CN108982471A - AgNR/O-g-C3N4Substrate, preparation method and its application in recyclable SERS Sensitive Detection - Google Patents
AgNR/O-g-C3N4Substrate, preparation method and its application in recyclable SERS Sensitive Detection Download PDFInfo
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- CN108982471A CN108982471A CN201810874980.6A CN201810874980A CN108982471A CN 108982471 A CN108982471 A CN 108982471A CN 201810874980 A CN201810874980 A CN 201810874980A CN 108982471 A CN108982471 A CN 108982471A
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- 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
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- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
Abstract
AgNR/O‑g‑C3N4The preparation method of substrate, by carrying out O-g-C to the surface AgNR3N4More performance nanostructures for sensitive and recyclable SERS analysis are prepared in modification.The AgNR/O-g-C of above-mentioned preparation method preparation3N4Substrate and its application in recyclable SERS Sensitive Detection.AgNR/O-g-C of the invention3N4The preparation method preparation process of substrate is simple；AgNR/O-g-C of the invention3N4Substrate, O-g-C thereon3N4The adsorption capacity that molecule can be improved, improves the SERS performance of AgNRs, and is avoided that AgNR is directly contacted with atmosphere, improves the stability of AgNRs；AgNR/O-g-C of the invention3N4Substrate can produce significant Raman enhancement effect, from AgNR/O-g-C3N4The SERS signal intensity of acquisition is than about three times by force of unmodified AgNR, and it has excellent light degradation property, can be carried out multiple cycle detection with high reproducibility and stability.
Description
Technical field
The present invention relates to SERS substrates, and in particular to AgNR/O-g-C3N4Substrate, preparation method and its recyclable
Application in SERS Sensitive Detection.
Background technique
Due to population rapid development, agricultural and industrial activity increase, and a large amount of organic pollutant is discharged into aquatic environment
In.These pollutants can be entered in organism by biological chain, influence human health, or even have acute toxicity and carcinogenic
Property.Technology such as fluorescence spectrum common at present, chromatography, Capillary Electrophoresis and electrochemical analysis have been realized in these environment
The detection of organic pollutant, but the usual technical requirements of these methods are higher, and time-consuming and sensitivity is low.Therefore, the whole world is caused
Extensive concern.Currently, the whole world is making great efforts to develop a kind of next organic contamination effectively detected in water of quick and sensitive technology
Object.SERS substrate based on Ag is cheap and has higher SERS activity, so Ag is widely used in substrate system at present
It is standby.But Ag is once exposed in air, will be oxidized rapidly, so as to cause the reduction of SERS activity.And due to analyte
Saturation absorption, substrate typically exhibit weak reusability.
Summary of the invention
The purpose of the present invention is to provide a kind of stability of silver nanoparticle array in raising substrate and sensitivity and it is recycled
The SERS substrate used.
To achieve the above object, technical scheme is as follows:
AgNR/O-g-C3N4The preparation method of substrate, comprising steps of
S1: it is placed in deposition platform after glass slide is cleaned and dried；
S2: using glass slide as support substrate, in electron-beam evaporator, in 1 × 10-6In Torr vacuum, deposit respectively
Titanium film and silverskin system；
S3: with 86 ° of rotating and depositing platforms of angle of deposit, silverskin is deposited, AgNR array is obtained；
S4: melamine being placed in Muffle furnace and is calcined, cooled to room temperature, obtains blocky O-g-C3N4；
S5: by blocky g-C3N4It crushes, being put into potcal pot calcination postscript is M-O-g-C3N4, calcine M-O-g-C3N4Obtain single layer
O-g-C3N4；
S6: by single layer O-g-C3N4It is dispersed in organic solution by ultrasonic treatment, the O-g-C after taking ultrasonic treatment3N4Liquid
Drop drop toasts AgNR substrate in AgNR substrate, and washing obtains AgNR/O-g-C3N4Substrate.
Further, step S2 is specifically included: using glass slide as support substrate, in electron-beam evaporator, in 1 ×
10-6Under the pressure of Torr, with the titanium film of 0.2nm/s rate deposition 20nm, with the silverskin system of the rate deposition 500nm of 0.3nm/s
System.
Further, step S3 is specifically included: with 86 ° of rotating and depositing platforms of angle of deposit, being deposited with the rate of 0.3nm/s
2000nm silverskin.
Further, step S4 is specifically included: 2g melamine being placed in Muffle furnace, is heated up with the rate of 2 DEG C/min
To 550 DEG C, calcines 4 hours, by calcined melamine cooled to room temperature, obtain blocky g-C3N4。
Further, step S5 is specifically included: by 500mg bulk g-C3N4It after crushing, is put into crucible, with 5 DEG C/min
Rate be warming up to 550 DEG C, after calcining 1 hour yellow sample, be denoted as M-O-g-C3N4, by M-O-g-C3N4With 2 DEG C/min
550 DEG C are heated to, 2h is calcined, obtains white pigmented samples, be expressed as single layer O-g-C3N4。
Further, step S6 is specifically included: by 1mg single layer O-g-C3N4By 2 minutes ultrasonic disperses in 5mL isopropyl
80 μ L O-g-C in alcoholic solution, after taking ultrasonic treatment3N4Drop drips in AgNR substrate, then by AgNR substrate at 50 DEG C
It is toasted 10 seconds on electric boiling plate, AgNR substrate is washed with deionized later and obtains AgNR/O-g-C more than three times3N4Substrate.
Aforementioned AgNR/O-g-C3N4AgNR/O-g-C prepared by the preparation method of substrate3N4Substrate.
Aforementioned AgNR/O-g-C3N4Substrate is in the application in recyclable SERS Sensitive Detection.
Compared with prior art, beneficial effects of the present invention: AgNR/O-g-C of the invention3N4The preparation method of substrate is logical
It crosses and O-g-C is carried out to the surface AgNR3N4More performance nanostructures for sensitive and recyclable SERS analysis are prepared in modification,
And preparation method is simple；AgNR/O-g-C of the invention3N4Substrate, O-g-C thereon3N4The adsorption capacity of molecule can be improved,
The SERS performance of AgNRs is improved, and is avoided that AgNR is directly contacted with atmosphere, improves the stability of AgNRs；Of the invention
AgNR/O-g-C3N4Substrate can produce significant Raman enhancement effect, from AgNR/O-g-C3N4The SERS signal intensity ratio of acquisition
About three times by force of unmodified AgNR, and it has excellent light degradation property, can be carried out more with high reproducibility and stability
Secondary cycle detection.
Detailed description of the invention
Fig. 1 is AgNR/O-g-C in the embodiment of the present invention 13N4The preparation flow figure of substrate；
Fig. 2 is the SEM figure of the AgNR substrate in the embodiment of the present invention 1, wherein A is prepared by oblique angle deposition technique
The vertical view SEM image of AgNR substrate, B AgNRs/O-g-C3N4The vertical view SEM image of substrate；
Fig. 3 is AgNR/O-g-C in the embodiment of the present invention 23N4The SERS spectra of the R6G of various concentration in substrate, wherein
It is to be adsorbed on AgNR/O-g-C in A3N4The SERS spectra of the R6G of various concentration in substrate: a) 1.0 × 10-9M, b) 1.0
×10-8M, c) 1.0 × 10-7M, d) 1.0 × 10-6M, and e) 1.0 × 10-5M, B be under a series of R6G concentration of logarithmic form,
In 1362cm-1Locate SERS Strength Changes；
Fig. 4 is AgNR/O-g-C under the holding times different in the embodiment of the present invention 23N4In substrate the SERS spectra of R6G and
1362cm-1The corresponding SERS intensity at place, wherein A is under the different holding times: 7 days, 14 days, 21 days, AgNR/O-g-C3N4Base
The SERS spectra of R6G on bottom, B 1362cm-1The corresponding SERS intensity at place；
AgNR/O-g-C is adsorbed in Fig. 5 embodiment of the present invention 23N4R6G (5.0 × 10 on nanocomposite-6M) light
The SERS spectra of catalytic degradation process；
Fig. 6 is AgNR/O-g-C in the embodiment of the present invention 23N4Substrate photocatalytic degradation R6G (5.0 × 10-6M) recyclable
The performance test results.
Specific embodiment:
The present invention is described further with reference to the accompanying drawings.
1 AgNR/O-g-C of embodiment3N4The preparation of substrate
1. preparing AgNR array
By glass slide, the cleaning in Piranha solution (80% sulfuric acid, 20% hydrogen peroxide), is rinsed with deionized water, and
It is dry in nitrogen atmosphere.Then, the glass slide cleaned is placed in deposition platform.In electron-beam evaporator (DE500 electricity
Beamlet evaporation deposition method) in, 1 × 10-6Under the pressure of Torr, 20nm is deposited with the rate of 0.2nm/s and 0.3nm/s respectively
Titanium film and 500nm silverskin system.Then with 86 ° of spin deposition station of angle of deposit, 2000nm is deposited with the rate of 0.3nm/s
Silverskin obtains AgNR array.
2. preparing single layer O-g-C3N4
Firstly, melamine (2g) is placed in Muffle furnace, and 550 DEG C are raised the temperature to the rate of 2 DEG C/min, forged
It burns 4 hours.Then, by melamine cooled to room temperature, glassy yellow sample is obtained, is denoted as blocky g-C3N4.Then, will
500mg bulk g-C3N4Crush, be reentered into crucible, and with the rate of 5 DEG C/min be warming up to 550 DEG C further calcining it is 1 small
When.Prepared sample be it is faint yellow, be denoted as M-O-g-C3N4.Then, by M-O-g-C3N4550 DEG C are heated to 2 DEG C/min
And 2h is calcined, white pigmented samples are finally obtained, single layer O-g-C is expressed as3N4。
3. preparing AgNR/O-g-C3N4Substrate
Fig. 1 show AgNR/O-g-C3N4The preparation process of substrate, firstly, by single layer O-g-C3N4(1mg) passes through 2 points
The ultrasound of clock is thoroughly dispersed in aqueous isopropanol (5mL), 80 μ L O-g-C after taking ultrasonic treatment3N4Drop is dripped in AgNR base
On bottom.Then, substrate is toasted to 10 seconds on 50 DEG C of electric boiling plate with evaporating completely solvent.Finally, being washed with deionized
Substrate is at least three times to remove unmodified O-g-C3N4.In Fig. 2, A show the AgNR substrate prepared by oblique angle deposition technique
Vertical view SEM image；B show AgNRs/O-g-C3N4The vertical view SEM image of substrate；From figure 2 it can be seen that transparent monolayer
O-g-C3N4Successfully AgNR is arrived in modification.
2 AgNR/O-g-C of embodiment3N4The performance measurement of substrate
1.AgNR/O-g-C3N4The SERS sensitivity determination of substrate
The standard solution for preparing various various concentrations, with water by 10-3It is 1.0 × 10 that the R6G solution of M, which is diluted to concentration,-5M
To 1.0 × 10-9The solution of M.For each sample, three SERS spectras are obtained from the different location of substrate.Laser power is 10
MW, time of integration 5s, as a result as shown in Figure 3.As can be seen from Figure 3 R6G detection is limited down to 8.2 × 10-10M shows
AgNR/O-g-C3N4Substrate has very high detection sensitivity.
2.AgNR/O-g-C3N4The Stability Determination of substrate
Identical substrate is placed in air, every the 5 × 10 of 7 days detection R6G-5The signal of M, testing result such as Fig. 4
It is shown, figure 4, it is seen that the SERS signal of R6G after 21 days almost without too big change, show AgNR/O-g-
C3N4Substrate has good stability.
3.AgNR/O-g-C3N4The self-cleaning performance of substrate measures
R6G (5 × 10 will be contained-6M, 80 μ L) AgNRs/C3N4When about 30 μ L ultrapure waters being added in substrate, while increasing
Between (from 15 minutes to 90 minute).Lamp is fixed on AgNRs/O-g-C3N4At the about 2cm of the top of substrate, to ensure that they are equal
Even irradiation.Purpose is the variation in order to track R6G amount in substrate, records the SERS signal of different interval, measurement result such as Fig. 5 institute
Show.From figure 5 it can be seen that substrate, after the illumination by 60min, the signal of R6G has completely disappeared, show AgNR/O-
g-C3N4Substrate has good self-cleaning performance.
4.AgNR/O-g-C3N4Performance measurement is recycled in substrate
In SERS measuring study AgNRs/C3N4After substrate, substrate is irradiated after sixty minutes under visible light, then use deionization
It is rinsed in water at least three times to remove remaining ion, then, substrate is dried in vacuo at room temperature, be recycled for subsequent
SERS detection.With under identical experiment condition for the first time, substrate is for detecting R6G.Each circulating repetition 4 times, as a result such as Fig. 6
It is shown.From fig. 6 it can be seen that AgNR/O-g-C3N4Substrate is by 4 detections and automatically cleaning process, the SERS signal of R6G
Almost without changing, show AgNR/O-g-C3N4Substrate has is recycled performance well.
Claims (8)
1.AgNR/O-g-C3N4The preparation method of substrate, which is characterized in that comprising steps of
S1: it is placed in deposition platform after glass slide is cleaned and dried；
S2: using glass slide as support substrate, in electron-beam evaporator, in 1 × 10-6In Torr vacuum, titanium film is deposited respectively
With silverskin system；
S3: with 86 ° of rotating and depositing platforms of angle of deposit, silverskin is deposited, AgNR array is obtained；
S4: melamine being placed in Muffle furnace and is calcined, cooled to room temperature, obtains blocky g-C3N4；
S5: by blocky g-C3N4It crushes, being put into potcal pot calcination postscript is M-O-g-C3N4, calcine M-O-g-C3N4Obtain single layer O-g-
C3N4；
S6: by single layer O-g-C3N4It is dispersed in organic solution by ultrasonic treatment, the O-g-C after taking ultrasonic treatment3N4Drop drop
In AgNR substrate, AgNR substrate is toasted, washing obtains AgNR/O-g-C3N4Substrate.
2. AgNR/O-g-C according to claim 13N4The preparation method of substrate, which is characterized in that the step S2 is specific
It include: using glass slide as support substrate, in electron-beam evaporator, in 1 × 10-6Under the pressure of Torr, with 0.2nm/s rate
The titanium film of 20nm is deposited, with the silverskin system of the rate deposition 500nm of 0.3nm/s.
3. AgNR/O-g-C according to claim 13N4The preparation method of substrate, which is characterized in that the step S3 is specific
It include: that 2000nm silverskin is deposited with the rate of 0.3nm/s with 86 ° of rotating and depositing platforms of angle of deposit.
4. AgNR/O-g-C according to claim 13N4The preparation method of substrate, which is characterized in that the step S4 is specific
Include: that 2g melamine is placed in Muffle furnace, is warming up to 550 DEG C with the rate of 2 DEG C/min, calcines 4 hours, it will be calcined
Melamine cooled to room temperature obtains blocky g-C3N4。
5. AgNR/O-g-C according to claim 13N4The preparation method of substrate, which is characterized in that the step S5 is specific
It include: by 500mg bulk g-C3N4It after crushing, is put into crucible, after being warming up to 550 DEG C, calcining 1 hour with the rate of 5 DEG C/min
Yellow sample is obtained, M-O-g-C is denoted as3N4, by M-O-g-C3N4550 DEG C are heated to 2 DEG C/min, 2h is calcined, obtains white pigmented samples,
It is expressed as single layer O-g-C3N4。
6. AgNR/O-g-C according to claim 13N4The preparation method of substrate, which is characterized in that the step S6 is specific
It include: by 1mg single layer O-g-C3N4The 80 μ L through 2 minutes ultrasonic disperses in 5mL aqueous isopropanol, after taking ultrasonic treatment
O-g-C3N4Drop drip in AgNR substrate, then AgNR substrate is toasted 10 seconds on 50 DEG C of electric boiling plate, spend later from
Sub- water washing AgNR substrate obtains AgNR/O-g-C more than three times3N4Substrate.
7. the AgNR/O-g-C as described in any of the above claim3N4AgNR/O-g-C prepared by the preparation method of substrate3N4
Substrate.
8. AgNR/O-g-C described in claim 73N4Substrate is in the application in recyclable SERS Sensitive Detection.
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