CN103399003B - Preparation method at the bottom of a kind of SERS nano silver-group - Google Patents
Preparation method at the bottom of a kind of SERS nano silver-group Download PDFInfo
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- CN103399003B CN103399003B CN201310352817.0A CN201310352817A CN103399003B CN 103399003 B CN103399003 B CN 103399003B CN 201310352817 A CN201310352817 A CN 201310352817A CN 103399003 B CN103399003 B CN 103399003B
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Abstract
The open <b> preparation method </b> of </b><bGreatT.Gre aT.GTSERS</b><bG reatT.GreaT.GT at the bottom of nano silver-group of the present invention.Cellulose derivative is dissolved in deionized water, add a certain amount of sodium citrate, after stirring, be elevated to uniform temperature, the silver ammino solution with methocel solution same volume is added under the condition stirred, adjust ph is within the scope of 6-8, after reacting 1.5-3.5 hour, obtains at the bottom of SERS nano silver-group at 60-90 DEG C.Cheaper starting materials of the present invention, technique are simple, easy to operate, preparation is quick, easy control of process conditions, enormously simplify production process, save the time, reduce cost, there is at the bottom of prepared nano silver-group size tunable, adjustable, holding time length, steady performance, the Nano Silver of preparation has very strong surface-enhanced Raman benefit, has a wide range of applications.
Description
Technical field
The invention belongs to nanomaterial science and laser raman detection technique field, to be specifically related at the bottom of a kind of nano silver-group of Surface enhanced raman spectroscopy 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 grown up thus is that one has supersensitive Surface testing spectroscopy technique, and be used successfully to the fields such as surface chemistry, galvanochemistry, analytical chemistry and biological detection, Surface enhanced raman spectroscopy technology (SERS) is few to the requirement detecting sample, to sample without destructiveness, and highly sensitive advantage.
In 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 Raman scattering observed in an experiment mainly strengthens from the local electric field of metallic nanostructured surface, and secondly, Raman strengthens also by the impact that the particular electrical sub-resonance of raman active molecule directly contacts with metal surface with them.
Therefore the preparation of SERS substrate seems most important.Existing SERS substrate also exists the shortcomings such as reappearance is undesirable, the holding time is short, the bad regulation and control of substrate, cause SERS technology to be applied to quantitative test and there is larger difficulty, the substrate that current SERS adopts is generally the metal such as gold, silver, copper, wherein utilize silver nitrate, colloidal sol prepared by reductive agent silver, be SERS substrate the most frequently used at present.But the colloidal sol silver of at present preparation has the problems such as poor reproducibility, storage life be short, seriously limit SERS technology material quantitatively in application.
Cellulose derivative, cellulosederivatives, cellulose derivative be with the hydroxyl in cellulosic polymer and chemical reagent generation esterification or etherification reaction after product.Cellulose derivative can be divided into cellulose ether and cellulose esters and cellulose ether-esters three major types according to the design feature of resultant of reaction.The cellulose esters of actualsization 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, ester ether mixed derivative is also had.
Summary of the invention
There is the shortcomings such as reappearance is undesirable, the holding time is short, the bad regulation and control of substrate to overcome existing SERS substrate, the object of this invention is to provide the preparation method at the bottom of a kind of SERS nano silver-group, there is the advantages such as technique is simple, easy to operate, preparation is quick, easy control of process conditions.
To achieve these goals, present invention employs following technical scheme:
Preparation method at the bottom of a kind of SERS nano silver-group of the present invention, comprises the steps:
Sodium citrate is added in water-soluble cellulose ether class solution, heat after stirring and add the silver ammino solution with cellulose ethers solution same volume under the condition stirred, adjust ph is within the scope of 6-8, reacts and obtain at the bottom of the nano silver-group of SERS at 50-90 DEG C of temperature.
One in described water-soluble cellulose ether class preferable methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose or more than two kinds combinations.
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 DEG C; 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 to be more specifically:
Adopt cellulose ethers (one in methylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose or the two kinds of combinations) solution of deionized water configuration quality mark 0.05%-1%, add the sodium citrate of cellulose ethers quality 20-100%, after stirring, be elevated to 50-90 DEG C, add and the silver ammino solution of cellulose ethers solution same volume (concentration of silver ammino solution is 2mmol/L-25mmol/L) under the condition stirred, adjust ph is within the scope of 6-8, react 1.5-3.5 hour at 50-90 DEG C after, obtain at the bottom of SERS nano silver-group.
Advantage of the present invention is: 1) simple, easy to operate, the preparation of cheaper starting materials, technique fast, easy control of process conditions, enormously simplify production process, save the time, reduce cost, there is at the bottom of prepared nano silver-group size tunable, adjustable, holding time length, 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, can prepare at the bottom of the SERS nano silver-group of different-shape and particle size; Utilize the hydroxyl reductibility of cellulose ethers, the effect of preparation SERS Nano Silver seed can be played, reduce the consumption of reductive agent, reach control SERS substrate pattern and size very well; Utilize the polymer characteristics of cellulose ethers, the reunion of Nano Silver can be prevented, achieve the advantages such as the long-time preservation (storage life reaches more than 8 months) at the bottom of SERS nano silver-group.Solve prior art and prepare that the pattern that SERS Nano Silver exists is wayward, poor reproducibility, product are single, storage life is short shortcomings such as (about 3 months), at the bottom of SERS nano silver-group of the present invention as can be seen here, storage life is more than two sesquialters of prior art.
3) the nano silver-group basal surface that prepared by the present invention is also wrapped in one deck cellulose ether quasi-molecule, to polar material to be measured (material containing amino, hydroxyl or carboxyl isopolarity group), there is inrichment, thus realize enrichment and detect the effect united two into one, (do not use cellulose ethers as auxiliary agent with classic method, Nano Silver is prepared in the reduction of direct employing reductive agent) compare at the bottom of the nano silver-group prepared, there is higher sensitivity, sensitivity of the present invention is at least 10ng/L, is 100 times of prior art.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure at the bottom of nano silver-group of preparation in embodiment 1.
Fig. 2 is the transmission electron microscope figure at the bottom of nano silver-group of preparation in embodiment 2.
Fig. 3 is the transmission electron microscope figure at the bottom of nano silver-group of preparation in embodiment 3.
Fig. 4 is the Surface enhanced raman spectroscopy figure to rhodamine at the bottom of the nano silver-group of preparation in embodiment 1.
Fig. 5 is the Surface enhanced raman spectroscopy figure to rhodamine at the bottom of the nano silver-group of preparation in embodiment 2.
Fig. 6 is the Surface enhanced raman spectroscopy figure to rhodamine at the bottom of the nano silver-group of preparation in embodiment 3.
Embodiment
Below with reference to embodiment and accompanying drawing, the present invention will be further described.
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, add the sodium citrate of methylcellulose quality 0.1g, after stirring, be elevated to 75 DEG C, the silver ammino solution of 100ml10mmol/L is added under the condition stirred, adjust ph is 6.8, react at 75 DEG C after 2.5 hours, obtain at the bottom of SERS nano silver-group, transmission electron microscope figure at the bottom of nano silver-group is shown in 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, add the sodium citrate of 0.5g, after stirring, be elevated to 70 DEG C, the silver ammino solution of 100ml5mmol/L is added under the condition stirred, adjust ph is 7, react at 70 DEG C after 3 hours, obtain at the bottom of SERS nano silver-group, transmission electron microscope figure at the bottom of nano silver-group is shown in 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, add the sodium citrate of 0.05g, after stirring, be elevated to 75 DEG C, 100ml7.5mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react after 1.5 hours at 75 DEG C, obtain at the bottom of SERS nano silver-group, the transmission electron microscope figure at the bottom of nano silver-group is shown in Fig. 3, 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, add the sodium citrate of methylcellulose quality 0.3g, after stirring, be elevated to 60 DEG C, under the condition stirred, add the silver ammino solution of 100ml15mmol/L, adjust ph is 6.8, react after 2 hours at 60 DEG C, obtain, at the bottom of SERS nano silver-group, stablizing storage life 8 months.
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, add the sodium citrate of 0.15g, after stirring, be elevated to 60 DEG C, under the condition stirred, add the silver ammino solution of 100ml17.5mmol/L, adjust ph is 7, react after 3 hours at 60 DEG C, obtain, at the bottom of SERS nano silver-group, stablizing storage life 8 months.
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 DEG C, under the condition stirred, add 100ml5mmol/L silver ammino solution, adjust ph is 7, reacts after 3 hours at 75 DEG C, obtain, at the bottom of SERS nano silver-group, stablizing 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), the solution of cellulose derivative 100ml of 0.15% mass concentration is configured with deionized water, add the sodium citrate of 0.1g, after stirring, be elevated to 75 DEG C, 100ml10mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react at 75 DEG C after 2 hours, obtain at the bottom of SERS nano silver-group, stablize 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), the solution of cellulose derivative 100ml of 0.225% mass concentration is configured with deionized water, add the sodium citrate of 0.1g, after stirring, be elevated to 75 DEG C, 100ml10mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react at 75 DEG C after 2 hours, obtain at the bottom of SERS nano silver-group, stablize 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%), the solution of cellulose derivative 100ml of 0.3% mass concentration is configured with deionized water, add the sodium citrate of 0.2g, after stirring, be elevated to 75 DEG C, 100ml17.5mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react at 75 DEG C after 3 hours, obtain at the bottom of SERS nano silver-group, stablize 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%), the solution of cellulose derivative 100ml of 0.45% mass concentration is configured with deionized water, add the sodium citrate of 0.2g, after stirring, be elevated to 75 DEG C, 100ml15mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react at 75 DEG C after 3 hours, obtain at the bottom of SERS nano silver-group, stablize 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), the solution of cellulose derivative 100ml of 0.3% mass concentration is configured with deionized water, add the sodium citrate of 0.15g, after stirring, be elevated to 60 DEG C, 100ml10mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react after 2 hours at 60 DEG C, obtain, at the bottom of SERS nano silver-group, stablizing storage life 8 months.
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), the solution of cellulose derivative 100ml of 0.45% mass concentration is configured with deionized water, add the sodium citrate of 0.3g, after stirring, be elevated to 55 DEG C, 100ml17.5mmol/L silver ammino solution is added under the condition stirred, adjust ph is 7, react at 55 DEG C after 2.5 hours, obtain at the bottom of SERS nano silver-group, stablize storage life 8 months.
Application experiment
By the centrifugal 10min under 10000 turns/min condition of the obtained nano silver colloidal sol in embodiment 1, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul0.6umol/L rhodamine liquor, mix, characterize under Reinshaw RenishawInVia type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that semiconductor laser sends, and the laser power be radiated on sample strengthens signal according to this Raman and adjusts, and the Raman spectrum scope of collection is from 200cm
-1-1800cm
-1.As shown in Figure 4, in embodiment 1, the SERS substrate of preparation has rhodamine molecule and well strengthens effect, and sensitivity is 10ng/L; It is a kind of substrate of excellent performance.
By the centrifugal 10min under 10000 turns/min condition of the obtained nano silver colloidal sol in embodiment 2, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul0.6umol/L rhodamine liquor, mix, characterize under Reinshaw RenishawInVia type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that semiconductor laser sends, and the laser power be radiated on sample strengthens signal according to this Raman and adjusts, and the Raman spectrum scope of collection is from 200cm
-1-1800cm
-1.As shown in Figure 5, in embodiment 2, the SERS substrate of preparation has rhodamine molecule and well strengthens effect, and sensitivity is 8ng/L; It is a kind of substrate of excellent performance.
By the centrifugal 10min under 10000 turns/min condition of the obtained nano silver colloidal sol in embodiment 3, remove supernatant, pipetting 50ul lower floor Nano Silver is deposited on masking foil, add 50ul0.6umol/L rhodamine liquor, mix, characterize under Reinshaw RenishawInVia type micro confocal laser raman, its resolution is 2cm
-1, excitation source is the laser of the 785nm wavelength that semiconductor laser sends, and the laser power be radiated on sample strengthens signal according to this Raman and adjusts, and the Raman spectrum scope of collection is from 200cm
-1-1800cm
-1.As shown in Figure 6, in embodiment 3, the SERS substrate of preparation has rhodamine molecule and well strengthens effect, and sensitivity is 10ng/L; It is a kind of substrate of excellent performance.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (1)
1. the preparation method of SERS at the bottom of nano silver-group, comprises the steps:
Sodium citrate is added in water-soluble cellulose ether class solution, heat after stirring and add the silver ammino solution with cellulose ethers solution same volume under the condition stirred, adjust ph is within the scope of 6-8, reacts and obtain at the bottom of the nano silver-group of SERS at 50-90 DEG C of temperature; Described water-soluble cellulose ether class is one in methylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose or more than two kinds combinations; The concentration of described water-soluble cellulose ether class is massfraction 0.05%-1%; The amount of sodium citrate is the 20-100% of water-soluble cellulose ether class quality; The concentration of described silver ammino solution is 2mmol/L-25mmol/L; 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%, and hydroxypropyl content is 7.0-12%.
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CN104237204A (en) * | 2014-10-16 | 2014-12-24 | 福建师范大学 | Preparation method of cellulose-nano-silver composite microsphere substrate for SERS (Surface Enhanced Raman Scattering) |
CN106323942A (en) * | 2016-09-08 | 2017-01-11 | 福建师范大学 | Fast detecting method of grease peroxidation value |
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