CN103399003A - Preparation method of nano silver substrate for SERS (Surface Enhanced Raman Scattering) - Google Patents
Preparation method of nano silver substrate for SERS (Surface Enhanced Raman Scattering) Download PDFInfo
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- CN103399003A CN103399003A CN2013103528170A CN201310352817A CN103399003A CN 103399003 A CN103399003 A CN 103399003A CN 2013103528170 A CN2013103528170 A CN 2013103528170A CN 201310352817 A CN201310352817 A CN 201310352817A CN 103399003 A CN103399003 A CN 103399003A
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Abstract
The invention discloses a preparation method of a nano silver substrate for SERS (Surface Enhanced Raman Scattering). The preparation method comprises the steps of dissolving a cellulose derivative in deionized water, adding a certain amount of sodium citrate, uniformly stirring while heating to a certain temperature, adding a silver ammonia solution with the same volume as that of a methylcellulose solution, regulating the pH value to be 6-8, and reacting for 1.5h-3.5h at a temperature of 60-90 DEG C to obtain the nano silver substrate for SERS. The preparation method is simple in process, convenient to operate and rapid in preparation; raw materials are low in cost and process conditions are easily controlled; the production process is greatly simplified, time is saved and the cost is lowered. The prepared nano silver substrate has the advantages of controllable and adjustable particle size, long storage time, stable property and the like, and has a strong SERS effect and wide application prospect.
Description
Technical field
The invention belongs to nanomaterial science and laser raman detection technique field, be specifically related at the bottom of nano silver-group that a kind of Surface enhanced raman spectroscopy uses and preparation method thereof.
Background technology
Surface enhanced raman spectroscopy (SERS) effect can make the Raman signal intensity of some specific nanostructured surface adsorbing species greatly be strengthened, the Surface enhanced raman spectroscopy that grows up thus is a kind of supersensitive surface detection spectroscopy technique that has, and successfully for fields such as surface chemistry, galvanochemistry, analytical chemistry and biological detection, Surface enhanced raman spectroscopy technology (SERS) is few to the requirement of test sample, to sample without destructiveness, and highly sensitive advantage.
In the Surface enhanced raman spectroscopy technology, the analysis that laser wavelength of incidence, excitation intensity, metal SERS active substrate effects on surface strengthen Raman spectrum is three vital factors; The very big enhancing of the Raman scattering that observes in experiment mainly strengthens from the local electric field on metal Nano structure surface, and secondly, Raman strengthens the impact that the particular electrical sub-resonance that also is subjected to raman active molecule directly contacts with metal surface with them.
Therefore the preparation of SERS substrate seems most important.Existing SERS substrate exists the shortcomings such as reappearance is undesirable, the holding time is short, the bad regulation and control of substrate, cause the SERS technology to be applied to quantitative test and have larger difficulty, the substrate of SERS employing at present is generally the metals such as gold, silver, copper, wherein utilizing the colloidal sol silver of silver nitrate, reductive agent preparation, is the most frequently used SERS substrate at present.But at present the colloidal sol silver of preparation has the problems such as poor reproducibility, storage life be short, has seriously limited the application in quantitatively at material of SERS technology.
Cellulose derivative, cellulose derivatives, cellulose derivative is with the product after the hydroxyl in the cellulose macromolecule and chemical reagent generation esterification or etherification reaction.Design feature according to resultant of reaction can be divided into cellulose derivative cellulose ether and cellulose esters and cellulose ether-esters three major types.The cellulose esters of actuals application has: cellulose nitrate, cellulose ethanoate, cellulose acetate butyrate and cellulose xanthate.Cellulose ethers has: methylcellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose, cyanethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methylcellulose etc.In addition, also has ester ether mixed derivative.
Summary of the invention
Exist the shortcomings such as reappearance is undesirable, the holding time is short, the bad regulation and control of substrate in order to overcome existing SERS substrate, the purpose of this invention is to provide a kind of SERS with the preparation method at the bottom of nano silver-group, have the advantages such as technique is simple, easy to operate, preparation is quick, easy control of process conditions.
To achieve these goals, the present invention has adopted following technical scheme:
A kind of SERS of the present invention, with the preparation method at the bottom of nano silver-group, comprises the steps:
Add sodium citrate in water-soluble cellulose ether class solution, heat after stirring and add silver ammino solution with cellulose ethers solution equal volume under the condition that stirs, regulating pH value is in the 6-8 scope, obtain nano silver-group that SERS uses in reacting at 50-90 ℃ of temperature at the bottom of.
A kind of or combination more than two kinds in described water-soluble cellulose ether class preferable methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose.
The concentration of described water-soluble cellulose ether class is that massfraction is preferably 0.05%-1%.
The amount of described sodium citrate is preferably the 20-100% of water-soluble cellulose ether class quality.
Described temperature of heating is preferably 50-90 ℃; The concentration of described silver ammino solution is preferably 2mmol/L-25mmol/L.
The molecular weight of described methylcellulose is preferably 30000-150000, and methoxyl content is 25-30%; The molecular weight of hydroxyethyl cellulose is preferably 220000 – 250000, and degree of substitution is 1.8-2.0; The molecular weight of hydroxypropyl methylcellulose is preferably 20000-150000, and methoxyl content is 25-30%, hydroxypropyl 7.0-12%.
The present invention adopts technical scheme more specifically to be:
Adopt cellulose ethers (a kind of or two kinds of combinations in methylcellulose, hydroxyethyl cellulose, the hydroxypropyl methylcellulose) solution of deionized water configuration quality mark 0.05%-1%, the sodium citrate that adds cellulose ethers quality 20-100%, after stirring, be elevated to 50-90 ℃, add the silver ammino solution (concentration of silver ammino solution is 2mmol/L-25mmol/L) with cellulose ethers solution equal volume under the condition that stirs, regulating the pH value is in the 6-8 scope, in reaction under 50-90 ℃ after 1.5-3.5 hour, at the bottom of obtaining SERS and using nano silver-group.
Advantage of the present invention is: 1) raw material is cheap, technique is simple, easy to operate, the preparation quick, easy control of process conditions, greatly simplified production process, saved the time, reduced cost, have at the bottom of prepared nano silver-group that particle diameter is controlled, adjustable, the holding time is long, steady performance, the Nano Silver of preparation has very strong surface-enhanced Raman benefit, has a wide range of applications.
2) utilize the diversity of the molecular structure of cellulose ethers, at the bottom of the SERS that can prepare different-shape and particle size uses nano silver-group; Utilize the hydroxyl reductibility of cellulose ethers, can play the effect of preparation SERS Nano Silver seed, reduce the consumption of reductive agent, reach fine control SERS substrate pattern and size; Utilize the polymer characteristics of cellulose ethers, can prevent the reunion of Nano Silver, realized the advantages such as long-time preservation (storage life reached more than 8 months) at the bottom of SERS is with nano silver-group.Solved that prior art prepares that SERS is wayward with the pattern that Nano Silver exists, poor reproducibility, product is single, storage life is short shortcomings such as (approximately 3 months), this shows SERS of the present invention with nano silver-group at the bottom of storage life be more than two sesquialters of prior art.
3) the nano silver-group basal surface of the present invention's preparation also is wrapped in one deck cellulose ether quasi-molecule, polar material to be measured (material that contains amino, hydroxyl or carboxyl isopolarity group) had inrichment, thereby realize enrichment and detect the effect that unites two into one, (do not use cellulose ethers as auxiliary agent with classic method, directly adopt the reductive agent reduction to prepare Nano Silver) compare at the bottom of the nano silver-group of preparation, has higher sensitivity, sensitivity of the present invention is at least 10ng/L, is 100 times of prior art.
Description of drawings
Fig. 1 is the transmission electron microscope figure at the bottom of the nano silver-group for preparing in embodiment 1.
Fig. 2 is the transmission electron microscope figure at the bottom of the nano silver-group for preparing in embodiment 2.
Fig. 3 is the transmission electron microscope figure at the bottom of the nano silver-group for preparing in embodiment 3.
Fig. 4 is to the Surface enhanced raman spectroscopy figure of rhodamine at the bottom of the nano silver-group of preparation in embodiment 1.
Fig. 5 is to the Surface enhanced raman spectroscopy figure of rhodamine at the bottom of the nano silver-group of preparation in embodiment 2.
Fig. 6 is to the Surface enhanced raman spectroscopy figure of rhodamine at the bottom of the nano silver-group of preparation in embodiment 3.
Embodiment
The present invention will be further described below with reference to embodiment and accompanying drawing.
Embodiment 1
(molecular weight is 100000 to the methylcellulose of employing deionized water configuration quality mark 0.1%, methoxyl content is 27.5%) solution 100ml, the sodium citrate that adds methylcellulose quality 0.1g, after stirring, be elevated to 75 ℃, the silver ammino solution that adds 100ml 10mmol/L under the condition that stirs, regulating the pH value is 6.8, after reacting 2.5 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, transmission electron microscope figure at the bottom of nano silver-group sees Fig. 1, and nano-scale is 50-80nm, stablizes storage life 8 months.
Embodiment 2
(molecular weight of hydroxyethyl cellulose is 220000 – 250000 to the hydroxyethyl cellulose of employing deionized water configuration quality mark 0.75%, degree of substitution is 1.8-2.0) solution 100ml, the sodium citrate that adds 0.5g, after stirring, be elevated to 70 ℃, the silver ammino solution that adds 100ml 5mmol/L under the condition that stirs, regulating the pH value is 7, after reacting 3 hours under 70 ℃, at the bottom of obtaining SERS and using nano silver-group, transmission electron microscope figure at the bottom of nano silver-group sees Fig. 2, and nano-scale is 60-80nm, stablizes storage life 8 months.
Embodiment 3
(molecular weight is 20000-150000 to the hydroxypropyl methylcellulose of employing deionized water configuration quality mark 0.075%, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) solution 100ml, the sodium citrate that adds 0.05g, after stirring, be elevated to 75 ℃, add 100ml 7.5mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after 1.5 hours, at the bottom of obtaining SERS and using nano silver-group, the transmission electron microscope figure at the bottom of nano silver-group sees Fig. 3 in reaction under 75 ℃, nano-scale is 60-70nm, stablizes storage life 8 months.
Embodiment 4
(molecular weight is 80000 to the methylcellulose of employing deionized water configuration quality mark 0.75%, methoxyl content is 27.5%) solution 100ml, the sodium citrate that adds methylcellulose quality 0.3g, after stirring, be elevated to 60 ℃, add the silver ammino solution of 100ml 15mmol/L under the condition that stirs, regulating the pH value is 6.8, after 2 hours, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months in reaction under 60 ℃.
Embodiment 5
(molecular weight of hydroxyethyl cellulose is 220000 – 250000 to the hydroxyethyl cellulose of employing deionized water configuration quality mark 0.3%, degree of substitution is 1.8-2.0) solution 100ml, the sodium citrate that adds 0.15g, after stirring, be elevated to 60 ℃, add the silver ammino solution of 100ml 17.5mmol/L under the condition that stirs, regulating the pH value is 7, after 3 hours, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months in reaction under 60 ℃.
Embodiment 6
(molecular weight is 20000-150000 to the hydroxypropyl methylcellulose of employing deionized water configuration quality mark 0.075%, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) solution 100ml, add the sodium citrate of 0.03g, after stirring, be elevated to 75 ℃, add 100ml 5mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 3 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Embodiment 7
(molecular weight is 20000-150000 to take the hydroxypropyl methylcellulose of 0.075g, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) (molecular weight of hydroxyethyl cellulose is 220000 – 250000 with the hydroxyethyl cellulose of 0.075g, degree of substitution is 1.8-2.0), solution of cellulose derivative 100ml with deionized water configuration 0.15% mass concentration, the sodium citrate that adds 0.1g, after stirring, be elevated to 75 ℃, add 100ml 10mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 2 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Embodiment 8
(molecular weight is 20000-150000 to take the hydroxypropyl methylcellulose of 0.075g, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) (molecular weight of hydroxyethyl cellulose is 220000 – 250000 with the hydroxyethyl cellulose of 0.15g, degree of substitution is 1.8-2.0), solution of cellulose derivative 100ml with deionized water configuration 0.225% mass concentration, the sodium citrate that adds 0.1g, after stirring, be elevated to 75 ℃, add 100ml 10mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 2 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Embodiment 9
(molecular weight is 20000-150000 to take the hydroxypropyl methylcellulose of 0.15g, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) (molecular weight is 80000 with the methylcellulose of 0.15g, methoxyl content is 27.5%), solution of cellulose derivative 100ml with deionized water configuration 0.3% mass concentration, the sodium citrate that adds 0.2g, after stirring, be elevated to 75 ℃, add 100ml 17.5mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 3 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Embodiment 10
(molecular weight is 20000-150000 to take the hydroxypropyl methylcellulose of 0.3g, methoxyl content is 25-30%, hydroxypropyl 7.0-12%) (molecular weight is 80000 with the methylcellulose of 0.15g, methoxyl content is 27.5%), solution of cellulose derivative 100ml with deionized water configuration 0.45% mass concentration, the sodium citrate that adds 0.2g, after stirring, be elevated to 75 ℃, add 100ml 15mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 3 hours under 75 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Embodiment 11
(molecular weight is 80000 to take the methylcellulose of 0.15g, methoxyl content is 27.5%) (molecular weight of hydroxyethyl cellulose is 220000 – 250000 with the hydroxyethyl cellulose of 0.15g, degree of substitution is 1.8-2.0), solution of cellulose derivative 100ml with deionized water configuration 0.3% mass concentration, the sodium citrate that adds 0.15g, after stirring, be elevated to 60 ℃, add 100ml 10mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after 2 hours, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months in reaction under 60 ℃.
Embodiment 12
(molecular weight is 80000 to take the methylcellulose of 0.15g, methoxyl content is 27.5%) (molecular weight of hydroxyethyl cellulose is 220000 – 250000 with the hydroxyethyl cellulose of 0.3g, degree of substitution is 1.8-2.0), solution of cellulose derivative 100ml with deionized water configuration 0.45% mass concentration, the sodium citrate that adds 0.3g, after stirring, be elevated to 55 ℃, add 100ml 17.5mmol/L silver ammino solution under the condition that stirs, regulating the pH value is 7, after reacting 2.5 hours under 55 ℃, at the bottom of obtaining SERS and using nano silver-group, stablized storage life 8 months.
Application experiment
With centrifugal 10min under making nano silver colloidal sol and turn 10000 in embodiment 1/min condition, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul 0.6umol/L rhodamine solution, mix, characterize under Reinshaw Renishaw In Via type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that sends of semiconductor laser, and the power of Ear Mucosa Treated by He Ne Laser Irradiation on sample strengthens signal according to this Raman to be adjusted, and the Raman spectrum scope of collection is from 200 cm
-1-1800cm
-1As shown in Figure 4, in embodiment 1, the SERS substrate of preparation has good enhancing effect to the rhodamine molecule, and sensitivity is 10ng/L; It is a kind of substrate of excellent performance.
With centrifugal 10min under making nano silver colloidal sol and turn 10000 in embodiment 2/min condition, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul 0.6umol/L rhodamine solution, mix, characterize under Reinshaw Renishaw In Via type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that sends of semiconductor laser, and the power of Ear Mucosa Treated by He Ne Laser Irradiation on sample strengthens signal according to this Raman to be adjusted, and the Raman spectrum scope of collection is from 200 cm
-1-1800cm
-1As shown in Figure 5, in embodiment 2, the SERS substrate of preparation has good enhancing effect to the rhodamine molecule, and sensitivity is 8ng/L; It is a kind of substrate of excellent performance.
With centrifugal 10min under making nano silver colloidal sol and turn 10000 in embodiment 3/min condition, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul 0.6umol/L rhodamine solution, mix, characterize under Reinshaw Renishaw In Via type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that sends of semiconductor laser, and the power of Ear Mucosa Treated by He Ne Laser Irradiation on sample strengthens signal according to this Raman to be adjusted, and the Raman spectrum scope of collection is from 200 cm
-1-1800cm
-1As shown in Figure 6, in embodiment 3, the SERS substrate of preparation has good enhancing effect to the rhodamine molecule, and sensitivity is 10ng/L; It is a kind of substrate of excellent performance.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (6)
1. a SERS, with the preparation method at the bottom of nano silver-group, comprises the steps:
Add sodium citrate in water-soluble cellulose ether class solution, heat after stirring and add silver ammino solution with cellulose ethers solution equal volume under the condition that stirs, regulating pH value is in the 6-8 scope, obtain nano silver-group that SERS uses in reacting at 50-90 ℃ of temperature at the bottom of.
2. a kind of SERS according to claim 1 is with the preparation method at the bottom of nano silver-group, and it is characterized in that: described water-soluble cellulose ether class is a kind of or combination more than two kinds in methylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose.
3. a kind of SERS according to claim 1 and 2 is with the preparation method at the bottom of nano silver-group, and it is characterized in that: the concentration of described water-soluble cellulose ether class is massfraction 0.05%-1%.
4. a kind of SERS according to claim 1 and 2 is with the preparation method at the bottom of nano silver-group, and it is characterized in that: the amount of sodium citrate is the 20-100% of water-soluble cellulose ether class quality.
5. a kind of SERS according to claim 1 and 2 is with the preparation method at the bottom of nano silver-group, and it is characterized in that: described temperature of heating is 50-90 ℃; The concentration of described silver ammino solution is 2mmol/L-25mmol/L.
6. a kind of SERS according to claim 2 is with the preparation method at the bottom of nano silver-group, and it is characterized in that: the molecular weight of described methylcellulose is 30000-150000, and methoxyl content is 25-30%; The molecular weight of hydroxyethyl cellulose is 220000 – 250000, and degree of substitution is 1.8-2.0; The molecular weight of hydroxypropyl methylcellulose is 20000-150000, and methoxyl content is 25-30%, hydroxypropyl 7.0-12%.
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| CN106383106A (en) * | 2016-09-08 | 2017-02-08 | 福建师范大学 | Quick detection method of trace antioxidant in grease |
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