CN102692405A - Rice-grain-shaped fluoride/silver composite nanometer material and preparation method and application thereof - Google Patents
Rice-grain-shaped fluoride/silver composite nanometer material and preparation method and application thereof Download PDFInfo
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- CN102692405A CN102692405A CN2012101860650A CN201210186065A CN102692405A CN 102692405 A CN102692405 A CN 102692405A CN 2012101860650 A CN2012101860650 A CN 2012101860650A CN 201210186065 A CN201210186065 A CN 201210186065A CN 102692405 A CN102692405 A CN 102692405A
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Abstract
The invention discloses a rice-grain-shaped fluoride/silver composite nanometer material. The material consists of rice-grain-shaped fluoride cores and a silver nano-particle layer, wherein silver nano-particles are gathered on the surfaces of the rice-grain-shaped cores. The invention also discloses a preparation method for the rice-grain-shaped fluoride/silver composite nanometer material and application of the rice-grain-shaped fluoride/silver composite nanometer material. Rice-grain-shaped fluoride is prepared by a hydrothermal method, and conditions are mild and controllable; the source of the rice-grain-shaped fluoride is wide, and multiple kinds of fluorides can be obtained; the silver nano-particles are sputtered in a magnetron sputtering mode, so that the method is convenient, quick, time-saving and low in cost; the product has high morphological reproducibility and can be massively produced; organic molecules and surfactant molecules are not contained in the product, so that the fluorescence interference is avoided; and according to the fluoride/silver composite nanostructure system, the fluoride absorbs the energy and transfers the energy to silver, so that the Raman scattering effect is effectively strengthened, and the single-molecule detection level can be reached on the detection of analytes.
Description
Technical field
The present invention relates to a kind of grain of rice shape fluoride/silver-colored composite nanostructure and preparation method with surface reinforced Raman active substrate.
Background technology
The fast detecting of explosive TNT/DNT is significant aspect national security, public place and environmental monitoring and protection.Current examination criteria method to the TNT/DNT liquid phase has chromatography of ions, high performance liquid chromatography.Since under the room temperature steam of TNT/DNT force down (＜100ppb), direct explosive detection gas difficulty.Gas chromatography technology (GC/MS) is that gas phase TNT/DNT detects the most frequently used method.But there are defectives such as the detection cost is high, instrument is huge, consuming time, sensitivity is low in these methods, and the public place requires and must in need not sample preparation and fast response time, accomplish with open-air detection to explosive.The current detection technology can not satisfy the requirement of on-the-spot high sensitivity fast detecting explosive, therefore, country and society be badly in need of a kind of simple, method carries out that scene is quick, these explosives of the accurate detection and Identification of high sensitivity reliably.SERS (SERS) technology because can realize fast, high sensitivity, harmless in situ detection receive extensive concern, has been applied to chemical and biology sensor, biomedical detection and fields such as trace detection and analysis.The characteristics of SERS technology are that the detection and Identification of trace TNT/DNT gas provide a kind of reliable on-the-spot new tool that detects.
In fact, how the SERS The Application of Technology depends on to a great extent that picked up signal evenly and have at the bottom of the higher SERS active group.Research shows that the rice-granule nano particle that has than big L/D ratio has desirable enhancement effect, when the dimension of polarization of incident light direction and nano material is mated, can excite maximum LSPR, produces strong SERS effect thus.The researcher utilizes distinct methods to synthesize Fe recently
2O
3Au or Fe
2O
3The Ag composite structure, as utilize triamido propyl trimethoxy silicane (APTMS) with grain of rice shape Fe
2O
3After showing functionalization, adhere to the Au seed and form Fe at last
2O
3The Au nucleocapsid structure; At grain of rice shape Fe
2O
3Surface-coated skim SiO
2As the middle layer, show deposition layer of Au or Ag at it again, form rice grain structure.Although yet existing method has obtained comparatively ideal SERS performance; But introduced couplant in the building-up process; Like alkyl, biomolecule etc., these possibly cause extra signal to disturb, especially analyte molecule the signal similar of Raman signal and coupling group the time disturb bigger.In addition, that some method also exists is time-consuming, program is loaded down with trivial details, cost is high, needs special defectives such as post-processed.
Summary of the invention
The objective of the invention is to, the deficiency in the existing detection technique provides a kind of grain of rice shape fluoride/silver-colored composite nanostructure with surface reinforced Raman active substrate and preparation method thereof.
Grain of rice shape fluoride of the present invention/silver-colored composite nano materials is that fluoride kernel and the silver nano-grain layer by grain of rice shape constitutes, and said silver nano-grain accumulates in the surface of grain of rice shape kernel.
The preparation method of grain of rice shape fluoride of the present invention/silver-colored composite nano materials comprises the steps:
(1) with volumetric molar concentration 0.1-2 molL
-1EDTA solution, slowly join volumetric molar concentration 0.1-3 molL
-1Rare-earth chloride solution in, the mol ratio of EDTA and rare earth-iron-boron is 1:1, stirring reaction 10-60 minute;
(2) in above-mentioned solution, add volumetric molar concentration 0.1-3 molL
-1Sodium fluoride or potassium fluoride solution, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner; Be provided with temperature 60-180 ℃; Continue reaction after 1-72 hour, naturally cool to room temperature, use the supercentrifuge centrifuging; Water and absolute ethyl alcohol wash respectively, obtain grain of rice shape fluoride nano material;
(3) with grain of rice shape fluoride nano material be distributed in the absolute ethyl alcohol suspension, get suspension and drop on the monocrystalline silicon piece drying;
(4) monocrystalline silicon piece is put into the vacuum chamber of magnetron sputtering apparatus, regulated 1-300 watt of magnetron sputtering power, sputtering time 1-30 minute, the magnetron sputtering silver nano-grain obtained grain of rice shape fluoride/silver-colored composite nano materials.
In step (1) and the step (2), the mol ratio of said sodium fluoride or potassium fluoride and rare earth-iron-boron is 1-20.
In the step (1), said rare earth-iron-boron is a neodymium,, the chloride of samarium, europium, terbium or holmium.
In the step (2), said washing is to carry out as cleansing solution as cleansing solution and then with absolute ethyl alcohol with deionized water earlier.
In the step (4), 10-200 watt of said magnetron sputtering power, sputtering time 5-200 second.
Grain of rice shape fluoride of the present invention/silver-colored composite nano materials is applied to the trace detection of surface enhanced Raman scattering effect.
The present invention utilizes the physical sputtering method directly the argent nano particle to be splashed on the grain of rice shape fluoride on the monocrystalline silicon piece, and fluoride nano particles is as good luminous host material, and is surperficial by after Au or the Ag modification, has good luminous enhancing ability.Fluoride shifts to metal after absorbing excitation energy as energy donor, produces huge local surface plasma resonance, can predict, and also will produce strong SERS effect.
Among the preparation method of the present invention, need not add any surfactant, organism and coupling agent, eliminate the interference that other group the product possibly cause the product Raman signal from the source, this method cost is low, simple to operate, the time spent short.Particularly, sputter procedure can firmly be fixed on Nano silver grain on the silicon chip, in actual detected, can directly place analyte to carry out the SERS test this silicon chip, and is convenient, fast, need not post-processed.The present invention, develops novel optics chemical sensitisation device and is used for trace detection the important techniques support is provided based on the senser element that SERS analyzes for development.
Do not add surfactant and organic molecule in grain of rice shape fluoride of the present invention/silver-colored composite nano materials, eliminated of the interference of unknown group from the source, improved sensitivity for analysis Raman signal.This fluoride/silver-colored composite nanostructure system, fluoride absorb energy, and shift and give silver, have effectively strengthened Raman scattering effect, can reach the Single Molecule Detection level to the detection of analyte.Can be in the use through selecting to use factors such as different sputtering times, power; The architectural feature of product is changed; Thereby make pattern, size, the surface structure of product, and surface plasma body resonant vibration that causes thus and SERS performance etc. has Modulatory character.This method is easy, efficient, cost is low, simple to operate, be fit to large-scale production.This compound substance is easy to be made into the substrate of certain size, satisfies open-air and the on-the-spot demand that detects in public place.
Beneficial effect of the present invention is:
(1) grain of rice shape fluoride adopts Hydrothermal Preparation, and mild condition is controlled;
(2) grain of rice shape fluoride wide material sources, available fluoride NaLnF
4(Ln=neodymium Nd, samarium Sm, europium Eu, terbium Tb, holmium Ho);
(3) through magnetron sputtering mode sputtering silver nano particle, convenient and swift, save time, cost is low;
(4) product pattern favorable reproducibility, but large-scale production;
(5) product does not contain any organic molecule and surfactant molecule, has avoided fluorescence interference;
(6) fluoride/silver-colored composite nanostructure system, fluoride absorb energy, and shift and give silver, have effectively strengthened Raman scattering effect, can reach the Single Molecule Detection level to the detection of analyte.
Description of drawings
Fig. 1 .1 is grain of rice shape NaNdF
4The high power scanning electron microscope diagram sheet (SEM) of nano particle, grain of rice shape NaNdF
4About 190 nm of length, about 60 nm of diameter, the size homogeneous demonstrates good monodispersity.
Fig. 1 .2 is grain of rice shape NaSmF
4The high power scanning electron microscope diagram sheet (SEM) of nano particle, grain of rice shape NaSmF
4About 190 nm of length, about 60 nm of diameter, the size homogeneous demonstrates good monodispersity.
Fig. 2 .1 is with NaSmF
4As the substrate template, fixing magnetron sputtering power 50 W, the SEM figure of sputtering time 10 s gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 2 .2 is with NaSmF
4As the substrate template, fixing magnetron sputtering power 50 W, the SEM figure of sputtering time 30 s gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 2 .3 is with NaSmF
4As the substrate template, fixing magnetron sputtering power 50 W, the SEM figure of sputtering time 150 s gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 3 .1 is with NaSmF
4As the substrate template, fixing magnetron sputtering times 30 s, the SEM figure of sputtering power 30 W gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 3 .2 is with NaSmF
4As the substrate template, fixing magnetron sputtering times 30 s, the SEM figure of sputtering power 50 W gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 3 .3 is with NaSmF
4As the substrate template, fixing magnetron sputtering times 30 s, the SEM figure of sputtering power 150 W gained grain of rice shape fluoride/silver-colored composite nano materials;
Fig. 4 is the SERS figure of grain of rice shape fluoride of the present invention/Ag composite nanostructure;
Embodiment
Following embodiment is the further description to content of the present invention; Its purpose is the explanation technology contents of the present invention of more detailed tool; But this description does not constitute any restriction to connotation of the present invention; Therefore, any based on connotation of the present invention distortion or change to work as and belong within the present invention's scope required for protection.
Embodiment 1(the synthetic grain of rice shape NaNdF of solwution method under the room temperature
4Nano particle)
Get 1 mL volumetric molar concentration, 0.2 molL
-1Neodymium trichloride solution in 100 mL beakers, add 30 mL deionized waters and mix, in beaker, add 1mL volumetric molar concentration 0.2 molL again
-1Ethylenediamine tetraacetic acid (EDTA), magnetic agitation is after 30 minutes, in above solution, adds 10 mL volumetric molar concentrations, 0.2 molL at last
-1Fluorinse, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner, 120 ℃ of temperature are set, constant temperature naturally cooled to room temperature after 24 hours.Use the supercentrifuge centrifuging, solid and with deionized water cyclic washing 3 times, more once, then it is distributed in the 5 mL absolute ethyl alcohols with absolute ethanol washing, can obtain grain of rice shape NaNdF
4The nano particle suspension, grain of rice shape NaNdF
4Appearance structure shown in Fig. 1 .1.
Embodiment 2(the synthetic grain of rice shape NaSmF of solwution method under the room temperature
4Nano particle)
Get 1 mL volumetric molar concentration, 1 molL
-1Samarium trichloride solution in 100 mL beakers, add 30 mL deionized waters and mix, in beaker, add 1mL volumetric molar concentration 1 molL again
-1EDTA, magnetic agitation is after 30 minutes, in above solution, adds 10 mL volumetric molar concentrations, 1 molL at last
-1Fluorinse, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner, 120 ℃ of temperature are set, constant temperature naturally cooled to room temperature after 24 hours.Use the supercentrifuge centrifuging,, more once, be distributed in the 5 mL absolute ethyl alcohols, can obtain grain of rice shape NaSmF with absolute ethanol washing with deionized water cyclic washing 3 times
4The nano particle suspension, grain of rice shape NaSmF
4Structure shown in Fig. 1 .2.
Embodiment 3(the synthetic grain of rice shape NaEuF of solwution method under the room temperature
4Nano particle)
Get 1 mL volumetric molar concentration, 2 molL
-1Europium chloride solution in 100 mL beakers, add 30 mL deionized waters and mix, in beaker, add 1mL volumetric molar concentration 2 molL again
-1EDTA, magnetic agitation is after 30 minutes, in above solution, adds 10 mL volumetric molar concentrations, 3 molL at last
-1Fluorinse, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner; 140 ℃ of temperature are set, and constant temperature naturally cooled to room temperature after 36 hours; Use the supercentrifuge centrifuging, with deionized water cyclic washing 3 times, more once with absolute ethanol washing; Be distributed in the 5 mL absolute ethyl alcohols, can obtain grain of rice shape NaEuF
4The nano particle suspension.
Embodiment 4(the synthetic grain of rice shape NaTbF of solwution method under the room temperature
4Nano particle)
Get 1 mL volumetric molar concentration, 0.5 molL
-1Terbium trichloride solution in 100 mL beakers, add 30 mL deionized waters and mix, in beaker, add 1mL volumetric molar concentration 0.5 molL again
-1EDTA, magnetic agitation is after 30 minutes, in above solution, adds 10 mL volumetric molar concentrations, 0.5 molL at last
-1Fluorinse, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner; Put into baking oven, 150 ℃ of temperature are set, constant temperature is after 48 hours; Naturally cool to room temperature, use the supercentrifuge centrifuging, with deionized water cyclic washing 3 times; Again once, be distributed in the 5 mL absolute ethyl alcohols, can obtain grain of rice shape NaTbF with absolute ethanol washing
4The nano particle suspension.
Embodiment 5(the synthetic grain of rice shape NaHoF of solwution method under the room temperature
4Nano particle)
Get 1 mL volumetric molar concentration, 1 molL
-1Tri-chlorination holmium solution in 100 mL beakers, add 30 mL deionized waters and mix, in beaker, add 1mL volumetric molar concentration 1molL again
-1EDTA, magnetic agitation is after 30 minutes, in above solution, adds 10 mL volumetric molar concentrations, 2 molL at last
-1Fluorinse, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner, put into baking oven, 160 ℃ of temperature are set, constant temperature naturally cooled to room temperature after 24 hours., use the supercentrifuge centrifuging, with deionized water cyclic washing 3 times, more once, be distributed in the 5 mL absolute ethyl alcohols with absolute ethanol washing, can obtain grain of rice shape NaHoF
4The nano particle suspension.
Embodiment 6(with embodiment 2 gained grain of rice shape NaSmF
4Nanoparticle is as the substrate template, and fixedly magnetron sputtering power 50 W change sputtering time)
Get embodiment 2 gained NaSmF
4Suspension drops on 2 cm * 2 cm monocrystalline silicon pieces, drying.Silicon chip is put into the vacuum chamber of magnetron sputtering apparatus, airtight, the magnetron sputtering silver nano-grain.Instrument parameter is set, opens mechanical pump, the operation molecular pump is taken out low vacuum, and vacuum tightness reaches 10
-4Pa, regulating heater current is 5 A.Logical argon gas makes about 5 Pa of sputtering chamber air pressure.Open radio-frequency power supply, fixing power 50 W of magnetron sputtering, sputter 5 s in advance open baffle plate and timing earlier, and sputtering time is 10-150 s, closes overhead gage.Instrument is cooled to room temperature, takes out silicon chip, can obtain the grain of rice shape fluoride/silver-colored composite nanostructure of different shell thicknesses and diameter.Shown in the photo that Fig. 2 .1-2.3 provides, fixing other reaction conditions, the surface structure of products therefrom is obviously different under different sputtering times, and during 10 s, the small amount of silver nano particle is only assembled on the fluoride surface.During 30 s, the fluoride surface is covered by silver nano-grain basically.Continue to prolong sputtering time, it is big that the diameter of grain of rice shape fluoride/Ag composite structure becomes, and length increases, surperficial roughening.And during 150 s, the mutual adhesion of Nano silver grain, boundary is fuzzy between the grain of rice and the grain of rice, makes grain of rice length shorten a little.
Embodiment 7(with embodiment 2 gained grain of rice shape NaSmF
4Nanoparticle is as the substrate template, and fixedly magnetron sputtering times 30 s changes sputtering power)
Get embodiment 2 gained NaSmF
4Suspension drops on 2 cm * 2 cm monocrystalline silicon pieces, drying.Silicon chip is put into the vacuum chamber of magnetron sputtering apparatus, airtight, the magnetron sputtering silver nano-grain.Set instrument parameter, adjust sputtering power 30 W respectively to 150 W, sputter 5 s open baffle plate and timing in advance, behind sputter 30 s, close overhead gage.Instrument is cooled to room temperature, takes out silicon chip, can obtain the grain of rice shape fluoride/silver-colored composite nanostructure of different shell thicknesses and diameter.Shown in the photo that Fig. 3 .1-3.3 provides.Other reaction conditions is fixed in the instance explanation, under different sputtering powers, also obtains the grain of rice shape fluoride/Ag composite structure of different surfaces structure.Its forming process is similar with sputtering time, and promptly during 30 W, the small amount of silver nano particle is splashed to grain of rice shape fluoride surface.During 50 W, silver nano-grain continues to assemble formation skim silver and covers the fluoride surface.Continue to increase sputtering power, it is big that the diameter of grain of rice shape fluoride/Ag composite structure becomes, and length increases, surperficial roughening.During power 150 W, obtained the bigger fluoride/silver composite structure of diameter, but adhesion mutually between the grain of rice, boundary is fuzzy, makes grain of rice length shorten.
Can draw through above embodiment 6,7: the power and the time of control magnetron sputtering; Can realize effective control, thereby realize the surface plasma body resonant vibration of product and the regulation and control of surface-enhanced Raman performance to product surface topography, fine structure and size.
Embodiment 8: the embodiment product is made Performance Detection
Get embodiment 2 gained NaSmF
4Suspension drops on 2 cm * 2 cm monocrystalline silicon pieces, drying.Silicon chip is put into the vacuum chamber of magnetron sputtering apparatus, airtight, the magnetron sputtering silver nano-grain.Instrument parameter is set, fixing power 50 W of magnetron sputtering, sputter 5 s in advance open baffle plate and timing earlier, and sputter 120 s close overhead gage.Instrument is cooled to room temperature, takes out silicon chip, can obtain shaggy grain of rice shape fluoride/silver-colored composite nanostructure.
With fluoride/silver-colored composite nanostructure of obtaining under this condition as the SERS active group at the bottom of, in the rhodamine 6G (R6G) of different low concentrations, soak after 12 hours respectively, take out dry; Survey its Raman signal then; Obtain SERS figure, as shown in Figure 4, with grain of rice shape fluoride/silver-colored composite nanostructure as substrate; R6G is the Raman spectrogram of probe molecule, and the minimal detectable concentration that records is 1 * 10
-17M, highest detection concentration 1 * 10
-11M, enhancer reaches 10
14Doubly, reached the Single Molecule Detection level, the signal of R6G is detailed in the spectrogram, and resolution is high.This embodiment obtains, and grain of rice shape fluoride/silver-colored composite nanostructure is as the SERS substrate, and signal is even, favorable repeatability, and detection sensitivity is high, can be used for the detection of ultratrace organic molecule and biomolecule.
Claims (7)
1. grain of rice shape fluoride/silver-colored composite nano materials, it is to be made up of the fluoride kernel of grain of rice shape and silver nano-grain layer, said silver nano-grain accumulates in the surface of grain of rice shape kernel.
2. the preparation method of the described grain of rice shape of claim 1 fluoride/silver-colored composite nano materials comprises the steps:
(1) with volumetric molar concentration 0.1-2 molL
-1EDTA solution, slowly join volumetric molar concentration 0.1-3 molL
-1Rare-earth chloride solution in, the mol ratio of EDTA and rare earth-iron-boron is 1:1, stirring reaction 10-60 minute;
(2) in above-mentioned solution, add volumetric molar concentration 0.1-3 molL
-1Sodium fluoride or potassium fluoride solution, after stirring, be transferred in the autoclave that contains polytetrafluoroethylliner liner; Be provided with temperature 60-180 ℃; Continue reaction after 1-72 hour, naturally cool to room temperature, use the supercentrifuge centrifuging; Water and absolute ethyl alcohol wash respectively, obtain grain of rice shape fluoride nano material;
(3) with grain of rice shape fluoride nano material be distributed in the absolute ethyl alcohol suspension, get suspension and drop on the monocrystalline silicon piece drying;
(4) monocrystalline silicon piece is put into the vacuum chamber of magnetron sputtering apparatus, regulated 1-300 watt of magnetron sputtering power, sputtering time 1-30 minute, the magnetron sputtering silver nano-grain obtained grain of rice shape fluoride/silver-colored composite nano materials.
3. the preparation method of grain of rice shape fluoride as claimed in claim 2/silver-colored composite nano materials is characterized in that: in step (1) and the step (2), the mol ratio of said sodium fluoride or potassium fluoride and rare earth-iron-boron is 1-20.
4. the preparation method of grain of rice shape fluoride as claimed in claim 2/silver-colored composite nano materials is characterized in that: in the step (1), said rare earth-iron-boron is a neodymium,, the chloride of samarium, europium, terbium or holmium.
5. the preparation method of grain of rice shape fluoride as claimed in claim 2/silver-colored composite nano materials is characterized in that: in the step (2), said washing is to carry out as cleansing solution as cleansing solution and then with absolute ethyl alcohol with deionized water earlier.
6. the preparation method of grain of rice shape fluoride as claimed in claim 2/silver-colored composite nano materials is characterized in that: in the step (4), and 10-200 watt of said magnetron sputtering power, sputtering time 5-200 second.
7. the grain of rice shape fluoride/silver-colored composite nano materials that is made by each described preparation method among the claim 2-6 is applied to the trace detection of surface enhanced Raman scattering effect.
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