CN105424672A - Non-stoichiometric oxide SERS substrate and preparation method thereof - Google Patents
Non-stoichiometric oxide SERS substrate and preparation method thereof Download PDFInfo
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- CN105424672A CN105424672A CN201410448710.0A CN201410448710A CN105424672A CN 105424672 A CN105424672 A CN 105424672A CN 201410448710 A CN201410448710 A CN 201410448710A CN 105424672 A CN105424672 A CN 105424672A
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- G—PHYSICS
- 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 present invention discloses a non-stoichiometric oxide SERS substrate and a preparation method thereof, wherein the substrate comprises a carrier and a non-stoichiometric oxide growing on the carrier surface. The preparation method comprises: uniformly mixing a transition metal precursor, an organic solvent and a polymer compound, placing into a carrier, and carrying out a complete reaction at a temperature of 50-280 DEG C in a sealed environment to grow the non-stoichiometric oxide material on the carrier surface so as to obtain the non-stoichiometric oxide SERS substrate, wherein the organic solvent is a polar organic solvent capable of dissolving the transition metal precursor and the polymer compound. According to the present invention, the SERS substrate has characteristics of easy preparation, low cost, wide application material system range and controlled morphology; with the simple surface modification, the regulation on the material surface phase structure can be achieved; the Raman response signal of the detected organic matter molecules can be substantially enhanced in Raman detection; and the obtained SERS substrate has the detection limit equivalent to the existing noble metal SERS substrate.
Description
Technical field
The present invention relates to a kind of SERS(Surface Enhanced Raman Scattering Spectrum) substrate and preparation method thereof, be specifically related to a kind of non-stoichiometric oxide SERS substrate and preparation method thereof, belong to molecular recognition technical field.
Background technology
Surface enhanced raman spectroscopy (SERS) is a kind of surperficial spectroscopy technique having future, can effectively molecular detection interphase interaction and interfacial characteristics, sign molecular structure and molecular adsorption behavior, thus play an increasingly important role in surface and interface science, material and even life science.SERS substrate is the key obtaining clear Raman signal, and noble metal (Au, Ag) etc. is the SERS backing material be most widely used, and Raman enhancer can reach 10
4-10
9the order of magnitude, but there is high cost, the problems such as bio-compatibility difference [
science 1997, 275,1102-1106.].Therefore, by of a great variety, the inexpensive and semiconductor material with good biological activity is applied to SERS substrate research work is subject to people's attention gradually, such as TiO
2have higher biocompatibility to have good chemical stability concurrently as SERS substrate, can tenable environment pH and temperature change [
j.Am.Chem.Soc. 2009, 131,6040-6041.].The group that simultaneously semiconducting compound surface is abundant has greatly expanded the application that SERS characterizes, and such as follows the tracks of the interfacial chemical reaction on semiconductor particle surface, the reaction kinetics research for systems such as photocatalysis provide foundation [
nanoLett. 2012, 12,4242-4246.].But the existing compound-material system with SERS activity is very limited, is confined to ZnO, Fe
2o
3, a few compound such as CdTe, and ubiquity enhancer (only 10-10 on the low side
3) shortcoming [
appl.Phys.Lett. 2007, 91,221106;
mater.Lett. 2009, 63,185-187;
j.Phys.Chem.C 2010, 114,17460-17464.].Therefore the new semiconductor material system with higher SERS activity is developed particularly important.
Summary of the invention
An object of the present invention is to provide a kind of non-stoichiometric oxide SERS substrate, it is with low cost, the Raman response signal of detected organic molecule greatly can be strengthened in Raman detection, and there is the detectability suitable with conventional noble metal SERS substrate, be applicable to many oxide nanocrystalline material system, there is universality, thus overcome deficiency of the prior art.
Two of object of the present invention is the preparation method providing described non-stoichiometric oxide SERS substrate, and it is simple that this preparation method has technique, with low cost, is easy to the advantages such as scale enforcement.
For achieving the above object, present invention employs following technical scheme:
A kind of non-stoichiometric oxide SERS substrate, comprises carrier and is grown on the non-stoichiometric oxide of carrier surface.
Further, described oxide is preferably transition metal oxide.
A kind of preparation method of non-stoichiometric oxide SERS substrate, comprise: by transition metal precursor and organic solvent and macromolecular compound Homogeneous phase mixing, and insert carrier, fully react in 50 ~ 280 DEG C in sealed environment again, thus form the non-stoichiometric oxide material with nanostructured in carrier surface growth, obtain non-stoichiometric oxide SERS substrate, wherein said organic solvent adopts the polar organic solvent that can dissolve described transition metal precursor and macromolecular compound.
Further, the mass volume ratio (g/ml) of the transition metal precursor adopted in this preparation method and organic solvent is 0.02 ~ 0.5:20 ~ 50, and the mass ratio of transition metal precursor and macromolecular compound is 0.02 ~ 0.5:0.001 ~ 50.
Further, this preparation method also can comprise: by be grown on carrier surface described non-stoichiometric oxide material in selected environment in 50 ~ 900 DEG C of calcination processing 0.5 ~ 10h, thus make described non-stoichiometric oxide material surface modifying.
Further, described polar organic solvent can be selected from but be not limited to absolute ethyl alcohol.
Further, described non-stoichiometric oxide material comprises the transition metal oxide with the phase composition of nonstoichiometry thing, such as tungsten oxide, titanium dioxide, iron oxide, zinc paste or cupric oxide etc., and is not limited thereto.
Further, described transition metal precursor comprises transition metal chloride or Organotransitionmetal complex.Wherein said transition metal can be selected from tungsten, titanium, iron, zinc, copper etc., and described Organotransitionmetal complex can be selected from tungsten chloride, butyl titanate, ferrocene, zinc acetate or Schweinfurt green, and is not limited thereto.
Further, described macromolecular compound is optional from polyglycol (PEG), polyvinylpyrrolidone (PVP), in ethyl cellulose (EC) any one, any one derivant, combinations two or more arbitrarily or derivants two or more arbitrarily combination.
Further, described carrier can adopt surface cleaning and the silicon chip of mild oxidation, but is not limited thereto.
Further, described selected environment can be selected from vacuum environment, protective atmosphere or atmosphere reactive etc., and described atmosphere reactive can be selected from but be not limited to oxidizing atmosphere or reducing atmosphere.
Further, the gas for the formation of described chosen atmosphere can be selected from any one or any two or more combination among oxygen, nitrogen, argon gas, helium, hydrogen etc., but is not limited thereto.
Further, the form of described non-stoichiometric oxide material can be unformed shape block, or preferably from quantum dot, nanometer rods, nano wire or nanometer sheet etc. or other special nanostructured.
A kind of non-stoichiometric oxide SERS substrate, primarily of aforesaid any one method preparation.
Compared with prior art, beneficial effect of the present invention comprises: this non-stoichiometric oxide SERS substrate fabrication method concise in technology, cost is low, suitable material system scope is wide, morphology controllable, and the regulation and control that can realize material surface phase structure through simple surfaces modification, the SERS that significantly can promote material is further active, thus it is high to efficiently solve existing noble metal SERS substrate cost, and semiconducting compound SERS backing material system limitation, performance is the problem such as poor generally.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 a-Fig. 1 b is XRD material phase analysis and ultraviolet-visible absorption spectroscopy figure, the respectively corresponding lines A of nonstoichiometry oxidation tungsten material in embodiment of the present invention 1-3, B, C;
Fig. 2 a-Fig. 2 c is the scanning electron microscope image of the pattern of tungsten oxide material in embodiment of the present invention 1-3;
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of tungsten oxide material after different atmosphere process in embodiment of the present invention 6-8;
Fig. 4 is the SERS performance of tungsten oxide material after different atmosphere process in embodiment of the present invention 6-8.
Fig. 5 a-Fig. 5 c be in the embodiment of the present invention 1,6,8 obtain the XPS Determination of Different Valence States collection of illustrative plates of W element in tungsten oxide material;
Fig. 6 is the Raman signal of commodity tungsten oxide and silicon chip surface.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.The example of these preferred implementations illustrates in the accompanying drawings.Shown in accompanying drawing and the embodiments of the present invention described with reference to the accompanying drawings be only exemplary, and the present invention is not limited to these embodiments.
At this, also it should be noted that, in order to avoid the present invention fuzzy because of unnecessary details, illustrate only in the accompanying drawings with according to the closely-related structure of the solution of the present invention and/or treatment step, and eliminate other details little with relation of the present invention.
Invention broadly provides a kind of preparation and surface modifying method of non-stoichiometric oxide SERS substrate of morphology controllable, it mainly adopts the macromolecule organics such as polymkeric substance to control material morphology, then reconcile material surface chemical composition and phase structure by the thermal treatment in different atmosphere, the SERS significantly promoting material while keeping material morphology is active.
Preparation and the surface modifying method of this non-stoichiometric oxide SERS substrate can comprise: mixed with absolute ethyl alcohol and macromolecular compound by transition metal precursor, proceed in hydrothermal reaction kettle, by carrier, such as silicon chip is placed in the mixed liquor of above-mentioned hydrothermal reaction kettle, in 50 ~ 280 DEG C of fully reactions (reaction time is preferably 0.5 ~ 24h) after sealing, obtain the non-stoichiometric oxide with certain nanostructured being grown on carrier surface, more successively through washing, drying, obtain product.
Wherein, described oxide comprises the conventional metal oxide, particularly transition metal oxide such as tungsten oxide, titanium dioxide, iron oxide, zinc paste, cupric oxide.
Wherein, described macromolecular compound can be selected but be not limited to dissolve in polymkeric substance or other macromolecular compounds of ethanol, such as polyglycol (PEG), polyvinylpyrrolidone (PVP), the or derivatives thereofs such as ethyl cellulose (EC).
Wherein, when adopting silicon chip as carrier, should fully clean before use to ensure surface cleaning, and need mild oxidation.
Further, the form of described substrate can be unformed shape block, but preferably has the nanostructured of special appearance from quantum dot, nanometer rods, nano wire, nanometer sheet etc., and is not limited thereto.
Preferably, also can carry out surface modifying method to obtained non-stoichiometric oxide, its process comprises: by the above-mentioned non-stoichiometric oxide being grown on carrier surface in different atmosphere in 50 ~ 900 DEG C, preferably at 100 ~ 500 DEG C of calcination processing 0.5 ~ 10h, thus realize the surface modification to non-stoichiometric oxide.
Further, described atmosphere comprises vacuum, atmospheric environment or pass into inertia, oxidisability, reducibility gas, such as, passes into gas and can select but any one or the wherein two or more arbitrarily combinations that are not limited to oxygen, nitrogen, argon gas, helium, hydrogen.
In an exemplary embodiments, this material preparation method can comprise the following steps: be scattered in absolute ethyl alcohol by transition metal precursor A and macromolecule organic B, certain atmosphere, after such as, stirring certain hour under normal atmospheric or the inert atmosphere such as nitrogen, helium, be transferred to hydrothermal reaction kettle, carrier is placed in described mixed liquor, thermal response certain hour is added after sealing, naturally cool to room temperature, successively after deionized water and ethanol washing several times, drying can obtain the non-stoichiometric oxide SERS substrate being grown on silicon chip.
Obviously, material preparation of the present invention and surface modifying method only need shirtsleeve operation and common agents and equipment to complete, convenient and swift, with low cost, are easy to scale and implement.
The present invention is applicable to various common metal oxide materials system, and the non-stoichiometric oxide through surface modification is especially suitable as the Raman analysis detection that SERS substrate is applied to gas chromatography molecule.
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.
embodiment 1
By the WCl of 0.1g
6be dissolved in 30ml absolute ethyl alcohol, N
2being transferred to volume after protection lower stirring 0.5h is in the teflon hydrothermal reaction kettle of 70ml; 1cm × 1cm silicon chip to be placed in aforesaid reaction vessel in reaction mixture through acetone supersound washing post-drying, at 180 DEG C of reaction 24h after sealing, naturally cool to room temperature, take out silicon chip fully to wash with deionized water, ethanol successively, dry 12h for 60 DEG C, obtain the nonstoichiometry oxidation tungsten SERS backing material being grown on silicon chip surface, wherein XPS ultimate analysis+6 valency is shown in Fig. 5 a with the relative scale of+5 valency tungsten.
embodiment 2
By the WCl of 0.1g
6be dissolved in 30ml absolute ethyl alcohol and mix with the PEG-400 of 20ml, N
2being transferred to volume after protection lower stirring 0.5h is in the teflon hydrothermal reaction kettle of 70ml; 1cm × 1cm silicon chip to be placed in aforesaid reaction vessel in reaction mixture through acetone supersound washing post-drying, at 180 DEG C of reaction 18h after sealing, naturally cool to room temperature, take out silicon chip fully to wash with deionized water, ethanol successively, dry 12h for 60 DEG C, obtain the nonstoichiometry oxidation tungsten SERS backing material being grown on silicon chip surface.
embodiment 3
By the WCl of 0.1g
630ml absolute ethyl alcohol is jointly dissolved in, N with the PVP of 5mg
2being transferred to volume after protection lower stirring 0.5h is in the teflon hydrothermal reaction kettle of 70ml; 1cm × 1cm silicon chip to be placed in aforesaid reaction vessel in reaction mixture through acetone supersound washing post-drying, at 180 DEG C of reaction 18h after sealing, naturally cool to room temperature, take out silicon chip fully to wash with deionized water, ethanol successively, dry 12h for 60 DEG C, obtain the nonstoichiometry oxidation tungsten SERS backing material being grown on silicon chip surface.
embodiment 4
The butyl titanate of 0.2g is dissolved in 40ml absolute ethyl alcohol, N
2being transferred to volume after protection lower stirring 0.5h is in the teflon hydrothermal reaction kettle of 70ml; 1cm × 1cm silicon chip to be placed in aforesaid reaction vessel in reaction mixture through acetone supersound washing post-drying, at 180 DEG C of reaction 24h after sealing, naturally cool to room temperature, take out silicon chip fully to wash with deionized water, ethanol successively, dry 12h for 60 DEG C, obtain the nonstoichiometry oxidation titanium SERS backing material being grown on silicon chip surface.
embodiment 5
The zinc acetate of 0.1g is dissolved in 40ml absolute ethyl alcohol, N
2being transferred to solvent after protection lower stirring 0.5h is in the teflon hydrothermal reaction kettle of 70ml; 1cm × 1cm silicon chip to be placed in aforesaid reaction vessel in reaction mixture through acetone supersound washing post-drying, at 180 DEG C of reaction 24h after sealing, naturally cool to room temperature, take out silicon chip fully to wash with deionized water, ethanol successively, dry 12h for 60 DEG C, obtain the nonstoichiometry oxidation zinc SERS backing material being grown on silicon chip surface.
embodiment 6
To be grown on tungsten oxide SERS backing material 350 DEG C of calcining 3h in air atmosphere of silicon chip surface in embodiment 1, obtain the nonstoichiometry oxidation tungsten SERS substrate of surface modification, be designated as A, wherein XPS ultimate analysis+6 valency is shown in Fig. 5 b with the relative scale of+5 valency tungsten.
embodiment 7
Tungsten oxide SERS backing material 350 DEG C of calcining 3h under an argon atmosphere of silicon chip surface will be grown in embodiment 1, and obtain the nonstoichiometry oxidation tungsten SERS substrate of surface modification, be designated as B.
embodiment 8
Tungsten oxide SERS backing material 300 DEG C of calcining 3h under hydrogen/argon gas mixed atmosphere of silicon chip surface will be grown in embodiment 1, obtain the nonstoichiometry oxidation tungsten SERS substrate of surface modification, be designated as C, wherein XPS ultimate analysis+6 valency is shown in Fig. 5 c with the relative scale of+5 valency tungsten.
Consult XRD material phase analysis and ultraviolet-visible absorption spectroscopy figure that Fig. 1 a-1b is nonstoichiometry oxidation tungsten material in embodiment 1-3, and Fig. 2 a-Fig. 2 c is that in embodiment 1-3, institute obtains the scanning electron microscope image that nonstoichiometry is oxidized the pattern of tungsten material.
Refer to shown in Fig. 3 is that in embodiment 6-8, the ultraviolet-visible absorption spectroscopy figure of tungsten oxide material after different atmosphere process, Fig. 4 are the SERS performance of tungsten oxide material after different atmosphere process in embodiment 6-8 again.
Non-stoichiometric oxide SERS substrate of the present invention can be applicable in SERS test, and such as, the R6G aqueous dye solutions of 200 μ L can be coated embodiment 1-8 and obtain on non-stoichiometric oxide SERS substrate, lucifuge carries out Raman spectral detection after drying.Test condition is: optical maser wavelength 532nm, object lens magnification 50 times, signals collecting time 10s, 5 zones of different collection signals are selected respectively to same sample, and average to determine Raman peak intensity, can see that creating obvious Raman strengthens signal, namely 611,773,1186,1310,1360,1505,1570 and 1650cm
-1the Raman characteristic peak of dye molecule is observed in position.And commodity tungsten oxide or silicon chip, as there is no above Raman signal during substrate, are shown in Fig. 6 under same test condition.
The present invention builds SERS substrate by adopting a based semiconductor oxide with the phase composition of nonstoichiometry thing, it relates to many oxide nanocrystalline material system and has universality, greatly can strengthen the Raman response signal of detected organic molecule in Raman detection, and there is the detectability suitable with conventional noble metal SERS substrate.
It is pointed out that above-described embodiment is only and technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (12)
1. the preparation method of a non-stoichiometric oxide SERS substrate, it is characterized in that comprising: by transition metal precursor and organic solvent and macromolecular compound Homogeneous phase mixing, and insert carrier, fully react in 50 ~ 280 DEG C in sealed environment again, thus form the non-stoichiometric oxide material with nanostructured in carrier surface growth, obtain non-stoichiometric oxide SERS substrate, wherein said organic solvent adopts the polar organic solvent that can dissolve described transition metal precursor and macromolecular compound.
2. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1, characterized by further comprising: by be grown on carrier surface described non-stoichiometric oxide material in selected environment in 50 ~ 900 DEG C of calcination processing 0.5 ~ 10h, thus make described non-stoichiometric oxide material surface modifying.
3. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, is characterized in that described polar organic solvent comprises absolute ethyl alcohol.
4. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, it is characterized in that described non-stoichiometric oxide material comprises the transition metal oxide with the phase composition of nonstoichiometry thing, described transition metal oxide comprises tungsten oxide, titanium dioxide, iron oxide, zinc paste or cupric oxide.
5. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, it is characterized in that described transition metal precursor comprises transition metal chloride or Organotransitionmetal complex, described Organotransitionmetal complex comprises tungsten chloride, butyl titanate, ferrocene, zinc acetate or Schweinfurt green.
6. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, it is characterized in that described macromolecular compound comprise in polyglycol, polyvinylpyrrolidone, ethyl cellulose any one, any one derivant, combinations two or more arbitrarily or derivants two or more arbitrarily combination.
7. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, is characterized in that described carrier adopts surface cleaning and the silicon chip of mild oxidation.
8. the preparation method of non-stoichiometric oxide SERS substrate according to claim 2, it is characterized in that described selected environment comprises vacuum environment, protective atmosphere or atmosphere reactive, described atmosphere reactive comprises oxidizing atmosphere or reducing atmosphere.
9. the preparation method of non-stoichiometric oxide SERS substrate according to claim 2, is characterized in that any one or any two or more combination comprised for the formation of the gas of described chosen atmosphere in oxygen, nitrogen, argon gas, helium, hydrogen.
10. the preparation method of non-stoichiometric oxide SERS substrate according to claim 1 and 2, is characterized in that the form of described non-stoichiometric oxide material comprises unformed shape block, quantum dot, nanometer rods, nano wire or nanometer sheet.
11. 1 kinds of non-stoichiometric oxide SERS substrates, is characterized in that comprising carrier and being grown on the non-stoichiometric oxide with nanostructured of carrier surface.
12. 1 kinds of non-stoichiometric oxide SERS substrates that according to any one of claim 1-10 prepared by method.
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| CN106756853A (en) * | 2017-03-03 | 2017-05-31 | 东南大学 | Tungsten oxide substrate with SERS function and preparation method thereof |
| CN109342401A (en) * | 2018-12-06 | 2019-02-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application of the semiconducting compound in the identification and identification in vinegar vinegar age |
| CN109342400A (en) * | 2018-12-06 | 2019-02-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application of the semiconducting compound in the identification and identification in grape wine source area |
| CN109596595A (en) * | 2018-12-06 | 2019-04-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application and detection method of the semiconducting compound in benzaldehyde specific detection |
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| CN111103278A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | SERS chip and manufacturing and regenerating method thereof |
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| US11255792B2 (en) | 2016-07-21 | 2022-02-22 | Hewlett-Packard Development Company, L.P. | SERS sensor |
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| CN106756853A (en) * | 2017-03-03 | 2017-05-31 | 东南大学 | Tungsten oxide substrate with SERS function and preparation method thereof |
| CN111103278A (en) * | 2018-10-26 | 2020-05-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | SERS chip and manufacturing and regenerating method thereof |
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| CN110426384A (en) * | 2019-08-09 | 2019-11-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method for detecting specificity of 4- tert-butyl catechol in olefinic monomer |
| CN112156793A (en) * | 2020-10-19 | 2021-01-01 | 西安工程大学 | Silver nanowire-ReS2Functional composite material and preparation method thereof |
| CN112156793B (en) * | 2020-10-19 | 2023-03-24 | 西安工程大学 | Silver nanowire-ReS 2 Functional composite material and preparation method thereof |
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