering.Later, with the development of nanotechnology and the exploitation of all kinds of Raman spectrometers, SERS technology is gradually sent out
Exhibition is got up.Even to this day, the detection limit of SERS technology has been able to reach ppb grades, or even can be achieved on monomolecular detection.
On the one hand, the preparation method of existing SERS substrate is more complicated, and SERS application is made to be very limited, therefore,
Simple and quick preparation SERS substrate will keep being more widely applied for SERS quick；On the other hand, the particle ruler of surface enhanced substrate
Degree, shape and arrangement are closely related with SERS activity, and to improve SERS activity, researchers at home and abroad are exploring always preparation
The method of the higher substrate of SERS activity；In addition, the generally existing group of SERS substrate reinforcing material prepared using electrochemical method
Poly- phenomenon is serious, is not easy to be formed good porous pattern, the feature that Raman active site is few.
Summary of the invention
In view of this, the invention is directed to a kind of Nano silver piece and preparation method thereof and purposes, with a kind of simple
Electrochemical method preparation synthesis there is the Nano silver piece of porous pattern, and be used as Raman spectrum base, should
Substrate has preferable SERS activity, and preparation method is easy to operate.
In order to achieve the above objectives, the technical solution of the invention is achieved in that
A kind of preparation method of Nano silver piece, includes the following steps:
(1) electrolyte is configured；
(2) using electrochemical method in deposition on substrate Nano silver piece；
(3) it anneals.
Further, it is 30-40 DEG C that sedimentary condition described in step (2), which is electrolyte temperature, sedimentation time 4-6min.
Further, electrolyte described in step (1) includes silver nitrate, citrate and boric acid, the silver nitrate, lemon
Hydrochlorate and boric acid are weighed respectively and are remixed after being each configured to three kinds of solution.
Further, the citrate uses ammonium citrate.
Further, the configuration condition of the silver nitrate, citrate and boric acid solution is respectively as follows: in 30-40 DEG C of thermal station
Stir 0.5h or more.
Further, substrate described in step (2) is monocrystalline silicon piece.
Further, the current density of deposition current described in step (2) is 0.002A/dm2, two interelectrode working distances
From for 8-10cm.
Further, annealing process described in step (3) is to be placed in thermal station, and anneal 10min at 80 DEG C.
Using Nano silver piece made from above-mentioned preparation method, there is porous structure.
Further, the hole of the Nano silver piece is 15-20nm, nanometer sheet thickness 25-30nm, diameter 800nm-
1000nm。
Nano silver piece made from above-mentioned preparation method can be used in Raman spectrum base.
Preferably, the silver nitrate, ammonium citrate and boric acid solution the stirring and dissolving 0.5h or more at 35 DEG C respectively；It is described
Silver nitrate concentration is 0.02mol/L, and ammonium citrate concentration is 0.01mol/L, boric acid concentration 0.5mol/L；The electrolyte exists
It is 35 DEG C that temperature is kept in electrochemical reaction process；Step (2) utilizes electrochemical process, and constant current is in deposition on substrate silver nanoparticle
Piece, constant current current potential are 0.004A, and electro-deposition operating distance is 9cm；Step (2) chip area is 2cm2。
Compared with the existing technology, a kind of Nano silver piece that the invention is related to and preparation method thereof has following with purposes
Advantage:
(1) present invention uses electrochemical process, and the preparation method simple process is reproducible, at low cost, can give birth in batches
It produces.
(2) nanometer sheet can occur agglomeration and lose Raman enhancing activity in general electrochemical deposition process, and through this
Porous Nano silver piece made from the method control reaction time can effectively inhibit to reunite.
(3) variation of electrochemical deposition process temperature will affect the formation of porous pattern, reduce the number in Raman active site
Amount, and the Nano silver piece as made from this method control reaction temperature has porous pattern, forms a large amount of Raman active sites.
(4) a kind of Nano silver piece of the present invention is used for surface enhanced Raman substrate, has lower SERS detectable limit,
Preferable uniformity, lower cost, simple operation and other advantages.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image of Nano silver piece SERS substrate prepared by embodiment 1.
Fig. 2 is to use 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS prepared by embodiment 1
(concentration is respectively 1 × 10 to Raman signal enhancement effect of the substrate to the 4-MBA of various concentration-9M、1×10-10M)。
Fig. 3 is to use 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS prepared by embodiment 1
(concentration is respectively 1 × 10 to Raman signal enhancement effect of the substrate to the 4-MBA of various concentration-3M、1×10-4M、1×10-5M、1
×10-6M、1×10-7M、1×10-8M、1×10-9M、1×10-10M)。
Fig. 4 is the scanning electron microscope image of Nano silver piece SERS substrate prepared by embodiment 2.
Fig. 5 is to use 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS prepared by embodiment 2
For substrate to the Raman signal enhancement effect of the 4-MBA of various concentration, excitation laser wavelength is 532nm, firing time 1s.
Fig. 6 is the scanning electron microscope image of Nano silver piece SERS substrate prepared by embodiment 3.
Fig. 7 is to use 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS prepared by embodiment 3
For substrate to the Raman signal enhancement effect of the 4-MBA of various concentration, excitation laser wavelength is 532nm, firing time 1s.
Fig. 8 is the scanning electron microscope image of the Nano silver piece SERS substrate of different electrodeposition times preparation, and A is deposition
Time 4min, B are sedimentation time 10min, and C is sedimentation time 15min, and D is that (A, B, C, D depositing temperature are equal by sedimentation time 30min
It is 35 DEG C).
Fig. 9 is the scanning electron microscope image of the Nano silver piece SERS substrate of different electrodeposition temperatures preparation, and A is deposition
15 DEG C of temperature, B is 25 DEG C of depositing temperature, and C is 35 DEG C of depositing temperature, and D is that (A, B, C, D sedimentation time is 45 DEG C of depositing temperature
4min)。
Specific embodiment
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；
The experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings come the present invention will be described in detail create.
Embodiment 1
Specific implementation step is as follows:
1. the etching of substrate: silicon single crystal flake being put into 10% HF and etched, taking-up is rinsed with deionized water after 5min, is done
It is dry stand-by.Silicon single crystal flake producer used is No.46 Research Institute, China Electronic Science Group Co., Ltd, and resistivity is < 0.02
Ω cm, crystal orientation are 110 > ± 1 ° <, model N.
2. the cleaning of silver strip electrode: silver strip being carried out wiping with detergent and is cleaned；Silver strip is put into acetone after the completion
It is cleaned by ultrasonic 15min in ultrasonic machine；Silver strip is put into ethyl alcohol after the completion and is cleaned by ultrasonic 15min in ultrasonic machine；After the completion will
Silver strip is put into deionized water is cleaned by ultrasonic 15min in ultrasonic machine.
3. the preparation of electrolyte: weighing the silver nitrate of certain mass, ammonium citrate with electronic balance, boric acid powder is put respectively
Enter in beaker.It is poured into respectively with the deionized water that graduated cylinder measures inequality equipped with silver nitrate, the burning of ammonium citrate and boric acid drug
In cup, respectively at stirring and dissolving 0.5h or more at 35 DEG C.After the completion, three kinds of solution are evenly mixed in electrolytic cell, form electricity
Solve liquid.Wherein, silver nitrate concentration 0.02mol/L, ammonium citrate concentration are 0.01mol/L, boric acid concentration 0.5mol/L.
4. electro-deposition: prepared electrolyte being placed in thermal station, electrolyte temperature is controlled at 35 DEG C, connects with DC power supply
It connects, anode connects silver strip, and cathode connects silicon wafer, opens power supply output, electro-deposition 4min.
5. annealing: by obtained substrate take out, rinsed well, be placed in thermal station with deionized water, at 80 DEG C into
Row annealing 10min.
The scanning electron microscope image of the Nano silver piece SERS substrate of preparation is shown in Fig. 1, used scanning electron microscopy
A, B, C, D amplification factor are respectively in mirror model hitach su8010, acceleration voltage 5kv, extracted current 7uA, Fig. 1
80.0k,50.0k,30.0k,10.0k.As seen from the figure, Nano silver piece made from the present embodiment has porous structure, hole 15-
20nm, nanometer sheet thickness 25-30nm, diameter 800nm-1000nm.
It uses 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS substrate manufactured in the present embodiment
To the Raman signal enhancement effect of the 4-MBA of various concentration, testing result is shown in Fig. 2 and Fig. 3, detection method are as follows: by what is obtained
Raman enhancing substrate is cut into 0.1cm × 1cm shape, is respectively placed in 1 × 10-3M and 1 × 10-4M、1×10-5M、1×10-6M、1
×10-7M、1×10-8M、1×10-9M and 1 × 10-10The 4-MBA solution of M concentration impregnates 3h, is drawn using Britain's RENISHAW laser
Graceful spectrometer, excitation wavelength 532nm, sweep time 1s, scanning times 3 times.
The organic molecule and one end and metal surface that thiol group is contained in selection one end have the carboxylic acids compared with extensive chemical effect
The 4-MBA of organic molecule has studied the detection limit of porous Nano silver piece SERS substrate made from the present embodiment as analysis object.
Wherein ,~1590cm-1With~1080cm-1The peak of wave number be expressed as the vibration of aromatic rings.~1180cm-1Other weak band at place
It is C-H vibration.As the concentration of detection molecules reduces, the strength reduction of Raman signal.As seen from Figure 2,1 × 10-9M with
1×10-10Under M concentration ,~1590cm can be still detected-1With~1080cm-1Wave number peak, it is porous made from the present embodiment
The detection of Nano silver piece SERS substrate is limited up to 10-10, illustrate that Nano silver piece made from the present embodiment can be advantageously applied to surface increasing
Strong raman spectrum substrate.
Embodiment 2
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
Electro-deposition: prepared electrolyte is placed in thermal station, is controlled electrolyte temperature at 30 DEG C, is connected with DC power supply
It connects, anode connects silver strip, and cathode connects silicon wafer, opens power supply output, electro-deposition 5min.
The scanning electron microscope image of the Nano silver piece SERS substrate of preparation is shown in Fig. 4, and as seen from the figure, the present embodiment is made
Nano silver piece have porous structure, hole 15-20nm, nanometer sheet thickness 25-30nm, diameter 800nm-1000nm.
It uses 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS substrate manufactured in the present embodiment
To the Raman signal enhancement effect of the 4-MBA of various concentration, testing result is shown in Fig. 5, as seen from Figure 5,1 × 10-9M and 1
×10-10Under M concentration ,~1590cm can be still detected-1With~1080cm-1Wave number peak, it is porous made from the present embodiment
The detection of Nano silver piece SERS substrate is limited up to 10-10, illustrate that Nano silver piece made from the present embodiment can be advantageously applied to surface increasing
Strong raman spectrum substrate.
Embodiment 3
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
Electro-deposition: prepared electrolyte is placed in thermal station, is controlled electrolyte temperature at 40 DEG C, is connected with DC power supply
It connects, anode connects silver strip, and cathode connects silicon wafer, opens power supply output, electro-deposition 6min.
The scanning electron microscope image of the Nano silver piece SERS substrate of preparation is shown in Fig. 6, and as seen from the figure, the present embodiment is made
Nano silver piece have porous structure, hole 15-20nm, nanometer sheet thickness 25-30nm, diameter 800nm-1000nm.
It uses 4-MBA (4- mercaptobenzoic acid) as probe molecule, detects Nano silver piece SERS substrate manufactured in the present embodiment
To the Raman signal enhancement effect of the 4-MBA of various concentration, testing result is shown in Fig. 7, as seen from Figure 7,1 × 10-9M and 1
×10-10Under M concentration ,~1590cm can be still detected-1With~1080cm-1Wave number peak, it is porous made from the present embodiment
The detection of Nano silver piece SERS substrate is limited up to 10-10, illustrate that Nano silver piece made from the present embodiment can be advantageously applied to surface increasing
Strong raman spectrum substrate.
Comparative example 1
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition time is 10min.
Comparative example 2
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition time is 15min.
Comparative example 3
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition time is 30min.
Comparative example 4
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition temperature is 15 DEG C.
Comparative example 5
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition temperature is 25 DEG C.
Comparative example 6
From detection method in addition to the following conditions are different, other are same as Example 1 for specific implementation:
The electrodeposition temperature is 45 DEG C.
Fig. 8 be the Nano silver piece SERS substrate of different electrodeposition times preparation scanning electron microscope image (A in figure,
B, C, D are respectively that embodiment 1, comparative example 1, the scanning electron of Nano silver piece SERS substrate made from comparative example 2 and comparative example 3 are aobvious
Micro mirror figure), A is sedimentation time 4min, and B is sedimentation time 10min, and C is sedimentation time 15min, and D is sedimentation time 30min.
As shown in Figure 8, as electrodeposition time increases, the hole on nanometer sheet surface can disappear, and the stacking of nanometer sheet
Agglomeration is serious, largely reduces Raman active site, reduces SERS effect.
Fig. 9 be the Nano silver piece SERS substrate of different electrodeposition temperatures preparation scanning electron microscope image (A in figure,
B, C, D are respectively that comparative example 4, comparative example 5, the scanning electron of Nano silver piece SERS substrate made from embodiment 1 and comparative example 6 are aobvious
Micro mirror figure), A is 15 DEG C of depositing temperature, and B is 25 DEG C of depositing temperature, and C is 35 DEG C of depositing temperature, and D is 45 DEG C of depositing temperature.
As shown in Figure 9, electrodeposition temperature is too low, and growth tends to a direction, forms dendrite.Electrodeposition temperature rises to
After 35 DEG C, nanometer sheet is formed, and there is porous structure.If electrodeposition temperature is excessively high (45 DEG C), the porous pattern of the nanometer sheet of formation
Tend to disappear, and substrate coverage rate reduces, and influences Raman reinforcing effect.
Above embodiments 1-3 is only the preferred embodiment of the invention, is not intended to limit the invention creation, all
Within the spirit and principle of the invention, any modification, equivalent replacement, improvement and so on should be included in the present invention
Within the protection scope of creation；The above comparative example 1-6, for aiding in illustrating the beneficial effect of the invention.
Claims (10)
1. a kind of preparation method of Nano silver piece, it is characterised in that include the following steps:
(1) electrolyte is configured；
(2) using electrochemical method in deposition on substrate Nano silver piece；
(3) it anneals.
2. the preparation method of Nano silver piece according to claim 1, it is characterised in that: sedimentary condition described in step (2) is
Electrolyte temperature is 30-40 DEG C, sedimentation time 4-6min.
3. the preparation method of Nano silver piece according to claim 1, it is characterised in that: electrolyte described in step (1) includes
Silver nitrate, citrate and boric acid, after the silver nitrate, citrate and boric acid weigh respectively and is each configured to three kinds of solution
It remixes.
4. the preparation method of Nano silver piece according to claim 3, it is characterised in that: the silver nitrate, citrate and boron
The configuration condition of acid solution is respectively as follows: stirring 0.5h or more in 30-40 DEG C of thermal station.
5. the preparation method of Nano silver piece described in claim 1, it is characterised in that: substrate described in step (2) is monocrystalline silicon piece.
6. the preparation method of Nano silver piece according to claim 1, it is characterised in that: deposition current described in step (2)
Current density is 0.002A/dm2, two interelectrode operating distances are 8-10cm.
7. the preparation method of Nano silver piece according to claim 1, it is characterised in that: annealing conditions described in step (3) are
Anneal 10min at 80 DEG C.
8. Nano silver piece made from preparation method described in any one of claim 1-7, it is characterised in that: have porous knot
Structure.
9. Nano silver piece according to claim 8, it is characterised in that: the hole of the Nano silver piece is 15-20nm.
10. application of the Nano silver piece according to claim 8 in Raman spectrum base.
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| CN111364092A (en) * | 2020-03-26 | 2020-07-03 | 新疆艾旗斯德检测科技有限公司 | Preparation method of silver-porous silicon-based surface enhanced Raman scattering biological detection chip |
| WO2020220131A1 (en) | 2019-05-02 | 2020-11-05 | Queen's University At Kingston | Sensor elements having metallic nanostructures and uses thereof |
| CN112611743A (en) * | 2020-12-31 | 2021-04-06 | 安徽中科赛飞尔科技有限公司 | Method for rapidly detecting various drugs in hair |
| CN113279027A (en) * | 2021-04-29 | 2021-08-20 | 安徽大学 | Silver microparticle array and preparation method and application thereof |
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| CN112611743A (en) * | 2020-12-31 | 2021-04-06 | 安徽中科赛飞尔科技有限公司 | Method for rapidly detecting various drugs in hair |
| CN113279027A (en) * | 2021-04-29 | 2021-08-20 | 安徽大学 | Silver microparticle array and preparation method and application thereof |
| CN113279027B (en) * | 2021-04-29 | 2023-08-25 | 安徽大学 | Silver microparticle array and preparation method and application thereof |
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Application publication date: 20190111 |