CN105499602B - A kind of SERS substrate preparation method based on reduction method synthesis gold nano grain - Google Patents
A kind of SERS substrate preparation method based on reduction method synthesis gold nano grain Download PDFInfo
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Abstract
The present invention provides a kind of SERS substrate preparation methods based on reduction method synthesis gold nano grain, the method is by modifying silicon chip surface, realize amination, then gold nano grain is adsorbed on relatively evenly in substrate by the method for restoring chlorauric acid solution, SERS substrate that is repeatable, having high enhancement factor is made.SERS active-substrate prepared by the present invention has many advantages, such as that preparation is simple, repeatability is strong, enhancement factor is big, has the application potential of small molecule and big Molecular Detection.
Description
Technical field
The present invention relates to applications to nanostructures fields, and in particular, to one kind synthesizes gold nano grain based on reduction method
SERS substrate preparation method.
Background technique
From surface enhanced Raman scattering effect (SERS) discovery since by people be applied to environment measuring, chemical analysis,
The numerous areas such as biological medicine.In the past few decades, the preparation of SERS substrate is always a focus of people's research.Generally
For, the metal nanostructures such as gold and silver that the enhancing of Raman signal needs to have certain orderly above substrate, such as nanosphere, nanometer
Stick, island nanostructure etc..
Nanostructure needed for preparing SERS substrate such as directly utilizes metal-sol or will be in metal-sol there are many method
Nano particle be fixed in substrate, [Oliver Seitza et al. .Preparation and characterisation of
gold nanoparticle assemblies on silanised glass plates.Colloids and Surfaces
A:Physicochem.Eng.Aspects 218 (2003) 225/239], but such method is complex for operation step, is difficult to control,
And nano particle is since indirect attachment is in substrate, and it is extremely easy to drop, and also particle is relatively difficult to realize be uniformly distributed, shadow
Ring SERS effect.
Summary of the invention
In view of SERS substrate significance of the preparation in Raman signal detection and metal Nano structure are in substrate
It is not easy the problem of adhering to, for the defects in the prior art, the purpose of the present invention is to provide one kind based on reduction method synthesis gold
The SERS substrate preparation method of nano particle.
In order to achieve the above object, the present invention uses following technical scheme：The method of the present invention is by carrying out silicon chip surface
Amination is realized in modification, then so that gold nano grain is relatively evenly adsorbed on base by the method for restoring chlorauric acid solution
On bottom, SERS substrate that is repeatable, having high enhancement factor is made.
The present invention directly generates the metal Nano structures such as gold and silver by reduction reaction directly in solid substrate.In order in base
The nano particle of gold is generated on bottom, is first allowed to surface amination with silane coupling A PTES modification silicon wafer, and weak using amino is gone back
Originality forms gold nano grain in chlorauric acid solution.This method preparation substrate due to gold nano grain sticking ratio it is stronger,
Therefore reliable and stable, repeatability is high, and preparation means are simple, and detection range is wide, there is very big application prospect.
Specifically, the present invention provides a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, it is described
Method includes the following steps：
Step 1：Silicon wafer is put into concentrated hydrochloric acid and cleans up, take out；
Step 2：The silicon wafer cleaned is surface modified using silane coupling agent, completes surface amination process；
Step 3：Amidized silicon wafer obtained by step 2 is put into chlorauric acid solution and is stirred to react, is generated in silicon chip surface
Gold nano grain；
Step 4：The Wafer Cleaning that step 3 reaction is completed is dry, spare.
Preferably, in the step 1, including：
Step 1.1：10~15ml concentrated hydrochloric acid is added in clean and dry round-bottomed flask, is stirred at a temperature of 80~100 DEG C
Uniform 2~3 hours, 80~100r/min of mixing speed；
Step 1.2：The clean tweezers of silicon wafer are taken out, is successively rinsed well with alcohol and deionized water and is done naturally
It is dry, it is spare.
Preferably, in the step 2, including：
Step 2.1：Clean silicon wafer is put into silane coupler solution, 24~72h is stirred at 80~90 DEG C；
Step 2.2：The clean tweezers of silicon wafer are taken out, it is first primary with alcohol washes, then cleaned 3 times with deionized water,
It is spare after natural drying.
It is highly preferred that the silane coupling agent uses 3- aminopropyl triethoxysilane (APTES) or 3- aminopropyl front three
Oxysilane (APS).
It is highly preferred that the volume ratio of silane coupling agent and toluene is 0.1~0.5 in the step 2.1, further,
Volume ratio is 0.1~0.3.
Preferably, in the step 3, including：
Step 3.1：Chlorauric acid solution is configured with ultrapure water, wherein gold chloride mass fraction is 0.01% in chlorauric acid solution
~0.1%；
Step 3.2：The silicon wafer that step 2 is obtained is put into the configured chlorauric acid solution of step 3.1, is stirred at 30~40 DEG C
Reaction 12~for 24 hours is mixed, mixing speed is controlled in 100r/min.
Preferably, in the step 4, the silicon wafer substrate prepared is cleaned 2~3 times with deionized water, is spontaneously dried
Vacuum saves afterwards, spare.
The present invention modifies silicon chip surface with silane coupling agent 3- aminopropyl triethoxysilane (APTES) and completes amination
Journey makes it have reproducibility, then forms gold nano grain by reduction method and is adsorbed on silicon chip surface, after natural drying just
To a kind of ideal SERS substrate.
Compared with prior art, the present invention has following beneficial effect：
(1) with the skill of the existing certain nanostructures of substrate surface indirect attachment by self-assembling method in chemical modification
Art is compared, and the maximum innovative point of the present invention is：Modification has the chemical group (amino) of reproducibility directly on silicon wafer, then
By reduction reaction, direct " growth " forms nanostructure on silicon wafer
(2) the technology of the present invention preparation method is simple, and strong operability is extensive using probe molecule；
(3) SERS substrate surface gold nano grain prepared by the present invention not only distribution uniform, and adhesiveness is very strong, no
It is easy to fall off；
(4) SERS substrate prepared by the present invention reaches the enhancement factor of the small molecules such as glycerol (usual Raman signal is very weak)
To 104The order of magnitude, SERS effect are fine.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the transmission electron microscope photo of SERS substrate surface gold particle in the embodiment of the present invention, wherein：It (a) is to implement
The transmission electron microscope photo of SERS substrate surface gold particle in example 1；It (b) is the saturating of SERS substrate surface gold particle in example 2
Penetrate electromicroscopic photograph；
Fig. 2 is that pure glycerin prepares the enhancing Raman spectrogram in substrate in embodiment 1,2,3 and 4.
Specific embodiment
Technical solution of the present invention is further described combined with specific embodiments below.Following embodiment will be helpful to this field
Technical staff further understand the present invention, but the invention is not limited in any way.It should be pointed out that the general of this field
For logical technical staff, without departing from the inventive concept of the premise, various modifications and improvements can be made.These are belonged to
Protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, the method packets
Include following steps：
A. 10ml concentrated hydrochloric acid is added in clean and dry round-bottomed flask, is put into the silicon wafer (1 × 1cm) that will be cut dense
In hydrochloric acid, stirred evenly at a temperature of 80 DEG C 2 hours, mixing speed 100r/min；Concentrated hydrochloric acid is the concentrated hydrochloric acid generally defined, i.e. matter
Amount score is more than 37% hydrochloric acid.
B. the clean tweezers of silicon wafer are taken out, is successively rinsed well and spontaneously dried with alcohol and deionized water, it is spare
(ultrasonic cleaning cannot be used)；
C. clean silicon wafer is put into the toluene solution of 3- aminopropyl triethoxysilane (APTES), is stirred at 90 DEG C
For 24 hours, wherein the volume ratio of APTES and toluene is 0.1；
D. the clean tweezers of silicon wafer are taken out, it is first primary with alcohol washes, then cleaned three times with deionized water, it is naturally dry
It is spare after dry；
E. chlorauric acid solution is configured with ultrapure water, the mass fraction of chlorauric acid solution is 0.01%；
F. the obtained silicon wafer of step d is put into the configured chlorauric acid solution of step e, is stirred to react 12h at 30 DEG C, stirs
Speed control is mixed in 100r/min；
G. the silicon wafer substrate prepared is cleaned into 3 times (unavailable ultrasonic cleaning), vacuum after natural drying with deionized water
It saves, it is spare.
Embodiment 2
The present embodiment provides a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, the method packets
Include following steps：
A. 15ml concentrated hydrochloric acid is added in clean and dry round-bottomed flask, is put into the silicon wafer (1 × 1cm) that will be cut dense
In hydrochloric acid, stirred evenly at a temperature of 90 DEG C 2 hours, mixing speed 100r/min；
B. the clean tweezers of silicon wafer are taken out, is successively rinsed well and spontaneously dried with alcohol and deionized water, it is spare；
C. clean silicon wafer is put into the toluene solution of 3- aminopropyl triethoxysilane (APTES), is stirred at 90 DEG C
48h, wherein the volume ratio of APTES and toluene is 0.5；
D. the clean tweezers of silicon wafer are taken out, it is first primary with alcohol washes, then cleaned three times with deionized water, it is naturally dry
It is spare after dry；
E. chlorauric acid solution is configured with ultrapure water, the mass fraction of chlorauric acid solution is 0.1%；
F. the obtained silicon wafer of step d is put into the configured chlorauric acid solution of step e, is stirred to react for 24 hours, stirs at 30 DEG C
Speed control is mixed in 100r/min；
G. the silicon wafer substrate prepared is cleaned 3 times with deionized water, vacuum saves after natural drying, spare.
Embodiment 3
The present embodiment provides a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, the method packets
Include following steps：
A. 13ml concentrated hydrochloric acid is added in clean and dry round-bottomed flask, is put into the silicon wafer (1 × 1cm) that will be cut dense
In hydrochloric acid, stirred evenly at a temperature of 85 DEG C 2 hours, mixing speed 100r/min；
B. the clean tweezers of silicon wafer are taken out, is successively rinsed well and spontaneously dried with alcohol and deionized water, it is spare；
C. clean silicon wafer is put into the toluene solution of 3- aminopropyl triethoxysilane (APTES), is stirred at 90 DEG C
72h, wherein the volume ratio of APTES and toluene is 0.3；
D. the clean tweezers of silicon wafer are taken out, it is first primary with alcohol washes, then cleaned three times with deionized water, it is naturally dry
It is spare after dry；
E. chlorauric acid solution is configured with ultrapure water, the mass fraction of chlorauric acid solution is 0.05%；
F. the silicon wafer that step d is obtained is put into configured chlorauric acid solution, and 20h, mixing speed are stirred to react at 30 DEG C
Control is in 100r/min；
G. the silicon wafer substrate prepared is cleaned 3 times with deionized water, vacuum saves after natural drying, spare.
Embodiment 4
The present embodiment provides a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, the method packets
Include following steps：
A. 12ml concentrated hydrochloric acid is added in clean and dry round-bottomed flask, is put into the silicon wafer (1 × 1cm) that will be cut dense
In hydrochloric acid, stirred evenly at a temperature of 85 DEG C 2 hours, mixing speed 100r/min；
B. the clean tweezers of silicon wafer are taken out, is successively rinsed well and spontaneously dried with alcohol and deionized water, it is spare；
C. clean silicon wafer is put into the toluene solution of 3- aminopropyl triethoxysilane (APTES), is stirred at 90 DEG C
72h, wherein the volume ratio of APTES and toluene is 0.4；
D. the clean tweezers of silicon wafer are taken out, it is first primary with alcohol washes, then cleaned three times with deionized water, it is naturally dry
It is spare after dry；
E. chlorauric acid solution is configured with ultrapure water, the mass fraction of chlorauric acid solution is 0.08%；
F. the silicon wafer that step d is obtained is put into configured chlorauric acid solution, and 16h, mixing speed are stirred to react at 30 DEG C
Control is in 100r/min；
G. the silicon wafer substrate prepared is cleaned 3 times with deionized water, vacuum saves after natural drying, spare.
It is the transmission electron microscope photo of SERS substrate surface gold particle in embodiment 1, as shown in figure 1 as shown in figure 1 shown in (a)
(b) it show the transmission electron microscope photo of SERS substrate surface gold particle in example 2, it is seen that the method through this embodiment
The SERS substrate surface gold nano grain of preparation not only distribution uniform, and adhesiveness is very strong, it is not easily to fall off.
As shown in Fig. 2, preparing the enhancing Raman spectrogram in substrate in embodiment 1,2,3 and 4 for pure glycerin, it is seen that
Enhancing of the SERS substrate of the method preparation to the small molecules such as pure glycerin (usual Raman signal is very weak) through this embodiment
The factor reaches 104The order of magnitude, SERS effect are fine.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (4)
1. a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain, which is characterized in that the method includes
Following steps：
Step 1：Silicon wafer is put into concentrated hydrochloric acid and cleans up, take out；
In the step 1, including：
Step 1.1：10~15ml concentrated hydrochloric acid is added in clean and dry container, is put into concentrated hydrochloric acid with the silicon wafer that will be cut
In, it is stirred evenly at a temperature of 80~100 DEG C 2~3 hours, 80~100r/min of mixing speed；
Step 1.2：By silicon chip extracting, is successively rinsed well and spontaneously dried with alcohol and deionized water, it is spare；
Step 2：The silicon wafer cleaned is surface modified using silane coupling agent, completes surface amination process；
In the step 2, including：
Step 2.1：Clean silicon wafer is put into the toluene solution of silane coupling agent, 24~72h is stirred at 80~90 DEG C；It is described
The volume ratio of silane coupling agent and toluene is 0.1~0.5；
Step 2.2：By silicon chip extracting, alcohol washes are first used, then cleaned with deionized water, it is spare after natural drying；
Step 3：Amidized silicon wafer obtained by step 2 is put into chlorauric acid solution and is stirred to react, generates Jenner in silicon chip surface
Rice grain；
In the step 3, including：
Step 3.1：With ultrapure water configure chlorauric acid solution, wherein in chlorauric acid solution gold chloride mass fraction be 0.01%~
0.1%；
Step 3.2：The silicon wafer that step 2 is obtained is put into the configured chlorauric acid solution of step 3.1, is stirred at 30~40 DEG C anti-
Answer 12~for 24 hours, mixing speed is controlled in 80~100r/min；
Step 4：The Wafer Cleaning that step 3 reaction is completed is dry, spare.
2. a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain according to claim 1, special
Sign is that the silane coupling agent uses 3- aminopropyl triethoxysilane (APTES) or 3- aminopropyl trimethoxysilane
(APS)。
3. a kind of SERS substrate preparation method based on reduction method synthesis gold nano grain according to claim 1, special
Sign is, the step 2.2：It by silicon chip extracting, first uses alcohol washes 1 time, then cleaned 3 times with deionized water, spontaneously dries
It is spare afterwards.
4. a kind of SERS substrate preparation side based on reduction method synthesis gold nano grain according to claim 1-3
Method, which is characterized in that in the step 4, the silicon wafer substrate prepared is cleaned 2~3 times with deionized water, it is true after natural drying
Sky saves, spare.
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| CN107460462B (en) * | 2017-08-17 | 2019-03-19 | 西安工业大学 | The preparation method of silver nano-grain compacted zone on silicon wafer |
| CN107976431B (en) * | 2017-11-23 | 2021-06-08 | 深圳大学 | Surface enhanced Raman substrate based on metal nanoparticles and preparation method thereof |
| CN108760713B (en) * | 2018-03-02 | 2020-11-17 | 西安工业大学 | Preparation method of uniform SERS substrate based on gold nanoparticles |
| CN108645835A (en) * | 2018-04-24 | 2018-10-12 | 扬州大学 | Gold nanoparticle SERS active-substrate of highly branchedization and preparation method thereof |
| CN109030450A (en) * | 2018-05-25 | 2018-12-18 | 苏州大学 | A method of in the two-way controllable self assembly difference charged metal nanoparticle of substrate surface |
| CN108971515B (en) * | 2018-10-24 | 2021-07-27 | 吉林大学 | Method for synthesizing hollow gold nanoflowers with SERS activity by one-pot method |
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