CN101281133B - Preparation of surface reinforced Raman active substrate of large area micro-nano dendritical structure array - Google Patents
Preparation of surface reinforced Raman active substrate of large area micro-nano dendritical structure array Download PDFInfo
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- CN101281133B CN101281133B CN2008101005628A CN200810100562A CN101281133B CN 101281133 B CN101281133 B CN 101281133B CN 2008101005628 A CN2008101005628 A CN 2008101005628A CN 200810100562 A CN200810100562 A CN 200810100562A CN 101281133 B CN101281133 B CN 101281133B
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a preparation method for increasing raman activity of a basement in a surface of a large area of a micro-nano tree structure array, which firstly prepares a large area of a silicon micron cylinder array; a nanometer assembling technology is used for producing a nanometer stick in the silicon micron cylinder array. then a three-dimensional ordered periodic micro-nano structure array is obtained; and various appearance of metal nano-particles are embedded into the three-dimensional ordered periodic micro-nano structure array by using a way of a hydro-thermal synthesis method. A SERS activity basement of the invention can achieve homogenization from a centimeter grade to a large area. The invention designs SERS activity hot-particles on the three-dimensional ordered micro-nano structure, and assembles increasing effect of antenna, the increasing effect of metal/semiconductor intersection and the increasing effect of a gap into one body, then high sensitivity of the SERS activity is obtained, and the SERS activity hot-particles is firmly embedded into the tree micro-nano structure, then the invention is not only applicable for a SERS test of trace liquid-phase analyte, but also for the SERS test of trace gaseous-phase analyte.
Description
Technical field:
The present invention relates to field of nanometer material technology, chemistry, biological detection and evaluation field and Raman spectrum detection technique field, specifically is a kind of preparation method of surface reinforced Raman active substrate of large area micro-nano dendritical structure array.
Background technology:
Because surface-enhanced Raman (SERS) can provide abundant, high-quality surface molecular structural information, have in fields such as Surface Science, analysis science and life medical science extensively and great application prospect.Yet, remain the obstacle that hinders the SERS technical applicationization at the bottom of good reproducibility, the reliable high responsive SERS active group.The large-area homogenization of its key at the bottom of the SERS active group.And the maximum area that can reach homogenization at present is also only below micron order.On the other hand, because characteristics such as its ultra-high sensitive of SERS, high selectivity and response time are short more and more are subjected to the concern of sensory field in recent years, particularly Raman spectroscopy instrument has developed into the miniaturization portability, and SERS has had very big application prospect at aspects such as ultra-high sensitive, quick online trace gas detections.Yet at present a large amount of experimental studies about SERS all are to carry out on solid-liquid interface, or are soaked by liquid phase sample (or colloidal sol) and to drip dry back test at the bottom of the active group, and to detect report very less about go up SERS at solid-gas meter face (interface).And in actual biochemical material field monitoring, disease and health detection are used, need the recognition objective analyte to be dispersed in smell (analyte gas molecules) in the on-the-spot open air.Can reach other SERS technology of molecular level for detection sensitivity, the smell of surveying in this scene is to realize in theory.Key is how to allow the scent molecule of catching these minorities, makes it to be positioned on " focus " at the bottom of the SERS active group.So-called focus (hot spot) is exactly to have the metal Nano structure hot particle that strong SERS strengthens effect.At present both at home and abroad having report at the bottom of the SERS focus active group about design summarizes two classes are arranged: a class is to make close two or more metal nanoparticle aggregations on planar substrates; Another kind of is to make the slit by special template.For example, Wang etc. (Wang et al Adv.Mater.2006,18,491) by the method for electrochemical etching, control Al
2O
3Distance in the nano pore between the nano silver wire obtains " focus " that regulatable plasma resonance is coupled.Moskovits etc. (J.Am.Chem.Soc.2006,128,2200) control the time of corrosion by chemical corrosion method, have obtained the sandwich construction " focus " of metal/analyte molecule/metal.These strategies mainly distribute based on the focus on the planar substrates, its ability of catching gas molecule a little less than.
The SERS effect of extensively being approved at present is that the physical electromagnetic field strengthens and chemical charge shifts the synergy that strengthens, and wherein the enhancing of physical electromagnetic field accounts for leading.The generation that electromagnetic field strengthens is mainly returned and is come from metal local surface plasma resonance (LSPR).And LSPR can come cutting by size, pattern and the arrangement of adjusting metal nanoparticle.That is to say and to obtain by size, pattern and the arrangement of optimizing metal nanoparticle at the bottom of the active group of high electromagnetic field enhancing.Therefore, realize that at the bottom of good reproducibility, the reliable high responsive SERS active group, even, the high density that will effectively control " focus " distribute.The present invention is directed to the problem that above-mentioned SERS exists in detecting application, design uniform in the solid space of three-dimensional order " focus ", by special micro-nano structure design, collect multiple enhancer at the bottom of active group simultaneously.Improved the sensitivity at the bottom of the active group greatly.Being particularly suitable for SERS gas phase trace surveys.
Summary of the invention
The objective of the invention is to the needs surveyed at surface-enhanced Raman trace analysis thing (especially gas-phase analyte), the preparation method of surface reinforced Raman active substrate of the large area micro-nano dendritical structure array of the active focus of a kind of SERS of having is provided.
Technical scheme of the present invention:
A kind of preparation method of surface reinforced Raman active substrate of large area micro-nano dendritical structure array is characterized in that may further comprise the steps successively:
(1), the preparation of bulk silicon micron post array:
A, employing ultraviolet photolithographic technology realize a micron dot matrix pattern on silicon chip;
B, employing dry plasma etch technology prepare silicon micron post array on described silicon chip;
(2), adopt nanometer package technique even growing nano-rod of large tracts of land on described silicon micron post array, obtain three-dimensional order periodic micro/nano structure array;
(3), adopt hydrothermal synthesis method in three-dimensional order periodic micro/nano structure array, to inlay the metal nanoparticle of different-shape.
Described nanometer package technique specifically refers to chemical vapour deposition technique; The metal nanoparticle of inlaying refers to golden Au, silver-colored Ag or copper Cu nano particle.
Described growing nano-rod is meant growing ZnO nanorod.
Chemical vapour deposition technique is: the growth that will prepare the silicon chip of silicon micron post array of nanometer rods, horizontal left-hand thread is placed on the little porcelain boat that fills the chemical pure metal zinc, zinc powder in silicon chip and the little porcelain boat segment distance that staggers, vertical range between silicon chip and the zinc powder is 8-10mm, horizontal range is 2-10mm, above ready porcelain boat is put in the quartz tube furnace, begin heating then, feed argon gas simultaneously, argon flow amount is controlled at 45-55sccm (standard conditions cc/min), firing rate be the 9-12 degree/minute, when being warming up to 410-440 ℃, aerating oxygen, oxygen flow is controlled at 2-3sccm, thereafter, continues to be warming up to 550-780 ℃ with 8-12 ℃ of/minute speed, and kept this temperature 25-35 minute, naturally cool to room temperature then.
The method of embedded with metal nano particle is: synthesize the synthetic silver nano-grain of basic means original position in the ZnO nanorod surfaces of three-dimensional order periodic micro/nano structure array, space with low-temperature solvent heat.
The method of described embedded with metal nano particle is: with N, dinethylformamide is solvent preparation silver nitrate and polyvinylpyrrolidone mixed solution, wherein the proportional control of polyvinylpyrrolidone monomer and silver nitrate is at 3.0-5.0, silver nitrate concentration is the 90-150 mM, to have the silicon chip of three-dimensional order periodic micro/nano structure array and mixed solution puts into jointly and has the teflon-lined stainless steel autoclave, autoclave was remained in 140 ℃ of-180 ℃ of environment 1-2 hour, behind the natural cooling, take out silicon chip and use ethanol and deionized water rinsing respectively, nitrogen drying forms the surface reinforced Raman active substrate of micro-nano dendritical structure array.
Beneficial effect of the present invention
The present invention combines special silicon micron process technology with the nanometer package technique, obtain to have the micro-nano dendritical structure array of little, as to receive two range scales double periodicity.The present invention is based on the crystal growth kinetics theory, proposed that selectivity designs Seed Layer in advance on micrometer structure, fixed point, the even growth of nanostructures material of directed large tracts of land in specially designed growing environment are for the fusion of micro-processing technology and nanometer technology provides new effective way.
The present invention designs the active hot particle of SERS on the three-dimensional order micro-nano structure, integrate " antenna " enhancement effect, metal/semiconductor intersection enhancement effect and slit enhancement effect etc., has high-sensitive SERS activity, and the active hot particle of SERS firmly is embedded in the micro-nano structure array, make it both to be fit to trace liquid phase analysis thing SERS test, also be fit to the SERS test of trace gas-phase analyte.
Description of drawings
Fig. 1 is the synoptic diagram that the present invention prepares the surface reinforced Raman active substrate of large area micro-nano dendritical structure array.
Fig. 2 is the preparation process synoptic diagram of silicon micron post array in the inventive method.
Fig. 3 (a) and (b) obtain the photo of the scanning electron microscope of silicon micron post array.
The photo of the scanning electron microscope of the micro-nano structure array that Fig. 4 (a) and (b) are obtained.
The photo of the scanning electron microscope of the micro-nano dendritical structure array that is inlaid with silver-colored particle that Fig. 5 (a) and (b) are obtained.
Fig. 6 is 1 * 10
-5-1 * 10
-12The serial SERS spectrogram of the rhodamine of M (6GR) solution.
Fig. 7 is the SERS spectrogram of the gas phase TNT of 5ppbv.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Be three big basic step synoptic diagram of the surface reinforced Raman active substrate of preparation large area micro-nano dendritical structure array in the inventive method as shown in Figure 1.
The preparation of silicon micron post array
The preparation method of silicon microarray is mainly based on silicon dry plasma lithographic technique among the present invention.Figure 2 shows that the preparation flow figure of silicon microarray.At first adopt the ultraviolet photolithographic technology to realize micron dot matrix pattern on silicon chip, the etch mask that adopts is a ultraviolet positive photoresist.The ICP etching apparatus that adopts is the ICP180 plasma etch system that the England Oxford instrument is produced.It is characterized in that between following process conditions: 15 ℃ of temperature, etching gas SF6 flow 100sccm, passivation gas C4F8 flow 100sccm, RF power 10W, the power of ICP are 500W.
The assembling of the nanometer stick array on the silicon micron post array basis
At silicon micron post array growing nano-rod array, main chemical gas phase synthetic method grown silicon or the zinc oxide nano array that adopts based on gas-liquid-solid mechanism.The main equipment that uses is the horizontal quartz tube stove.
Concrete grammar: with the above silicon chip with silicon micrometre array post that obtains, horizontal left-hand thread is placed on the little porcelain boat that fills metal zinc (chemical pure), silicon chip and the zinc powder segment distance that staggers, and the vertical range of zinc powder and substrate is 10mm, horizontal range is 2-10mm.Put above ready porcelain boat into the quartz tube furnace center, begin then the heating, feed argon gas simultaneously, argon flow amount is controlled at 54sccm, firing rate be 10 the degree/minute, when being warming up to 420 ℃, aerating oxygen, oxygen flow is controlled at 3cm
3/ second, thereafter, continue to be warming up to preset temperature (550 ℃-780 ℃), and kept this temperature 30 minutes with 10 ℃ of/minute speed.Naturally cool to room temperature then.Nitrogen drying, the micro-nano structure array silicon chip forms.
Inlay noble metal granule in the micro-nano structure array
With low-temperature solvent heat synthesize basic means on micro-nano structure array the ZnO nanorod surfaces and the space of micro-nano structure array in the synthetic silver nano-grain of original position.Specific implementation method: with N, dinethylformamide is solvent preparation silver nitrate and polyvinylpyrrolidone mixed solution, and wherein the proportional control of polyvinylpyrrolidone monomer and silver nitrate is at 3.0-5.0.Silver nitrate concentration is the 90-150 mM, to have the silicon chip of three-dimensional order periodic micro/nano structure array and mixed solution puts into jointly and has the teflon-lined stainless steel autoclave, autoclave was remained in 140 ℃ of-180 ℃ of environment 1-2 hour, behind the natural cooling, take out silicon chip and use ethanol and deionized water rinsing respectively, nitrogen drying forms the surface reinforced Raman active substrate of micro-nano dendritical structure array.
As Fig. 5.
Embodiment 1: the rhodamine of variable concentrations is a probe, and with micro-nano dendritical structure array is SERS test at the bottom of the SERS active group
Utilizing at the bottom of the SERS active group of the present invention, is that probe has carried out the SERS spectral detection with the rhodamine of variable concentrations.Used Raman spectrometer is confocal poly-Raman spectrometer (France, JY LABRAM-HR), and LASER Light Source is an argon laser, and excitation wavelength is 514.5nm, and arriving the sample laser power is 1mW, 0.1 second integral time.Test result, the intensity that shows the rhodamine Raman scattering peak at the bottom of the SERS active group of the present invention descends with the density loss of rhodamine, can be used for detection by quantitative.See accompanying drawing 6.
Embodiment 2: with micro-nano dendritical structure array is to the SERS test of gas phase TNT at the bottom of the SERS active group
Utilize at the bottom of the SERS active group of the present invention, gas phase TNT has been carried out the SERS spectral detection.With putting into certain volume (0.3 cubic metre) closed container together with the TNT pressed powder at the bottom of the SERS active group of the present invention, after 8 hours, take out, the TNT vapor concentration is regarded as TNT saturated vapour pressure concentration, i.e. 5ppbv under the standard state in the closed container.To carrying out SERS test (seeing accompanying drawing 7) at the bottom of the active group, used Raman spectrometer is with embodiment 1., test parameter is: LASER Light Source is an argon laser, and excitation wavelength is 514.5nm, and arriving the sample laser power is 1mW, 0.5 second integral time.Test result shows that the TNT raman characteristic peak at the bottom of the SERS active group of the present invention is remarkable.
Claims (4)
1. preparation method with surface reinforced Raman active substrate of large area micro-nano dendritical structure array is characterized in that may further comprise the steps successively:
(1), the preparation of bulk silicon micron post array:
A, employing ultraviolet photolithographic technology realize a micron dot matrix pattern on silicon chip;
B, employing dry plasma etch technology prepare silicon micron post array on described silicon chip;
(2), adopt nanometer package technique large tracts of land on described silicon micron post array Zn0 nanometer rods of evenly growing, obtain three-dimensional order periodic micro/nano structure array;
(3), adopt hydrothermal synthesis method in three-dimensional order periodic micro/nano structure array, to inlay the metal nanoparticle of different-shape.
2. the preparation method with surface reinforced Raman active substrate of large area micro-nano dendritical structure array according to claim 1 is characterized in that described nanometer package technique specifically refers to chemical vapour deposition technique; The metal nanoparticle of inlaying refers to golden Au, silver-colored Ag or copper Cu nano particle.
3. the preparation method with surface reinforced Raman active substrate of large area micro-nano dendritical structure array according to claim 2, it is characterized in that chemical vapour deposition technique is: with the silicon chip of the silicon micron post array prepared, horizontal left-hand thread is placed on the little porcelain boat that fills the chemical pure metal zinc, zinc powder in silicon chip and the little porcelain boat segment distance that staggers, vertical range between silicon chip and the zinc powder is 8-10mm, horizontal range is 2-10mm, above ready porcelain boat is put in the quartz tube furnace, begin heating then, feed argon gas simultaneously, argon flow amount is controlled at 45-55sccm (standard conditions cc/min), firing rate be the 9-12 degree/minute, when being warming up to 410-440 ℃, aerating oxygen, oxygen flow is controlled at 2-3sccm, thereafter, continuation is warming up to 550-780 ℃ with 8-12 ℃ of/minute speed, and keeps this temperature 25-35 minute, naturally cools to room temperature then.
4. the preparation method with surface reinforced Raman active substrate of large area micro-nano dendritical structure array according to claim 1 is characterized in that the method for embedded with metal nano particle is: synthesize the synthetic silver nano-grain of basic means original position in the Zn0 nanorod surfaces of three-dimensional order periodic micro/nano structure array and space with low-temperature solvent heat.
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