CN105002657A - Porous polymer-Ag composite film serving as SERS substrate - Google Patents
Porous polymer-Ag composite film serving as SERS substrate Download PDFInfo
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- CN105002657A CN105002657A CN201510336645.7A CN201510336645A CN105002657A CN 105002657 A CN105002657 A CN 105002657A CN 201510336645 A CN201510336645 A CN 201510336645A CN 105002657 A CN105002657 A CN 105002657A
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- porous polymer
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- nano silver
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Abstract
The invention discloses a porous polymer-Ag composite film serving as an SERS substrate, and relates to the technical field of SERS substrate materials. A conventional SERS enhancement substrate is low in heat stability, and needs a quite strict preparing condition, i.e., the high vacuum condition. The composite film is a polylactic acid fiber accumulation film. The surface of the polylactic acid fiber is densely provided with holes of nanometer size, the diameter of each hole is 100-600 nm, and the depth of each hole is 200-500 nm. Each hole is loaded with rod-like silver nanoparticles, and the rod diameter of each rod-like silver nanoparticle is 50-65 nm. The mass of the polylactic acid fiber accounts for 80-95% of that of the polylactic acid fiber accumulation film, and the mass of the rod-like silver nanoparticles accounts for 20-5% of that of the polylactic acid fiber accumulation film. The diameter of the polylactic acid fiber is 1-8 [mu]m, and the length of the polylactic acid fiber is 300-800 [mu]m. A method for preparing the porous polymer-Ag composite film serving as the SERS substrate comprises following steps: firstly, the rod-like silver nanoparticles are prepared through a polyol reduction manner; and then fibers prepared from a spinning solution including polylactic acid and the rod-like silver nanoparticles are accumulated on a collection screen to form the porous polymer-Ag composite film through an electrostatic spinning manner.
Description
Technical field
The present invention relates to a kind of porous polymer-Ag laminated film being used as SERS substrate, belong to SERS base material technical field.
Background technology
Strengthen in substrate at existing SERS (SERS) and have a kind of metal island film SERS active-substrate, its preparation method is vacuum deposition method, i.e. depositing metal island film under the condition of high vacuum.Such as, copper substrate drips polystyrene microsphere, then under the condition of high vacuum, deposited the thick Ag island film of one deck 200nm, then modify Ag island film surface, the final Raman signal that obtains strengthens effect.This SERS strengthens substrate enrichment can detect object, this makes it possible to the material that detectable concentration is lower.But the heat endurance that this SERS strengthens substrate is bad, after temperature is elevated to a certain value, the SERS of Ag island film strengthens ability and obviously reduces.In addition, strengthen at this SERS in the preparation method of substrate, condition is very harsh, namely needs high vacuum.
Summary of the invention
Strengthen substrate to obtain a kind of SERS with good thermal stability, and preparation condition is loose, we have invented a kind of porous polymer-Ag laminated film being used as SERS substrate.
Porous polymer-Ag the laminated film being used as SERS substrate of the present invention is a kind of acid fiber by polylactic accumulating film, the hole of the densely covered nanometer scale size in its surface of described acid fiber by polylactic, and as shown in Figure 1, aperture is 100 ~ 600nm, and hole depth is 200 ~ 500nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 50 ~ 65nm, as shown in Figure 2; In described acid fiber by polylactic accumulating film, the mass percent of acid fiber by polylactic is 80 ~ 95%, and the mass percent of bar-shaped Nano silver grain is 20 ~ 5%; Described acid fiber by polylactic diameter is 1 ~ 8 μm, and as shown in Figure 3, length is 300 ~ 800 μm; Described porous polymer-Ag the laminated film being used as SERS substrate is prepared as follows, first polyol reduction method is adopted to prepare bar-shaped Nano silver grain, secondly method of electrostatic spinning is adopted by the spinning solution containing PLA, bar-shaped Nano silver grain at collection screen long-pending silk film forming, this film and porous polymer-Ag laminated film.
Its technique effect of the present invention is, porous polymer-Ag the laminated film of the present invention is used as SERS substrate, because the acid fiber by polylactic adopting method of electrostatic spinning to be formed is very very thin, the hole of nanometer scale size and gather in surface, therefore, more bar-shaped Nano silver grain can be loaded, meanwhile, the excellent footpath of described bar-shaped Nano silver grain is 50 ~ 65nm, has larger specific area, these features are all conducive to the enhancing of Raman signal, as shown in Figure 4.So the porous polymer-Ag laminated film of the present invention is equivalent to a kind of SERS and strengthens substrate.
Visible, compared with prior art, the present invention is not under the condition of high vacuum, first polymer microballoon is distributed in substrate, one deck Ag island film is deposited again at microsphere surface, again to the finishing of Ag island film, but employing method of electrostatic spinning will containing PLA, the spinning solution spinning of bar-shaped Nano silver grain, in the long-pending silk film forming of collection screen, described Nano silver grain is loaded into and gathers in the hole of polylactic acid fiber surface, so, porous polymer-Ag the complex thin film structure of the present invention is reasonable and firm, therefore, there is good heat endurance, simultaneously, its preparation does not require the harsh conditions that high vacuum is so yet.
Accompanying drawing explanation
Fig. 1 gathers the acid fiber by polylactic scanning electron microscopic picture in hole of nanometer scale size in the surface be used as in the porous polymer-Ag laminated film of SERS substrate of the present invention.Fig. 2 is the bar-shaped Nano silver grain scanning electron microscopic picture that the present invention is prepared in advance.Fig. 3 is the acid fiber by polylactic scanning electron microscopic picture be used as in the porous polymer-Ag laminated film of SERS substrate of the present invention.Fig. 4 is Raman signal intensity curve map, and this figure is simultaneously as Figure of abstract; The Raman signal intensity curve that in figure, curve A is is SERS substrate with acid fiber by polylactic accumulating film, curve B is load the Raman signal intensity curve that the acid fiber by polylactic accumulating film of bar-shaped Nano silver grain is SERS substrate, and curve C is to load bar-shaped Nano silver grain and the acid fiber by polylactic accumulating film of the PLA benzyltriethylammoinium chloride (TEBAC) that adulterates is the Raman signal intensity curve of SERS substrate.
Detailed description of the invention
Porous polymer-Ag the laminated film being used as SERS substrate of the present invention is a kind of acid fiber by polylactic accumulating film, the hole of the densely covered nanometer scale size in its surface of described acid fiber by polylactic, and aperture is 100 ~ 600nm, and hole depth is 200 ~ 500nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 50 ~ 65nm, as 60nm; In described acid fiber by polylactic accumulating film, the mass percent of acid fiber by polylactic is 80 ~ 95%, and the mass percent of bar-shaped Nano silver grain is 20 ~ 5%; Described acid fiber by polylactic diameter is 1 ~ 8 μm, and length is 300 ~ 800 μm; Described porous polymer-Ag the laminated film being used as SERS substrate is prepared as follows, first polyol reduction method is adopted to prepare bar-shaped Nano silver grain, secondly method of electrostatic spinning is adopted by the spinning solution containing PLA, bar-shaped Nano silver grain at collection screen long-pending silk film forming, this film and porous polymer-Ag laminated film.
Described its concrete scheme of porous polymer-Ag preparation method of composite film as SERS substrate is as described below.
The preparation of bar-shaped Nano silver grain:
The first step: by silver-colored source substance A gNO
3, surfactant PVP (polyvinylpyrrolidone), to mix as the EG (ethylene glycol) of reductant and solvent, magnetic agitation is to dissolving; Second step: again using the FeCl as presoma
3mix with EG and shake, in oil bath, adding thermal response; 3rd step: the product of the first two step is mixed, adds thermal response in oil bath, obtain bar-shaped Nano silver grain.The excellent footpath of described bar-shaped Nano silver grain is 50 ~ 65nm.
The preparation of porous polymer-Ag laminated film:
The CH of preparation PLA (PLA)
2cl
2(carrene) solution, adds bar-shaped Nano silver grain, as spinning solution electrostatic spinning, and long-pending silk film forming on collection screen, this film and porous polymer-Ag laminated film, acid fiber by polylactic diameter is wherein 1 ~ 8 μm, and length is 300 ~ 800 μm; The hole of the densely covered nanometer scale size in its surface of described acid fiber by polylactic, aperture is 100 ~ 600nm, and hole depth is 200 ~ 500nm.
Or in described spinning solution, also add TEBAC (benzyltriethylammoinium chloride), described TEBAC is organic synthesis phase transfer catalyst, the size of spinning fibre can be regulated and controled, spinning fibre is attenuated, such as, it is 1 ~ 2 μm that the acid fiber by polylactic diameter in porous polymer-Ag laminated film can be reduced to; Bar-shaped Nano silver grain surface active can also be helped, make it assemble, strengthen electric conductivity, obtain good SERS and strengthen ability, as shown in Figure 4.
Described method or before preparing porous polymer-Ag laminated film, in advance with the CH of PLA
2cl
2solution is spinning solution electrostatic spinning, and collection screen forms basement membrane.Porous polymer-Ag laminated film is long-pending silk film forming on this basement membrane again.
The embodiment of the described porous polymer-Ag preparation method of composite film as SERS substrate is as described below.
Embodiment 1
One, the preparation of bar-shaped Nano silver grain
The first step: the AgNO taking 0.1g
3with the PVP of 0.07g, be dissolved in the EG of 12mL, in beaker, magnetic agitation 30min is stand-by.
Second step: the EG getting 12mL again joins in there-necked flask, backward there-necked flask in add the FeCl of 1mL, 0.039mmol/L
3, mix and shake, in oil bath, being heated to 120 DEG C, maintaining reaction 5min.
3rd step: the product of the first two step is mixed, at 120 DEG C, in oil bath, react 1h, be cooled to room temperature, with acetone sedimentation reaction product, and with 6000rpm rotating speed centrifugal drying, collect lower sediment, then wash three times respectively with absolute ethyl alcohol and deionized water, remove reductant and other organic matters, obtain bar-shaped Nano silver grain powder, and be stored in ethanol.The excellent footpath of bar-shaped Nano silver grain is 60nm.
Two, the preparation of basement membrane
The CH of preparation PLA
2cl
2solution, the mass fraction of PLA in this solution is 8 ~ 12wt%, and as 10wt%, as spinning solution electrostatic spinning, spinning distance is 15cm, and spinning voltage is 15KV, long-pending silk film forming on collection screen.
Three, the preparation of porous polymer-Ag laminated film
The first step: preparation spinning solution.In described spinning solution, CH
2cl
2for solvent, the mass fraction of PLA is 8 ~ 12wt%, and as spinning fibre diameter when 10wt%, PLA mass fraction is 10wt% is more consistent, the mass fraction of bar-shaped Nano silver grain is 3 ~ 5wt%, as 3wt%; Stir 1h at normal temperatures, added each component is fully dissolved, obtains the brown solution of thickness.
Second step: electrostatic spinning.Spinning distance is 15 ~ 20cm, and as 15cm, spinning voltage is 10 ~ 15KV, as 15KV, is collecting long-pending silk film forming on the basement membrane on screen.This film and porous polymer-Ag laminated film, polylactic acid fiber surface is wherein gathered the hole of nanometer scale size, and aperture is 350nm, and hole depth is 500nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 60nm; In film, the mass percent of acid fiber by polylactic is 95%, and the mass percent of bar-shaped Nano silver grain is 5%; Described acid fiber by polylactic diameter is 5 μm, and length is 450 μm.
Embodiment 2
One, the preparation of bar-shaped Nano silver grain
The first step: the AgNO taking 0.12g
3with the PVP of 0.07g, be dissolved in the EG of 12mL, in beaker, magnetic agitation 30min is stand-by.
Second step: the EG getting 12mL again joins in there-necked flask, backward there-necked flask in add the FeCl of 1mL, 0.039mmol/L
3, mix and shake, in oil bath, being heated to 120 DEG C, maintaining reaction 5min.
3rd step: the product of the first two step is mixed, at 120 DEG C, in oil bath, react 1h, be cooled to room temperature, with acetone sedimentation reaction product, and with 6000rpm rotating speed centrifugal drying, collect lower sediment, then wash three times respectively with absolute ethyl alcohol and deionized water, remove reductant and other organic matters, obtain bar-shaped Nano silver grain powder, and be stored in ethanol.The excellent footpath of bar-shaped Nano silver grain is 50nm.
Two, the preparation of basement membrane
The CH of preparation PLA
2cl
2solution, the mass fraction of PLA in this solution is 8 ~ 12wt%, and as 10wt%, as spinning solution electrostatic spinning, spinning distance is 15cm, and spinning voltage is 15KV, long-pending silk film forming on collection screen.
Three, the preparation of porous polymer-Ag laminated film
The first step: preparation spinning solution.In described spinning solution, CH
2cl
2for solvent, the mass fraction of PLA is 8 ~ 12wt%, as 10wt%, when PLA mass fraction is 10wt%, spinning fibre diameter is more consistent, the mass fraction of bar-shaped Nano silver grain is 3 ~ 5wt%, as 3wt%, stirs 1h at normal temperatures, added each component is fully dissolved, obtains the brown solution of thickness.
Second step: electrostatic spinning.Spinning distance is 15 ~ 20cm, and as 15cm, spinning voltage is 10 ~ 15KV, as 15KV, is collecting long-pending silk film forming on the basement membrane on screen.This film and porous polymer-Ag laminated film, polylactic acid fiber surface is wherein gathered the hole of nanometer scale size, and aperture is 400nm, and hole depth is 300nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 50nm; In film, the mass percent of acid fiber by polylactic is 90%, and the mass percent of bar-shaped Nano silver grain is 10%; Described acid fiber by polylactic diameter is 8 μm, and length is 600 μm.
Embodiment 3:
Be with the difference of embodiment 1,2, in spinning solution, add TEBAC (benzyltriethylammoinium chloride), its content is 3 ~ 5wt%, as 3wt%.
Polylactic acid fiber surface in gained porous polymer-Ag laminated film is gathered the hole of nanometer scale size, and aperture is 400nm, and hole depth is 300nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 60nm; In film, the mass percent of acid fiber by polylactic is 90%, and the mass percent of bar-shaped Nano silver grain is 10%; Described acid fiber by polylactic diameter is 1 μm, and length is 300 μm.
Claims (6)
1. one kind is used as the porous polymer-Ag laminated film of SERS substrate, it is characterized in that, described porous polymer-Ag laminated film is a kind of acid fiber by polylactic accumulating film, the hole of the densely covered nanometer scale size in its surface of described acid fiber by polylactic, aperture is 100 ~ 600nm, and hole depth is 200 ~ 500nm; Load bar-shaped Nano silver grain in hole, the excellent footpath of described bar-shaped Nano silver grain is 50 ~ 65nm; In described acid fiber by polylactic accumulating film, the mass percent of acid fiber by polylactic is 80 ~ 95%, and the mass percent of bar-shaped Nano silver grain is 20 ~ 5%; Described acid fiber by polylactic diameter is 1 ~ 8 μm, and length is 300 ~ 800 μm; Described porous polymer-Ag the laminated film being used as SERS substrate is prepared as follows, first polyol reduction method is adopted to prepare bar-shaped Nano silver grain, secondly method of electrostatic spinning is adopted by the spinning solution containing PLA, bar-shaped Nano silver grain at collection screen long-pending silk film forming, this film and porous polymer-Ag laminated film.
2. porous polymer-Ag the laminated film being used as SERS substrate according to claim 1, it is characterized in that, a kind of concrete scheme that described employing polyol reduction method prepares bar-shaped Nano silver grain is: the first step: by silver-colored source substance A gNO
3, surfactant PVP, EG mixing as reductant and solvent, magnetic agitation is to dissolving; Second step: again using the FeCl as presoma
3mix with EG and shake, in oil bath, adding thermal response; 3rd step: the product of the first two step is mixed, adds thermal response in oil bath, obtain bar-shaped Nano silver grain.
3. porous polymer-Ag the laminated film being used as SERS substrate according to claim 1, it is characterized in that, a kind of concrete scheme that the spinning solution containing PLA, bar-shaped Nano silver grain is collecting the long-pending silk film forming of screen is by described employing method of electrostatic spinning: the CH of preparation PLA
2cl
2solution, adds bar-shaped Nano silver grain, as spinning solution electrostatic spinning, and long-pending silk film forming on collection screen.
4. porous polymer-Ag the laminated film being used as SERS substrate according to claim 1, is characterized in that, before preparing porous polymer-Ag laminated film, in advance with the CH of PLA
2cl
2solution is spinning solution electrostatic spinning, and collection screen forms basement membrane, and porous polymer-Ag laminated film amasss silk film forming on this basement membrane.
5. porous polymer-Ag the laminated film being used as SERS substrate according to claim 3, is characterized in that, in described spinning solution, also add TEBAC.
6. porous polymer-Ag the laminated film being used as SERS substrate according to claim 5, is characterized in that, in described spinning solution, and CH
2cl
2for solvent, the mass fraction of PLA is 8 ~ 12wt%, and the mass fraction of bar-shaped Nano silver grain is the mass fraction of 3 ~ 5wt%, TEBAC is 3 ~ 5wt%.
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| CN106498716A (en) * | 2016-10-17 | 2017-03-15 | 杭州师范大学 | A kind of polyformaldehyde/PLA SERS polymeric substrates and its preparation method and application |
| CN106702598A (en) * | 2017-01-22 | 2017-05-24 | 齐齐哈尔大学 | Method for preparing degradable graphene composite electrospun fibrous membrane |
| CN109916880A (en) * | 2019-04-22 | 2019-06-21 | 山东师范大学 | A kind of unidirectional electrostatic spinning three-dimensional Raman enhancing substrate and its preparation method and application |
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Application publication date: 20151028 |