CN102706852A - Nano island film with enhanced Raman signal and method for preparing nano island film - Google Patents
Nano island film with enhanced Raman signal and method for preparing nano island film Download PDFInfo
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- CN102706852A CN102706852A CN201210173415XA CN201210173415A CN102706852A CN 102706852 A CN102706852 A CN 102706852A CN 201210173415X A CN201210173415X A CN 201210173415XA CN 201210173415 A CN201210173415 A CN 201210173415A CN 102706852 A CN102706852 A CN 102706852A
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Abstract
The invention discloses a nano island film with an enhanced Raman signal. The nano island film comprises a polystyrene film and silicon dioxide layers which are laminated together, wherein metal nano material layers wrap the surfaces of silicon dioxide particles, which are protruded on the polystyrene film. A method for preparing the nano island film comprises the following steps of: firstly, tightly arranging silicon dioxide particle layers on the surface of slide glass by using a vertical deposition method; secondly, injecting polystyrene into the silicon dioxide layers, drying, and aminating the surface, namely connecting amino to the surface of silicon dioxide, which is protruded on the polystyrene; thirdly, absorbing gold nano particles to the surface of the silicon dioxide; and finally, adding growth liquid and a hydrogen dioxide solution, stirring and growing, and thus obtaining the nano island film with the enhanced Raman signal. The island film is low in preparation cost and high in uniformity. The island film is a good Raman enhanced substrate.
Description
Technical field
The present invention relates to island film preparation of a kind of nanometer and detection technique field, more specifically, have nanometer island film that strengthens Raman signal and preparation method thereof.
Background technology
SERS (SERS) has been widely used in fields such as chemistry, physics, medical science, biology, environmental monitoring as a kind of quick, sensitive detection method.Two kinds of enhancing substrates of SERS research original adoption are traditional solid phase substrate and colloidal metal solution.These two kinds of substrates are because the not enough homogeneous in its surface; Therefore in quantitative SERS research, use less; In recent years because the development and the widespread use of nanometer manufacturing and characterization method utilize the SERS enhancing substrate of the plasma resonance nanostructured of nano-fabrication technique preparation also to obtain increasing concern.The researchist thinks that for trace analysis substrate reinforced effects preferably is a precondition, and in quantitative test, the homogeneity of substrate is then important with repeatable preparation.Have many methods to be applied to comprise chemical self-assembly method, colloidal crystal template method, nanosphere etching method, LB module packing technique etc. in the manufacturing at the bottom of the nano based at present, nanoimprinting technology, Mechanical Method etc. then can directly depict nanostructured in substrate.Wherein, Nanosphere etching method, nanoimprinting technology, Mechanical Method etc. all need special instrument, and cost is higher; And the enhancing substrate of chemical self-assembly method preparation is not enough on homogeneity, therefore needs to seek a kind of method with low cost, simple to operate and carries out the preparation that Raman strengthens substrate.
Nanometer island film strengthens the existing long history of substrate as a kind of Raman, and traditional preparation method is redox electrochemical process, thermal vapor deposition method etc., and nanometer island its micromechanism of film of preparation is generally 50-500nm.These methods generally need special instrument, so cost is higher, and the nanometer island common homogeneity of film of preparation gained is relatively poor.
Summary of the invention
Technical matters: the purpose of this invention is to provide a kind of nanometer island film and preparation method thereof, have homogeneity and Raman enhanced activity preferably with enhancing Raman signal, and lower preparation cost.
The present invention adopts following technical scheme:
A kind of nanometer island film with enhancing Raman signal; Comprise polystyrene film and mutual silicon dioxide layer stacked together; Said silicon dioxide layer is by by array distribution and be compact arranged silicon dioxide granule and constitute; Silicon dioxide granule in the same silicon dioxide layer is positioned at same plane, and the silicon dioxide granule in the layer of silicon dioxide layer of the top protrudes in the surface of polystyrene film, in the surface clad layer of nanomaterial that protrudes in polystyrene film of silicon dioxide granule.
A kind of preparation method with the nanometer island film that strengthens Raman signal is characterized in that step is following:
Step 1) configuration volume ratio is the silicon dioxide ethanolic solution of 1:400 ~ 1:100, and microslide is vertically inserted, and after 3-5 days microslide is taken out, and can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer that compact arranged silicon dioxide granule constitutes;
Step 2) the distributed and arranged silica gel baffle plate in the both sides of silicon dioxide layer; Silicon dioxide layer perfusion volume ratio to slide surface is the polystyrene toluene solution of 1:10 again; Make its coated silica layer, dry 3-5 days, behind the formation polystyrene diaphragm solid; Automatically come off from slide surface, thereby make the silicon dioxide granule of polystyrene diaphragm solid surface protrude in the polystyrene film surface;
Diaphragm after step 3) is handled step 2 is immersed in 50 milliliters of ethanolic solutions, and adds 30 microlitre 3-aminopropyl triethoxysilanes, and 150 rev/mins of vibrations of shaking table are spent the night, and makes the silica surface of exposing surface modify upward amino;
Diaphragm after step 4) is handled step 3 is immersed in the solution of gold nanoparticles, and gold nanometer particle grain size is 4-10nm, stirs after 6 hours and takes out, cleans;
Diaphragm after step 5) is handled step 4 is immersed in 30 milliliters of growth-promoting medias, and add 150 microlitres, mass concentration is 3% superoxol, stirring reaction 30-45 minute; Promptly obtain having the nanometer island film that strengthens Raman signal; Described growth-promoting media preparation is dissolved in 25 milligrams of sal tartari in 100 ml pure waters as follows, stirs 10 minutes; Add 1.5 milliliters of mass concentrations afterwards and be 1% chlorauric acid solution, and stirred 20 minutes.
The present invention is polystyrene embedding silicon dioxide, and the silica surface that exposes on the top layer golden shell of growing.This structure is compared with other nanometer island films, and good enhancing Raman active and homogeneity are preferably arranged, and this structure owing to adopt wet chemistry method, do not need special instrument, so its preparation cost is very low, is applicable to large-scale preparation in preparation.Be solid-state structure after the polystyrene drying in addition, therefore be easy to carry.
Beneficial effect: compared with prior art, the present invention has following advantage:
(1) the present invention and the existing compared with techniques for preparing nanometer island film are with low cost, can prepare in enormous quantities.Traditional method for preparing the island film is generally electrochemical process, vapour deposition process etc., and these preparation methods generally need special instrument, so preparation cost is higher.Employed wet chemistry method does not need specific apparatus among the present invention, so preparation cost is lower.
(2) the present invention compares with the nanometer island film of classic method preparation, and better homogeneity is arranged.Shown in Figure 3 Fig. 4 is the nanometer island film Electronic Speculum figure of classic method preparation in order to utilize the nanometer island film Electronic Speculum figure of the method preparation among the present invention, and the nanometer island film that the nanometer island film that can find out the method preparation among the present invention prepares than classic method is homogeneous more.The nanometer island film of this uniform surface can make the Raman signal that records more stable, makes experimental result more reliable.
(3) the present invention be a kind of can be portable Raman strengthen substrate, be easy to carry, can be used for outdoor detection.In addition, this Raman strengthens substrate has the long holding time, as shown in Figure 6, and the raman spectrum strength decay of this nanometer island film after placing 15 days, 30 days is not obvious, and reinforced effects does not change basically.
Description of drawings
Fig. 1 is a kind of structural representation with the nanometer island film that strengthens Raman signal
Fig. 2 is a kind of preparation process synoptic diagram with the nanometer island film that strengthens Raman signal.
Fig. 3 is a kind of nanometer island film Electronic Speculum figure that strengthens Raman signal that has.
Fig. 4 is the nanometer island film Electronic Speculum figure with the classic method preparation.
Fig. 5 has the nanometer island film of metal level and the Raman spectrogram of the nanometer island film of no metal level.
Fig. 6 is a kind of its Raman reinforced effects of nanometer island film decay pattern in time that strengthens Raman signal that has.
Fig. 7 be a kind of have that the nanometer island film homogeneity that strengthens Raman signal detects draw the graceful figure of spectrum.
Embodiment
With reference to Fig. 1; A kind of nanometer island film that strengthens Raman signal that has of the present invention; Comprise: comprise polystyrene 102 and mutual silicon dioxide layer 101 stacked together; Said silicon dioxide layer is by by array distribution and be compact arranged silicon dioxide granule and constitute; Silicon dioxide granule in the same silicon dioxide layer is positioned at same plane, and the silicon dioxide granule in the layer of silicon dioxide layer of the top protrudes in the surface of polystyrene film, in the surface clad layer of nanomaterial 103 that protrudes in polystyrene film 102 of silicon dioxide granule.Wherein, the silicon dioxide granule particle diameter is 50-500nm, and the number of plies of silicon dioxide layer 101 is the 3-5 layer.
The preparation method of nanometer of the present invention island film:
Step 1) configuration volume ratio is the silicon dioxide ethanolic solution of 1:400 ~ 1:100, and microslide is vertically inserted, and after 3-5 days microslide is taken out, and can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer that compact arranged silicon dioxide granule constitutes;
Described silicon dioxide granule particle diameter is 50-500nm;
Step 2) the distributed and arranged silica gel baffle plate in the both sides of silicon dioxide layer; Silicon dioxide layer perfusion volume ratio to slide surface is the polystyrene toluene solution of 1:10 again; Make its coated silica layer, dry 3-5 days, behind the formation polystyrene diaphragm solid; Automatically come off from slide surface, thereby make the silicon dioxide granule of polystyrene diaphragm solid surface protrude in the polystyrene film surface;
Diaphragm after step 3) is handled step 2 is immersed in 50 milliliters of ethanolic solutions, and adds 30 microlitre 3-aminopropyl triethoxysilanes, and 150 rev/mins of vibrations of shaking table are spent the night, and the silica surface that is exposed at the surface is modified gone up amino;
Diaphragm after step 4) is handled step 3 is immersed in the solution of gold nanoparticles, and gold nanometer particle grain size is 4-10nm, stirs after 6 hours and takes out, cleans;
Diaphragm after step 5) is handled step 4 is immersed in 30 milliliters of growth-promoting medias, and add 150 microlitres, mass concentration is 3% superoxol, stirring reaction 30-45 minute; Promptly obtain having the nanometer island film that strengthens Raman signal; Described growth-promoting media preparation is dissolved in 25 milligrams of sal tartari in 100 ml pure waters as follows, stirs 10 minutes; Add 1.5 milliliters of mass concentrations afterwards and be 1% chlorauric acid solution, and stirred 20 minutes.
The SERS that the nanometer island film of above-mentioned preparation can carry out biomolecule detects.The solution of the biomolecule that needs are detected directly is added drop-wise to the surface of nanometer island film, waits for that use Raman spectrometer after several minutes can detect the SERS of this biomolecule.
Embodiment 1: the preparation of a kind of nanometer island film
As shown in Figure 2, the configuration volume ratio is silicon dioxide/ethanolic solution of 1:200, and microslide 11 is vertically inserted, with the microslide taking-up, can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer 12 that compact arranged silicon dioxide granule constitutes after 3-5 days.The both sides distributed and arranged silica gel baffle plate 13 of silicon dioxide layer, after the perfusion volume ratio was polystyrene/toluene solution 14 of 1:10, dry 3-5 days, polystyrene film can come off automatically, can obtain dry polystyrene film.In the one side that polystyrene film contacts with microslide, it is exposed outside to have part silicon dioxide.Polystyrene film is put into 50 milliliters of ethanolic solutions, and add 30 microlitre 3-aminopropyl triethoxysilanes, place shaking table, take out afterwards, clean with 150 rev/mins of concussions 12 hours.Put into 30 milliliters of solution of gold nanoparticles subsequently, stirred 6 hours, take out afterwash,, add 150 microlitre concentration and be 3% superoxol, stirred 30 minutes, can obtain nanometer island film with being placed in the growth-promoting media.
Embodiment 2: the preparation of a kind of nanometer island film
As shown in Figure 2, the configuration volume ratio is silicon dioxide/ethanolic solution of 1:400, and microslide 11 is vertically inserted, with the microslide taking-up, can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer 12 that compact arranged silicon dioxide granule constitutes after 3-5 days.The both sides distributed and arranged silica gel baffle plate 13 of silicon dioxide layer, after the perfusion volume ratio was polystyrene/toluene solution 14 of 1:10, dry 3 days, polystyrene film can come off automatically, can obtain dry polystyrene film.In the one side that polystyrene film contacts with microslide, it is exposed outside to have part silicon dioxide.Polystyrene film is put into 50 milliliters of ethanolic solutions, and add 30 microlitre 3-aminopropyl triethoxysilanes, place shaking table, take out afterwards, clean with 150 rev/mins of concussions 12 hours.Put into 30 milliliters of solution of gold nanoparticles subsequently, stirred 6 hours, take out afterwash,, add 150 microlitre concentration and be 3% superoxol, stirred 30 minutes, can obtain nanometer island film with being placed in the growth-promoting media.
Embodiment 3:
As shown in Figure 2, the configuration volume ratio is silicon dioxide/ethanolic solution of 1:100, and microslide 11 is vertically inserted, with the microslide taking-up, can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer 12 that compact arranged silicon dioxide granule constitutes after 3-5 days.The both sides distributed and arranged silica gel baffle plate 13 of silicon dioxide layer, after the perfusion volume ratio was polystyrene/toluene solution 14 of 1:10, dry 5 days, polystyrene film can come off automatically, can obtain dry polystyrene film.In the one side that polystyrene film contacts with microslide, it is exposed outside to have part silicon dioxide.Polystyrene film is put into 50 milliliters of ethanolic solutions, and add 30 microlitre 3-aminopropyl triethoxysilanes, place shaking table, take out afterwards, clean with 150 rev/mins of concussions 12 hours.Put into 30 milliliters of solution of gold nanoparticles subsequently, stirred 6 hours, take out afterwash,, add 150 microlitre concentration and be 3% superoxol, stirred 30 minutes, can obtain nanometer island film with being placed in the growth-promoting media.
Embodiment 4: the SERS of nanometer island film detects
Configuration concentration is 10
-4Mol/L and concentration are 10
-8The Nile blue A solution of mol/L, the nanometer island film of will not grow respectively golden shell and the golden shell of growth is immersed in 10
-4Mol/L and concentration are 10
-8In the Nile blue A solution of mol/L, take out after 2 hours, drying, and detect its Raman spectrum respectively.As shown in Figure 5, curve 1 was for soaking 10
-4The Raman spectrogram of the nanometer island film of the nothing gold shell growth of mol/L, its raman spectral signal intensity is about 3500, and curve 2 was for soaking 10
-8The Raman spectrum of the nanometer island film of the growth of the Nile blue A solution of mol/L gold shell, its signal intensity is about 140000, and the nanometer island film that can find out this golden shell of having grown has and strengthens Raman signal preferably.
Embodiment 5: the storage life of nanometer island film detects
Configuration concentration is 10
-8The Nile blue A solution of mol/L is soaked in the nanometer island film of the golden shell of having grown wherein, takes out after 2 hours, and drying, and detect its Raman spectrum.Place dry air to deposit nanometer island film afterwards, respectively at first quarter moon, take out after January, be immersed in 10 again
-8In the Nile blue A solution of mol/L 2 hours, its Raman spectrum was detected in dry back.Through the Raman spectrum that relatively detects for three times at 592cm
-1The peak at place is strong, calculates nanometer island film at the attenuation degree of preserving first quarter moon and the reinforced effects after January.As shown in Figure 6, the raman spectrum strength of preserving behind the first quarter moon does not change basically, preserve January after, the raman scattering intensity decay is about 20%, explains that this nanometer island film strengthens substrate as a kind of Raman long storage life is arranged.
Embodiment 6: the homogeneity of nanometer island film detects
Configuration concentration is 10
-8The Nile blue A solution of mol/L is soaked in the nanometer island film of the golden shell of having grown wherein, takes out after 2 hours, and drying, and detect its Raman spectrum.To with a slice nanometer island film, select 20 zones to carry out raman detection.As shown in Figure 7, spectrum is the Raman spectrum of the surperficial Buddhist nun rowland a-signal molecule of being surveyed of same nanometer island film among the figure, and these 20 spectra overlapping degree are high, and repeatability is good.In addition, extract these 20 spectrum at 592cm
-1The relative raman scattering intensity at place, and calculate their standard deviation, result of calculation is 5.96%, this standard deviation prepares the standard deviation of the nanometer island film of gained much smaller than classic method.The measured Raman signal of this nanometer island film is comparatively stable, favorable repeatability, mainly be since this nanometer island film in the preparation with SiO
2Nano particle is as template growth gold layer, and the homogeneity of the nanometer island film of last gained is good, thereby makes experimental result more reliable, can be used for the detection by quantitative of biomolecule.
Claims (3)
1. one kind has the nanometer island film that strengthens Raman signal; It is characterized in that; Comprise polystyrene film (102) and mutual silicon dioxide layer (101) stacked together; Said silicon dioxide layer (101) is by by array distribution and be compact arranged silicon dioxide granule and constitute; Silicon dioxide granule in the same silicon dioxide layer is positioned at same plane, and the silicon dioxide granule in the layer of silicon dioxide layer of the top protrudes in the surface of polystyrene film (102), coats gold nano-material layer (103) on the surface that protrudes in polystyrene film (102) of silicon dioxide granule.
2. the nanometer island film with enhancing Raman signal according to claim 1 is characterized in that the particle diameter of silicon dioxide granule is 50-500nm, and the number of plies of silicon dioxide layer (101) is the 3-5 layer.
3. preparation method with the nanometer island film that strengthens Raman signal is characterized in that step is following:
Step 1) configuration volume ratio is the silicon dioxide ethanolic solution of 1:400 ~ 1:100; And with the vertical insertion of microslide (11); After 3-5 days microslide is taken out, can obtain the 3-5 layer by by array distribution and be the silicon dioxide layer (12) that compact arranged silicon dioxide granule constitutes;
Step 2) the distributed and arranged silica gel baffle plate in the both sides of silicon dioxide layer (12); Silicon dioxide layer (12) perfusion volume ratio to slide surface is a 1:10 polystyrene toluene solution again; Make its coated silica layer, dry 3-5 days, behind the formation polystyrene diaphragm solid; Automatically come off from slide surface, thereby make the silicon dioxide granule of polystyrene diaphragm solid surface protrude in the polystyrene film surface;
Diaphragm after step 3) is handled step 2 is immersed in 50 milliliters of ethanolic solutions, and adds 30 microlitre 3-aminopropyl triethoxysilanes, places shaking table with 150 rev/mins of concussions 12 hours, and it is upward amino that the silica surface that exposes polystyrene diaphragm surface is modified;
Diaphragm after step 4) is handled step 3 is immersed in the solution of gold nanoparticles, and gold nanometer particle grain size is 4-10nm, stirs after 6 hours and takes out, cleans;
Diaphragm after step 5) is handled step 4 is immersed in 30 milliliters of growth-promoting medias, and add 150 microlitres, mass concentration is 3% superoxol, stirring reaction 30-45 minute; Promptly obtain having the nanometer island film that strengthens Raman signal; Described growth-promoting media preparation is dissolved in 25 milligrams of sal tartari in 100 ml pure waters as follows, stirs 10 minutes; Add 1.5 milliliters of mass concentrations afterwards and be 1% chlorauric acid solution, and stirred 20 minutes.
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Cited By (6)
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| CN103115912A (en) * | 2013-01-23 | 2013-05-22 | 中国科学院合肥物质科学研究院 | Surface enhanced raman spectrum printing test paper for field test and preparation method thereof |
| CN103213938A (en) * | 2013-04-16 | 2013-07-24 | 上海大学 | Surface-enhanced Raman active substrate with gold nano cap array and preparation method thereof |
| CN104458705A (en) * | 2014-12-31 | 2015-03-25 | 黑龙江大学 | Preparing method of surface enhancing Raman chip |
| CN110268250A (en) * | 2017-01-31 | 2019-09-20 | 惠普发展公司，有限责任合伙企业 | Surface enhanced infrared absorption platform |
| CN111289493A (en) * | 2020-03-27 | 2020-06-16 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| CN111426676A (en) * | 2020-04-21 | 2020-07-17 | 东华大学 | Surface enhanced Raman scattering substrate based on metal nanometer bowl and preparation method thereof |
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2012
- 2012-05-30 CN CN201210173415XA patent/CN102706852A/en active Pending
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| CLARENCE CHARNAY等: "Reduced Symmetry Metallodielectric Nanoparticles: Chemical Synthesis and Plasmonic Properties", 《JOURNAL OF PHYSICAL CHEMISTRY B》 * |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103115912A (en) * | 2013-01-23 | 2013-05-22 | 中国科学院合肥物质科学研究院 | Surface enhanced raman spectrum printing test paper for field test and preparation method thereof |
| CN103213938A (en) * | 2013-04-16 | 2013-07-24 | 上海大学 | Surface-enhanced Raman active substrate with gold nano cap array and preparation method thereof |
| CN103213938B (en) * | 2013-04-16 | 2015-12-09 | 上海大学 | Gold nano cap array surface strengthens Raman active substrate and preparation method thereof |
| CN104458705A (en) * | 2014-12-31 | 2015-03-25 | 黑龙江大学 | Preparing method of surface enhancing Raman chip |
| CN104458705B (en) * | 2014-12-31 | 2017-01-18 | 黑龙江大学 | Preparing method of surface enhancing Raman chip |
| CN110268250A (en) * | 2017-01-31 | 2019-09-20 | 惠普发展公司，有限责任合伙企业 | Surface enhanced infrared absorption platform |
| US11125693B2 (en) | 2017-01-31 | 2021-09-21 | Hewlett-Packard Development Company, L.P. | Surface enhanced infrared absorption stage |
| CN110268250B (en) * | 2017-01-31 | 2022-03-04 | 惠普发展公司，有限责任合伙企业 | Surface enhanced infrared absorption table |
| CN111289493A (en) * | 2020-03-27 | 2020-06-16 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| CN111289493B (en) * | 2020-03-27 | 2021-08-06 | 电子科技大学 | Surface-enhanced Raman substrate and preparation method thereof |
| CN111426676A (en) * | 2020-04-21 | 2020-07-17 | 东华大学 | Surface enhanced Raman scattering substrate based on metal nanometer bowl and preparation method thereof |
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Application publication date: 20121003 |