CN103837521A - Preparation method for sodium chloride assisted silver nano-particle self-assembled filter paper surface enhanced Raman spectrum base - Google Patents
Preparation method for sodium chloride assisted silver nano-particle self-assembled filter paper surface enhanced Raman spectrum base Download PDFInfo
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- CN103837521A CN103837521A CN201410116519.6A CN201410116519A CN103837521A CN 103837521 A CN103837521 A CN 103837521A CN 201410116519 A CN201410116519 A CN 201410116519A CN 103837521 A CN103837521 A CN 103837521A
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Abstract
The invention provides a preparation method for a sodium chloride assisted silver nano-particle self-assembled filter paper surface enhanced Raman spectrum (SERS) base, and aims to solve the problems that the sensitivity of the silver nano-particle SERS base prepared by adopting an existing method is low and the manufacturing process is complicated. The preparation method comprises the following steps: 1, dissolving silver nitrate into ultrapure water and boiling; adding a sodium citrate solution to prepare silver sol; 2, immersing a filtering paper sheet in a sodium chloride solution; and airing the taken sheet; and 3, immersing the filtering paper sheet in the silver sol; and airing the taken sheet to finish the preparation of the surface enhanced Raman spectrum base. The surface enhanced Raman spectrum base provided by the invention can be used for rapidly detecting substances with the concentration in a ppb magnitude order and is high in sensitivity; the Raman spectrum base is simple and convenient to operate and low in cost; the prepared base can be applied to the detection field of inorganic molecules and biological molecules.
Description
Technical field
The present invention relates to a kind of preparation method of Surface enhanced raman spectroscopy substrate.
Background technology
Surface enhanced raman spectroscopy (SERS) is the analysis and characterization technology of setting up on the basis of Raman scattering.Due to its have that bands of a spectrum are narrow, resolution is high, can cancellation fluorescence, water disturbs the advantages such as little, sensitivity is high, is widely used in surface catalysis, chemical analysis, food inspection, material science and the field such as biomedical.But, can Surface enhanced raman spectroscopy technology develop into the analytical technology that a kind of tool has significant practical applications, depend on to a great extent reappearance and the stability of Surface enhanced raman spectroscopy technology, wherein crucial part is exactly to prepare that highly sensitive, favorable reproducibility, stability are high, the surface-enhanced Raman spectrum active substrate of easy preparation.
Due to requirements at the higher level to work place study, fast detecting in recent years, the SERS substrate being assembled on filter paper has presented increasing advantage.Self assembly filter paper SERS substrate preparation process is simple, expense is low, even structure, be suitable for promote, be conducive to improve detect reappearance and sensitivity.Can be applied to the actual detection of chemistry and biomolecule.At present existing much work utilizes immersion coating technology that gold nanorods, bicone, nano particle are assembled in uniformly and on filter paper, prepare SERS substrate, but the Surface enhanced raman spectroscopy substrate sensitivity that above immersion coating technology prepares is lower, complex manufacturing technology.
Summary of the invention
The object of the invention is in order to solve silver nano-grain SERS substrate sensitivity prepared by existing method low, the problem of complex manufacturing technology, and the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate is provided.
The preparation method of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy of the present invention substrate follows these steps to realize:
One, the silver nitrate of 45～65mg be dissolved in the ultrapure water of 250ml and boil, then adding 5～10ml mass concentration is 1% sodium citrate solution, boils to naturally cool to room temperature after 1～1.5h and obtain silver sol;
Two, filter paper is cut into filter paper, the sodium chloride solution of then putting into concentration and be 0.1～0.5mol/L soaks, and takes out after filter paper and dries and obtain dry filter paper;
Three, after the silver sol of dry filter paper being put into step 1 soaks 12h～72h, take out, at room temperature dry and obtain the substrate of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy.
Surface enhanced raman spectroscopy substrate of the present invention can be used for the fast detecting of ppb magnitude concentration material, and evenly, highly sensitive, method of operating is easy in basal signal response, and cost is low.Quick and precisely, Raman signal is strong, and even structure for Surface enhanced raman spectroscopy substrate detection signal, stable in properties, greatly having simplified the running program detecting, improved detection efficiency, is that a kind of convenience, efficient, green, economic Surface enhanced raman spectroscopy detect substrate.Substrate prepared by the present invention can be applicable to the detection field of inorganic molecule and biomolecule.
Brief description of the drawings
Fig. 1 is that sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate enlargement factor prepared by embodiment bis-is the SEM figure of 10,000 times;
Fig. 2 is that sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate enlargement factor prepared by embodiment bis-is the SEM figure of 30,000 times;
Fig. 3 is that the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate detectable concentration of embodiment mono-to six preparation is 10
-5the Raman spectrum that mercaptobenzoic acid alcoholic solution is obtained of mol/L, 1 is the Raman spectrum substrate of embodiment mono-, 2 is the Raman spectrum substrate of embodiment bis-, 3 is the Raman spectrum substrate of embodiment tri-, 4 is the Raman spectrum substrate of embodiment tetra-, 5 is the Raman spectrum substrate of embodiment five, and 6 is the Raman spectrum substrate of embodiment six;
Fig. 4 is that the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate detectable concentration that embodiment bis-, embodiment seven, embodiment eight, embodiment nine and embodiment ten obtain is 10
-5the Raman spectrum that mercaptobenzoic acid alcoholic solution is obtained of mol/L, 1 is the Raman spectrum substrate of embodiment seven, and 2 is the Raman spectrum substrate of embodiment eight, and 3 is the Raman spectrum substrate of embodiment bis-, 4 is the Raman spectrum substrate of embodiment nine, and 5 is the Raman spectrum substrate of embodiment ten;
Fig. 5 is that the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate detectable concentration that embodiment bis-obtains is respectively 10
-5mol/L, 10
-6mol/L, 10
-7mol/L, 10
-8the Raman spectrum that mercaptobenzoic acid alcoholic solution is obtained of mol/L, 1 is 10
-5the embodiment of mol/L, 2 is 10
-6the embodiment of mol/L, 3 is 10
-7the embodiment of mol/L, 4 is 10
-8the embodiment of mol/L, 5 is blank test;
Fig. 6 takes up an official post and gets 25 points to mercaptobenzoic acid alcoholic solution is measured to obtained Raman spectrum for the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining at embodiment bis-.
Embodiment
Embodiment one: the preparation method of present embodiment sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate follows these steps to implement:
One, the silver nitrate of 45～65mg be dissolved in the ultrapure water of 250ml and boil, then adding 5～10ml mass concentration is 1% sodium citrate solution, boils to naturally cool to room temperature after 1～1.5h and obtain silver sol;
Two, filter paper is cut into filter paper, the sodium chloride solution of then putting into concentration and be 0.1～0.5mol/L soaks, and takes out after filter paper and dries and obtain dry filter paper;
Three, after the silver sol of dry filter paper being put into step 1 soaks 12h～72h, take out, at room temperature dry and obtain the substrate of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy.
In present embodiment step 3, come from the sodium chloride solution that once preparation obtains for soaking the sodium chloride solution of filter paper, in step 4, come from for soaking the silver sol of filter paper the silver sol of preparing with once.Simultaneously the use amount of silver sol should ensure that filter paper can all be immersed in silver sol, and to prepare the silver sol volume that substrate uses identical at every turn.
SERS substrate of the present invention is mainly by filter paper being soaked in to NaCl solution, be soaked in again and prepare in silver sol, remove and prepare by sodium citrate the citrate that is wrapped in silver nano-grain surface by the chlorion in NaCl solution, thereby testing sample can better be adsorbed.
Embodiment two: step 1 that what present embodiment was different with embodiment one is is dissolved in the silver nitrate of 45mg in the ultrapure water of 250ml and boils, then adding 5ml mass concentration is 1% sodium citrate solution.Other step and parameter are identical with embodiment one.
Embodiment three: the filter paper described in step 2 that what present embodiment was different with embodiment one or two is is middling speed quantitative filter paper.Other step and parameter are identical with embodiment one or two.
Filter paper is cut into triangle, ellipse or rectangle by present embodiment.
Embodiment four: the concentration of the sodium chloride solution described in step 2 that what one of present embodiment and embodiment one to three were different is is 0.25mol/L～0.35mol/L.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: the concentration of the sodium chloride solution described in step 2 that what one of present embodiment and embodiment one to three were different is is 0.3mol/L.Other step and parameter are identical with one of embodiment one to three.
Embodiment six: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what one of present embodiment and embodiment one to five were different is soaks 20h～26h.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what one of present embodiment and embodiment one to five were different is soaks 24h.Other step and parameter are identical with one of embodiment one to five.
Embodiment mono-: the preparation method of the present embodiment sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate follows these steps to realize:
One, the silver nitrate of 45mg be dissolved in the ultrapure water of 250ml and boil, then adding 5ml mass concentration is 1% sodium citrate solution, boils to naturally cool to room temperature after 1h and obtain silver sol;
Two, filter paper is cut into rectangle filter paper, the sodium chloride solution of then putting into concentration and be 0.3mol/L soaks, and takes out after filter paper and dries and obtain dry filter paper;
Three, after the silver sol of dry filter paper being put into step 1 soaks 12h, take out, at room temperature dry and obtain the substrate of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy.
Embodiment bis-: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what the present embodiment was different from embodiment mono-is soaks 24h.Other step and parameter are identical with embodiment mono-.
The SEM of the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate that the present embodiment prepares schemes as shown in Figure 1, and the SEM that amplifies 3 times schemes as shown in Figure 2.
Embodiment tri-: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what the present embodiment was different from embodiment mono-is soaks 36h.Other step and parameter are identical with embodiment mono-.
Embodiment tetra-: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what the present embodiment was different from embodiment mono-is soaks 48h.Other step and parameter are identical with embodiment mono-.
Embodiment five: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what the present embodiment was different from embodiment mono-is soaks 60h.Other step and parameter are identical with embodiment mono-.
Embodiment six: take out after the silver sol that dry filter paper is put into step 1 by step 3 that what the present embodiment was different from embodiment mono-is soaks 72h.Other step and parameter are identical with embodiment mono-.
It is 10 that the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining to embodiment mono-to six respectively drips concentration
-5mol/L to mercaptobenzoic acid alcoholic solution, then survey its Raman signal with Portable Raman spectrometer, gained Raman spectrum as shown in Figure 3.
As shown in Figure 3 in the time that the time that filter paper soaks in silver sol is 24h, in the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining, silver nano-grain aggregation is best, so the optimum soak time in silver sol is 24h for this substrate filter paper of preparation.
Embodiment seven: the preparation method of the present embodiment sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate follows these steps to realize:
One, the silver nitrate of 45mg be dissolved in the ultrapure water of 250ml and boil, then adding 5ml mass concentration is 1% sodium citrate solution, boils to naturally cool to room temperature after 1h and obtain silver sol;
Two, filter paper is cut into rectangle filter paper, the sodium chloride solution of then putting into concentration and be 0.1mol/L soaks, and takes out after filter paper and dries and obtain dry filter paper;
Three, after the silver sol of dry filter paper being put into step 1 soaks 24h, take out, at room temperature dry and obtain the substrate of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy.
Embodiment eight: it is that the sodium chloride solution of 0.2mol/L soaks that step 2 that what the present embodiment was different from embodiment seven is is put into concentration.Other step and parameter are identical with embodiment seven.
Embodiment nine: it is that the sodium chloride solution of 0.4mol/L soaks that step 2 that what the present embodiment was different from embodiment seven is is put into concentration.Other step and parameter are identical with embodiment seven.
Embodiment ten: it is that the sodium chloride solution of 0.5mol/L soaks that step 2 that what the present embodiment was different from embodiment seven is is put into concentration.Other step and parameter are identical with embodiment seven.
In the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining at embodiment bis-, embodiment seven, embodiment eight, embodiment nine, embodiment ten respectively, dripping concentration is 10
-5mol/L to mercaptobenzoic acid alcoholic solution, then survey its Raman signal with Portable Raman spectrometer, gained Raman spectrum as shown in Figure 4.
As shown in Figure 4 in the time that the concentration of sodium chloride is 0.3mol/L, in the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining, silver nano-grain aggregation is best, so be 0.3mol/L for the optimum concentration of this substrate sodium chloride of preparation.
In the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining at embodiment bis-, dripping respectively concentration is 10
-5mol/L, 10
-6mol/L, 10
-7mol/L, 10
-8mol/L to mercaptobenzoic acid alcoholic solution, then survey its Raman signal with Portable Raman spectrometer, gained Raman spectrum as shown in Figure 5, as seen from the figure, the Raman signal of the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate that embodiment bis-obtains is better, for to mercaptobenzoic acid 1075cm
-1and 1580cm
-1two characteristic peaks at place are all fairly obvious, and detection limit can reach 10
-8mol/L.
The sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate obtaining at embodiment bis-is taken up an official post and is got 25 points to mercaptobenzoic acid alcoholic solution is measured, and obtains Raman spectrum as shown in Figure 6, and SERS spectral intensity is at 1075cm
-1and 1580cm
-1the relative standard deviation at two places is respectively 9.21% and 8%, illustrates that substrate has good homogeneity.The silver nano-grain structure continuous uniform of the sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate making in conjunction with the known embodiment bis-of filter paper surface sweeping Electronic Speculum figure shown in Fig. 1, highly sensitive, can be used for detecting inorganic molecule and the biomolecule of 10ppb magnitude concentration.
Claims (7)
1. a preparation method for sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate, is characterized in that the preparation method of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy substrate follows these steps to realize:
One, the silver nitrate of 45～65mg be dissolved in the ultrapure water of 250ml and boil, then adding 5～10ml mass concentration is 1% sodium citrate solution, boils to naturally cool to room temperature after 1～1.5h and obtain silver sol;
Two, filter paper is cut into filter paper, the sodium chloride solution of then putting into concentration and be 0.1～0.5mol/L soaks, and takes out after filter paper and dries and obtain dry filter paper;
Three, after the silver sol of dry filter paper being put into step 1 soaks 12h～72h, take out, at room temperature dry and obtain the substrate of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy.
2. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 1 substrate, it is characterized in that step 1 is dissolved in the silver nitrate of 45mg in the ultrapure water of 250ml and boils, then adding 5ml mass concentration is 1% sodium citrate solution.
3. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 1 substrate, is characterized in that the filter paper described in step 2 is middling speed quantitative filter paper.
4. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 1 substrate, is characterized in that the concentration of the sodium chloride solution described in step 2 is 0.25mol/L～0.35mol/L.
5. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 4 substrate, is characterized in that the concentration of the sodium chloride solution described in step 2 is 0.3mol/L.
6. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 1 substrate, is characterized in that taking out after dry filter paper is put into step 1 by step 3 silver sol soaks 20h～26h.
7. the preparation method of a kind of sodium chloride Assisted Ag nano particle self assembly filter paper Surface enhanced raman spectroscopy according to claim 6 substrate, is characterized in that taking out after dry filter paper is put into step 1 by step 3 silver sol soaks 24h.
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| CN104237190A (en) * | 2014-10-09 | 2014-12-24 | 哈尔滨工业大学 | Methyl viologen visual detection method based on cadmium telluride quantum-dot/filter paper compound |
| CN104819975A (en) * | 2015-05-21 | 2015-08-05 | 中北大学 | Filter-paper-based silver-dendrite surface-enhanced Raman scattering active substrate and production method thereof |
| CN105403552A (en) * | 2015-11-02 | 2016-03-16 | 哈尔滨工业大学 | Preparation method of surface enhanced Raman substrate with high enhancing performance and high reproducibility |
| CN107012428A (en) * | 2017-03-20 | 2017-08-04 | 徐州赛恩斯源新材料科技有限公司 | A kind of preparation of surface enhanced substrate and the method for demarcation performance |
| CN107101990A (en) * | 2017-04-06 | 2017-08-29 | 佳木斯大学 | The surface enhanced Raman detection method of bisphenol A residues in a kind of milk |
| CN107290329A (en) * | 2017-05-17 | 2017-10-24 | 中国人民解放军第二军医大学 | A kind of preparation method and application of sulfydryl beta cyclodextrin functionalization SERS paper substrates |
| CN107727639A (en) * | 2017-11-16 | 2018-02-23 | 江苏师范大学 | The preparation method and application of the flexible sensing film of area load noble metal nano particles |
| CN108760716A (en) * | 2018-05-28 | 2018-11-06 | 山东农业大学 | A kind of Surface enhanced Raman spectroscopy wet tissue and the preparation method and application thereof |
| CN108918501A (en) * | 2018-07-17 | 2018-11-30 | 哈尔滨工业大学（深圳） | A kind of silver-paper base SERS test paper and preparation method thereof |
| CN110579465A (en) * | 2019-10-24 | 2019-12-17 | 汎锶科艺股份有限公司 | method for detecting dithiocarbamate pesticides |
| CN110907427A (en) * | 2019-12-12 | 2020-03-24 | 吉林大学 | Preparation method of SERS active test paper assisted by amino acid |
| CN111208111A (en) * | 2019-12-16 | 2020-05-29 | 北京华泰诺安探测技术有限公司 | Surface-enhanced Raman composite test paper |
| CN114414484A (en) * | 2022-01-19 | 2022-04-29 | 山东大学 | Device and method for detecting trace environmental nano pollutants by membrane filtration-surface enhanced Raman spectroscopy combination and application |
| CN115219479A (en) * | 2022-09-21 | 2022-10-21 | 中国科学院烟台海岸带研究所 | High-concentration Cl - Detection of Ag in the Environment + Method (2) |
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| CN104237190A (en) * | 2014-10-09 | 2014-12-24 | 哈尔滨工业大学 | Methyl viologen visual detection method based on cadmium telluride quantum-dot/filter paper compound |
| CN104819975A (en) * | 2015-05-21 | 2015-08-05 | 中北大学 | Filter-paper-based silver-dendrite surface-enhanced Raman scattering active substrate and production method thereof |
| CN105403552A (en) * | 2015-11-02 | 2016-03-16 | 哈尔滨工业大学 | Preparation method of surface enhanced Raman substrate with high enhancing performance and high reproducibility |
| CN107012428A (en) * | 2017-03-20 | 2017-08-04 | 徐州赛恩斯源新材料科技有限公司 | A kind of preparation of surface enhanced substrate and the method for demarcation performance |
| CN107101990B (en) * | 2017-04-06 | 2019-09-06 | 佳木斯大学 | The surface enhanced Raman detection method of bisphenol A residues in a kind of milk |
| CN107101990A (en) * | 2017-04-06 | 2017-08-29 | 佳木斯大学 | The surface enhanced Raman detection method of bisphenol A residues in a kind of milk |
| CN107290329A (en) * | 2017-05-17 | 2017-10-24 | 中国人民解放军第二军医大学 | A kind of preparation method and application of sulfydryl beta cyclodextrin functionalization SERS paper substrates |
| CN107727639A (en) * | 2017-11-16 | 2018-02-23 | 江苏师范大学 | The preparation method and application of the flexible sensing film of area load noble metal nano particles |
| CN108760716A (en) * | 2018-05-28 | 2018-11-06 | 山东农业大学 | A kind of Surface enhanced Raman spectroscopy wet tissue and the preparation method and application thereof |
| CN108918501A (en) * | 2018-07-17 | 2018-11-30 | 哈尔滨工业大学（深圳） | A kind of silver-paper base SERS test paper and preparation method thereof |
| CN110579465A (en) * | 2019-10-24 | 2019-12-17 | 汎锶科艺股份有限公司 | method for detecting dithiocarbamate pesticides |
| CN110907427A (en) * | 2019-12-12 | 2020-03-24 | 吉林大学 | Preparation method of SERS active test paper assisted by amino acid |
| CN110907427B (en) * | 2019-12-12 | 2021-11-19 | 吉林大学 | Preparation method of SERS active test paper assisted by amino acid |
| CN111208111A (en) * | 2019-12-16 | 2020-05-29 | 北京华泰诺安探测技术有限公司 | Surface-enhanced Raman composite test paper |
| CN114414484A (en) * | 2022-01-19 | 2022-04-29 | 山东大学 | Device and method for detecting trace environmental nano pollutants by membrane filtration-surface enhanced Raman spectroscopy combination and application |
| CN114414484B (en) * | 2022-01-19 | 2024-01-19 | 山东大学 | Device, method and application for detecting trace environmental nano pollutants by membrane filtration-surface enhanced Raman spectroscopy |
| CN115219479A (en) * | 2022-09-21 | 2022-10-21 | 中国科学院烟台海岸带研究所 | High-concentration Cl - Detection of Ag in the Environment + Method (2) |
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Application publication date: 20140604 |