CN111360280B - Raman enhancement material and rapid preparation method thereof - Google Patents
Raman enhancement material and rapid preparation method thereof Download PDFInfo
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- CN111360280B CN111360280B CN202010275760.9A CN202010275760A CN111360280B CN 111360280 B CN111360280 B CN 111360280B CN 202010275760 A CN202010275760 A CN 202010275760A CN 111360280 B CN111360280 B CN 111360280B
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The invention relates to a surface-enhanced scattering substrate material, in particular to a Raman-enhanced material and a rapid preparation method thereof. The method takes nano silicon carbide as a framework, and nano silver particles are reduced and grown on the surface and sharp edges of the nano silicon carbide. Mixing nano SiC with the nano silver precursor solution, adding a reducing agent into the mixed solution, and heating in a water bath; and after heating, quickly cooling the mixed solution, and centrifuging to obtain the product. The Raman enhancing material has low cost and quick preparation, has stronger SERS enhancing effect on exciting light with the wavelength of 785nm, and also has the SERS enhancing effect on exciting light with the wavelength of 532 nm.
Description
Technical Field
The invention relates to a surface-enhanced scattering substrate material, in particular to a low-cost Raman enhancement material which takes nano silicon carbide as a framework and has better response to 785nm exciting light and a rapid preparation method thereof.
Background
Raman spectroscopy, a type of molecular vibrational spectroscopy, was discovered by indian physicist c.v. raman in 1928. Raman spectroscopy is a structural feature of molecules and its principle is to collect reflected light after irradiating an object. But the reflected light intensity is only 10 of the incident light -6 ～10 -10 . Due to the restriction of the current weak signal acquisition and analysis level, the application and development of the Raman spectrum are greatly limited. Until 1974, Fleischmann et al roughened the smooth silver electrode surface and obtained a monomolecular layer of pyridine molecular raman signals, which was of significantly higher signal quality than before. This correlation on rough surfacesIs referred to as surface enhanced raman Scattering Effect (SERS).
Silver is a metal widely used in the preparation of Raman reinforced materials (Kerker, M; Siiman, O; Bumm, L A; Wang, D. Surface Enhanced Raman Scattering (SERS) of adsorbed on colloidal silver [ J ]. Applied optics,1980(19): 3253-5; lishow, jiahui hui glu, xu weiqing, zhang, zhao ice. Common morphologies of silver in SERS applications are: silver sol (LEOPOLD N, LENDL B.A New Method for Fast Preparation of high hly Surface-Enhanced Raman Scattering (SERS) Active Silver Colloids at Room Temperature by Reduction of Silver Nitrate with hydro xylamine Hydrochloride [ J ]. J Phys Chem B,2003,107(24): 5723-7; Silent Silver nanoparticle morphology control synthesis and SERS activity research [ D ]. Jilin university, 200.), Silver nanowires and nanorods (Liuteng, Lileijun, Cheng, von, Huangwen Yixing. Noxin on SERS wire substrate SERS spectrum detection [ J ]. light Scattering bulletin, 2017,29(04): 303), Silver nanoparticle structure (LEOPOLD N, LENDL B.A) nano Silver particle size Preparation controllable Silver nanoparticle size research [ SEN ] mechanical sample Surface spectrum enhancement university ] nano Silver nanoparticle size and nano particle Surface field application technology (SERS field Biochemical research [ D ]. Biochemical engineering university ] and Silver nanoparticle Surface field chemical engineering university [ D ] nano field chemical engineering university ] nano Silver nanoparticle size enhancement technology Institute), 2018).
The aggregation state of the silver sol has a very obvious influence on the SERS effect, and a 'hot point' is generated when the colloidal silver is aggregated, namely a very strong electromagnetic field exists, so that the very strong SERS effect is generated, but if the aggregation effect is required to be generated, the input amount of the nano silver precursor is increased, namely the cost is greatly increased. The preparation methods of the nano silver wire, the nano rod, the nano silver cubic structure and the flower type silver nano structure array comprise an electrodeposition method, a metal cation reduction method, a self-assembly mode, a photoetching method and an electron beam etching method, and the preparation methods have the problems that the sample preparation process is relatively complex, the self-assembly process is random, the consistency is poor, the preparation precision only reaches micron level, or large-scale equipment is needed, the time consumption is long, the cost is high, large-area preparation is difficult, the preparation is unstable under illumination, the aggregation and the precipitation are easy to occur, and the cost is high.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a nano silver particle modified SiC Raman reinforcing material and a rapid preparation method thereof.
In order to realize the purpose, the invention adopts the following technical scheme:
the invention provides a Raman reinforcing material, which takes nano silicon carbide as a framework and reduces and grows nano silver particles at sharp edges and corners on the surface of the nano silicon carbide.
The invention also provides a preparation method of the Raman enhancing material, which comprises the following steps:
(1) mixing the nano SiC and the nano silver precursor solution, adding a reducing agent into the mixed solution, and heating in a water bath.
(2) And (3) after the step (1) is finished, quickly cooling the mixed solution, and centrifuging to obtain the product.
In the above technical solution, further, the nano-silver precursor is silver nitrate, silver fluoride, silver perchlorate, or RCOOAg long-chain organic silver salt, or a complexed silver ammonia solution; the nano silver precursor is preferably silver nitrate.
In the above technical solution, further, the reducing agent is sodium citrate, ascorbic acid, urea and sodium borohydride; the reducing agent is preferably sodium citrate.
In the above technical solution, further, the method for mixing the nano SiC and the nano silver precursor solution in step (1) is ultrasonic or oscillation.
In the technical scheme, furthermore, the ultrasonic treatment is carried out for 8-12 min under the ultrasonic condition of 5-6 KHz; the oscillation is carried out for 150-200 min under 200-400 r/min.
In the technical scheme, the mass ratio of the nano SiC, the nano silver precursor and the reducing agent is 20-80: 3: 3.
in the technical scheme, further, the water bath temperature is 60-100 ℃, and the water bath time is 10-60 min.
In the technical scheme, furthermore, the centrifugal separation rotating speed is 2000-5000 r/min, and the centrifugal time is 10-30 min.
The invention has the beneficial effects that:
(1) the preparation cost of the Raman reinforcing material is low; the invention provides a framework for the growth of the nano-silver particles by using the nano-silicon carbide, the nano-silver particles are better dispersed due to the framework effect of the silicon carbide, the proportion of the nano-silver particles is greatly reduced, the consumption of nano-silver precursors for preparing the Raman enhancing material is reduced, and the preparation cost is reduced.
(2) The wavelength of the excitation light for the traditional nano silver particles to generate the SERS effect is usually in the range of 380nm to 620 nm. According to the characteristic that the Raman enhancement effect is sensitive to the shape, the nano silicon carbide with an irregular shape is used as the template, so that the excitation wavelength of the SERS effect generated by the nano silver is subjected to red shift, the Raman enhancement effect on 785nm excitation light is strong, and the Raman enhancement effect on 532nm excitation light is also good.
(3) The invention utilizes the irregular shape of the nanometer silicon carbide and the template action of the sharp edges to prepare the nanometer silver, the reduced zero-valent silver preferentially grows into the nanometer silver at the sharp edges and the surface energy, and the growth of the nanometer silver can be controlled easily by regulating the proportion of the silicon carbide, the silver precursor and the reducing agent.
Drawings
FIG. 1 is a flow chart of the operation of the preparation method of the present invention;
FIG. 2 is a graph of a particle size distribution of nano SiC;
FIG. 3 is a Scanning Electron Microscope (SEM) topography of nano SiC;
FIG. 4 shows the molecular structure of rhodamine 6G (R6G);
FIG. 5 is a scanning electron microscope and C, Si and Ag energy spectrum analysis mapping chart of the Raman reinforcing material of example 1;
FIG. 6 total spectrum of Raman enhanced material spectrum analysis of example 1;
FIG. 7 excitation light at 532nm R6G (10) of example 1 -4 mol/L) enhanced Raman spectra;
FIG. 8 excitation light at 785nm of example 1R 6G (10) -4 moL/L) enhanced Raman spectrum and R6G (10) -2 mol/L、10 -3 mol/L、10 -4 mol/L) Raman spectrum.
FIG. 9 excitation light at 785nm of example 2R 6G (10) -2 mol/L) of the sample.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
The operational flow diagram of the method of the present invention is shown in fig. 1. The SiC starting material used in all of the following examples was a mixture of nano-SiC and micro-SiC, available from zeita micro powder ltd, qingzhou. Dimethyl sulfoxide (analytically pure), sodium oleate (chemically pure), octadecyl trimethyl ammonium chloride (analytically pure), ethanol (analytically pure), silver nitrate (analytically pure), sodium citrate (analytically pure), and rhodamine 6G (analytically pure) were purchased from national medicine group chemical reagent, Inc. The particle size distribution was measured using a malvern particle size analyzer. The morphology of the SiC was determined using a QUNATA200FEG scanning electron microscope. And (3) carrying out high-temperature treatment by using a combined fertilizer family crystal KSL-1700X type box muffle furnace to prepare the nano silver particle modified silicon carbide surface enhanced Raman material. The Raman spectrum of rhodamine 6G is measured by adopting a HORIBA JY XploRA microscopic confocal Raman spectrometer, and the enhancement performance of the surface enhanced Raman material in the invention is verified, and the excitation wavelength is 532nm and 785 nm.
Example 1
(I) silicon carbide production
1. Mixing 500mL of dimethyl sulfoxide (DMSO) saturated solution of sodium oleate with 100g of SiC raw material powder (the ratio of the two is 5 mL: 1g), and performing ultrasonic treatment (5.5KHz) for 10min and shaking table oscillation (300r/min) for 180min to uniformly disperse the SiC powder in the solution; then, the mixture was left standing for 8 hours.
2. Transferring 70-80% of upper layer liquid in the mixed liquid after standing, performing centrifugation (4000 r/min; 30min) or filtration-backwashing separation, and drying the separated solid phase to obtain nano SiC, wherein the figure 2 is a nano silicon carbide particle size distribution diagram; FIG. 3 is a Scanning Electron Microscope (SEM) morphology of nano-SiC.
(II) preparation of Raman reinforced material
1. Ultrasonically mixing the nano SiC with a silver nitrate solution at 5.5KHz for 8 min; adding sodium citrate into the mixed solution, and heating in 80 deg.C water bath for 40 min. The mass ratio of the nano SiC to the silver nitrate to the sodium citrate is 24.93: 3: 3.
2. after the water bath was complete, the mixture was quickly cooled to room temperature. And then carrying out centrifugal treatment (4000r/min) to obtain the Raman enhancement material taking the nano silicon carbide as the framework.
FIG. 5 shows the results of mapping analysis of C, Si, Ag in the Raman-enhanced material using a scanning electron microscope equipped with a spectrum detector; as shown in fig. 5, the nano silver is uniformly distributed in the raman enhancing material. Fig. 6 is a total spectrum of the raman enhancing material by energy spectrum analysis.
(III) SERS performance verification
1. In the process of researching the SERS activity of the substrate, rhodamine 6G (R6G for short) is a common signal molecule, the molecular structure of the signal molecule is shown in figure 4, and the method takes R6G as a target molecule to analyze the SERS activity of the Raman enhancement material. The vibration frequency shift value of rhodamine 6G molecule is shown in Table 1:
TABLE 1
2. For R6G (10) -4 mol/L) solution is subjected to Raman spectrum collection, and the test parameters are 532nm exciting light, 50 times of objective lens, Auto mode, exposure time (1sec), superposition times (29), aperture (100 mu m), slit (200 mu m) and wave number range (500-1800 cm) -1 ) (ii) a For R6G (10) -2 mol/L、10 -3 mol/L、10 -4 mol/L) solution, with the test parameters of 785nm exciting light, 50 times of objective lens, Auto mode, exposure time (1sec), superposition times (34), aperture (500 μm), slit (200 μm) and wave number range (500-1800 cm) -1 )。
3. The raman-enhancing material of example 1 was added to R6G (10) -4 mol/L) solution, carrying out enhanced Raman spectrum collection, and testing parameters of 532nm exciting light, 50 times of objective lens, Auto mode, exposure time (1sec), superposition times (29), aperture (100 mu m) and slit (200)Mum) and wave number range (500-1800 cm) -1 ) (ii) a For R6G (10) -4 mol/L) solution, with the test parameters of 785nm exciting light, 50 times of objective lens, Auto mode, exposure time (1sec), superposition times (34), aperture (500 μm), slit (200 μm) and wave number range (500-1800 cm) -1 )。
(IV) discussion of results
The Raman characteristic peaks of the nano silicon carbide and the nano silver are not overlapped with the characteristic peak of the R6G molecule, so that the SERS enhancement effect is not influenced.
Under 532nm excitation light, the concentration is 10 -4 In mol/L R6G solution, Raman characteristic peaks of any R6G molecule cannot be detected (data are not shown in a meaningless way); as shown in FIG. 7, after the Raman enhancing material of example 1 was added, sharp Raman characteristic peaks (617, 643, 668, 778, 1134, 1190, 1317, 1367, 1429, 1513, 1575, 1651 cm) of R6G molecules were detected -1 ) The results show that the prepared material has obvious Raman enhancement effect.
As shown in FIG. 8, under 785nm excitation light, the concentration of the light was 10 -2 mol/L、10 -3 mol/L、10 -4 When the detection is carried out by using a mol/L R6G solution, the Raman signal of R6G is extremely weak; only 10 -2 Very weak signals can be detected by mol/L R6G solution; at 10 -3 mol/L and 10 -4 In mol/L of the R6G solution, no characteristic signal can be detected.
At 10 -4 After the Raman enhancing material of the embodiment 1 is added into mol/L R6G solution, sharp Raman characteristic peaks (565, 609, 631, 659, 768, 1086, 1127, 1184, 1310, 1360, 1507, 1595, 1640 and 1648 cm) of R6G can be detected -1 ) The material has the enhancement effect, and the Enhancement Factor (EF) is calculated to be 10 4 。
The enhancement factor is the key for researching the SERS effect, the size of the enhancement factor is one of important standards for evaluating the enhancement effect of the SERS active substrate, and the performance of the SERS active substrate is better when the enhancement factor is larger. The magnitude of the enhancement coefficient is expressed as:
in the formula I SERS SERS enhances the peak intensity on the spectrum;
I Raman -peak intensity on conventional raman spectra;
N SERS number of molecules in SERS enhanced Spectroscopy test
N Raman Number of molecules in conventional Raman Spectroscopy
C SERS -the concentration of the sample to be measured in the SERS enhanced spectroscopy test;
C Raman -the concentration of the sample to be tested in a conventional raman spectroscopy test.
Example 2
(one) silicon carbide production
1. Mixing 500mL of dimethyl sulfoxide saturated solution of sodium oleate with 100g of SiC raw material powder (the proportion of the two is 5 mL: 1g), and carrying out ultrasonic treatment (5.5KHz) for 10min and shaking table oscillation (300r/min) for 180min to uniformly disperse the SiC powder in the solution; then, the mixture was left standing for 8 hours.
2. And transferring 70-80% of upper layer liquid in the mixed liquid after standing, performing centrifugation (4000 r/min; 30min) or filtration-backwashing separation, and drying the separated solid phase to obtain the nano SiC. FIG. 2 is a distribution diagram of the nano-silicon carbide particle size; FIG. 3 is a Scanning Electron Microscope (SEM) morphology of nano-SiC.
(II) preparation of Raman reinforced material
1. Ultrasonically mixing the nano SiC with silver nitrate solution at 5.5KHz for 8 min; adding sodium citrate into the mixed solution, and heating in 80 deg.C water bath for 40 min. The mass ratio of the nano SiC to the silver nitrate to the sodium citrate is 74.79: 3: 3.
2. after the water bath was complete, the mixture was quickly cooled to room temperature. And then, carrying out centrifugal treatment (4000r/min) to obtain the Raman enhancement material taking the nano silicon carbide as a framework.
(III) SERS performance verification
1. For R6G (10) -2 mol/L) solution is subjected to Raman spectrum collection, and the test parameters are 785nm exciting light, 50 times of objective lens, Auto mode, exposure time (1sec), superposition times (34),Pore size (500 μm), slit (200 μm) and wave number range (500-1800 cm) -1 )。
2. The raman-enhanced material of example 2 was added to R6G (10) -2 mol/L) solution is subjected to enhanced Raman spectrum collection, and the test parameters are 785nm exciting light, 50-time objective lens, Auto mode, exposure time (1sec), superposition times (34), aperture (500 mu m), slit (200 mu m) and wave number range (500-1800 cm) -1 )。
(IV) discussion of results
785nm excitation light, 10 -2 The Raman signal of the mol/L R6G solution is very weak. As shown in FIG. 9, when the Raman enhancing material of example 2 was added and then measured with 785nm excitation light, sharp Raman characteristic peaks (568, 611, 634, 656, 769, 1085, 1128, 1184, 1309, 1361, 1508, 1597 and 1647 cm) were observed -1 ) Indicating that the raman signal is significantly enhanced.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (6)
1. A preparation method of a Raman enhancing material is characterized by comprising the following steps:
(1) mixing the nano SiC with the nano silver precursor solution, adding a reducing agent into the mixed solution, and heating in a water bath;
(2) after the step (1) is finished, quickly cooling the mixed solution, and centrifuging to obtain the product;
the mass ratio of the nano SiC, the nano silver precursor and the reducing agent is 20-80: 3: 3;
the preparation method of the nano SiC in the step (1) comprises the following steps:
1) mixing a dimethyl sulfoxide saturated solution of sodium oleate with SiC raw material powder, wherein the ratio of the dimethyl sulfoxide saturated solution of sodium oleate to SiC is 5 mL: 1g, carrying out 10min 5.5KHz ultrasonic treatment and 180min 300r/min table shaking to uniformly disperse the SiC powder in the solution, and then standing for 8 h;
2) and transferring 70-80% of upper layer liquid in the mixed solution after standing, performing centrifugation at 4000r/min for 30min or filtering-backwashing separation, and drying the separated solid phase to obtain the nano SiC.
2. A method for preparing a raman enhancing material according to claim 1, wherein the nano silver precursor is silver nitrate, silver fluoride, silver perchlorate, or RCOOAg long-chain organic silver salt, or a complexed silver ammonia solution.
3. A method for preparing a raman enhancing material according to claim 1, wherein said reducing agent is sodium citrate, ascorbic acid, urea and sodium borohydride.
4. The method for preparing a Raman-enhanced material according to claim 1, wherein the water bath temperature is 60 ℃ to 100 ℃, and the water bath time is 10min to 60 min.
5. The method for preparing a Raman enhancing material according to claim 1, wherein the centrifugal separation rotation speed is 2000-5000 r/min, and the centrifugal time is 10-30 min.
6. The Raman reinforcing material prepared by the preparation method of any one of claims 1-5, wherein the Raman reinforcing material takes nano silicon carbide as a framework, and nano silver particles are reduced and grown at sharp corners on the surface of the nano silicon carbide.
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