CN110104679B - Ti with SERS effect2O3Synthesis method and application of nanosheet self-assembled microspheres - Google Patents
Ti with SERS effect2O3Synthesis method and application of nanosheet self-assembled microspheres Download PDFInfo
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- CN110104679B CN110104679B CN201910445035.9A CN201910445035A CN110104679B CN 110104679 B CN110104679 B CN 110104679B CN 201910445035 A CN201910445035 A CN 201910445035A CN 110104679 B CN110104679 B CN 110104679B
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Abstract
The invention discloses Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembly microsphere comprises the following steps: s1: dispersing a titanium source in an organic solvent, placing the organic solvent in a reaction kettle for heating reaction, and separating a solid product from a system after the reaction; s2: and heating the solid product obtained in the step S1 under the protection of gas. The synthesis method adopts the solvothermal reaction to prepare the nano particles, has the characteristics of simple operation, high repeatability, no pollution and the like, and is easy to popularize and produce. Ti obtained by the synthesis method of the invention2O3The nano-scale composite material accords with the characteristics of a nano structure and has the appearance of a nano-sheet self-assembled microsphere. Ti of the nano-sheet self-assembled microsphere2O3The nanometer material can be directly used as a surface enhanced Raman substrate to realize the surface enhanced Raman effect, and the enhancement factor can reach 106。
Description
Technical Field
The invention belongs to the field of detection, and particularly relates to a synthesis method and application of a titanium oxide material for surface enhanced Raman spectroscopy.
Background
The surface enhanced raman spectroscopy is a very sensitive detection technology and is widely applied to the fields of chemical detection, biological imaging, disease diagnosis and the like, but the traditional surface enhanced raman spectroscopy technology adopts precious metal gold and silver nanostructure materials as a signal enhancement substrate, so that the price is high, the stability is not high, and the popularization of the Surface Enhanced Raman Scattering (SERS) technology is not facilitated. The semiconductor is used as a substrate of the surface enhanced Raman scattering, so that the Raman molecular signals can be greatly enhanced, and the semiconductor has the advantages of high stability, strong heat resistance, low price and the like, and is favorable for large-scale popularization of the surface enhanced Raman substrate.
Unlike conventional wide band gap semiconductors, metallic semiconductors have some conductivity due to a certain amount of free electrons. When the frequency of the incident light is the same as the vibration frequency of the free electrons of the metallic semiconductor, a localized surface plasmon resonance phenomenon is generated on the surface of the metallic semiconductor, and the incident light is greatly absorbed. The localized surface plasmon resonance generates a very strong electric field at the semiconductor surface, and the raman active molecular signal at the semiconductor surface is enhanced because the surface enhanced raman signal is proportional to the square of the electric field strength. The metallic semiconductor material with rough surface and oxygen-deficient nanometer size not only has large specific surface area, but also can generate stronger local surface plasma resonance effect, and has great advantages in the surface enhanced Raman scattering substrate.
Metallic Ti2O3The nano-composite material has high concentration of free electrons and high room temperature conductivity, and can generate a strong surface plasma resonance effect under the irradiation of visible light, thereby generating an excellent Raman scattering signal enhancement effect. But for a long time Ti with specific ultra-thin two-dimensional nanostructures2O3It has not been reported.
Disclosure of Invention
The technical problem to be solved by the invention is to provide Ti with SERS effect, which has the characteristics of simple operation, high repeatability, no pollution and the like, and is easy to popularize and produce2O3A synthesis method of nano-sheet self-assembly microspheres.
The invention also aims to provide the material obtained by the synthesis method.
It is still another object of the present invention to provide the Ti2O3The application of the nano-sheet self-assembly microsphere is provided.
Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembled microsphere comprises the steps ofThe following steps:
s1: dispersing a titanium source in an organic solvent, placing the organic solvent in a reaction kettle for heating reaction, and separating a solid product from a system after the reaction;
s2: and heating the solid product obtained in the step S1 under the protection of gas.
The Ti with SERS effect provided by the invention2O3The synthesis method of the nano-sheet self-assembly microsphere comprises the following steps of (1) synthesizing nano-sheet self-assembly microspheres, wherein the titanium source is acetylacetone titanium and/or diisopropyl titanate; the organic solvent is one or more of ethanol, glycol, propanol, butanol and methanol.
The Ti with SERS effect provided by the invention2O3The synthesis method of the nanosheet self-assembled microsphere comprises the step of synthesizing the nanosheet self-assembled microsphere, wherein the mass ratio of the titanium source to the organic solvent is 1 (100-200).
The Ti with SERS effect provided by the invention2O3The synthesis method of the nanosheet self-assembled microspheres comprises the following steps of: (10-15) a mixed solvent of methanol and propanol.
The Ti with SERS effect provided by the invention2O3The synthesis method of the nanosheet self-assembled microspheres comprises the steps of heating to 180-240 ℃ in the reaction kettle, keeping for 12-20 hours, and naturally cooling to room temperature.
The Ti with SERS effect provided by the invention2O3The synthesis method of the nanosheet self-assembled microspheres comprises the step S2 of heating in a tube furnace at the temperature of 400-500 ℃ for 5-9 hours, and then naturally cooling to room temperature.
The Ti with SERS effect provided by the invention2O3Ti prepared by synthesis method of nanosheet self-assembled microspheres2O3The nano-sheet self-assembly microsphere.
Ti of the invention2O3The nano-sheet self-assembly microsphere is applied to high-sensitivity surface-enhanced Raman spectrum detection.
The invention relates to a surface enhanced Raman spectroscopy detection method, which is used for detecting Ti2O3Nanosheet self-assemblyThe microsphere is used as a substrate, probe molecules are uniformly adsorbed on the surface of the substrate material, and surface enhanced Raman spectroscopy testing is carried out under the action of a detection excitation light source.
The surface-enhanced Raman spectroscopy detection method provided by the invention is characterized in that the number of the probe molecules is 10-7The rhodamine 6G solution of M uses 532nm laser as a light source, and the laser power is 1 percent.
Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembly microsphere is different from the prior art in that:
the synthesis method adopts the solvothermal reaction to prepare the nano particles, has the characteristics of simple operation, high repeatability, no pollution and the like, and is easy to popularize and produce.
Ti obtained by the synthesis method of the invention2O3The nano-scale composite material accords with the characteristics of a nano structure and has the appearance of a nano-sheet self-assembled microsphere. Ti of the nano-sheet self-assembled microsphere2O3The nanometer material can be directly used as a surface enhanced Raman substrate to realize the surface enhanced Raman effect, and the enhancement factor can reach 106。
The Ti with SERS effect of the invention is shown in the following by combining the attached drawings2O3The synthesis method and application of the nano-sheet self-assembly microsphere are further described.
Drawings
FIG. 1 shows Ti obtained by the synthesis method of the present invention2O3Scanning electron microscope photo of the nano-sheet self-assembly microsphere;
FIG. 2 shows Ti obtained by the synthesis method of the present invention2O310 obtained on nanosheet SERS substrate-7M rhodamine 6G molecular signal.
Detailed Description
Example 1:
ti2O3A nanosheet self-assembled microsphere prepared by the steps of:
0.5g of titanium acetylacetonate was added to a mixed solution of 60mL of anhydrous propanol and 15mL of anhydrous methanol, and stirred for 1 hour on a magnetic stirrer, followed by transferring to a reaction vessel and heating to 220 ℃ for 12 hours.
And centrifugally collecting the precipitate obtained by the reaction, placing the precipitate in a tubular furnace, heating the precipitate to 450 ℃ in a hydrogen atmosphere, keeping the temperature for 6 hours, and naturally cooling the precipitate to room temperature.
The obtained product is characterized by XRD, SEM, TEM, EDS and the like, and is determined to be Ti with nano-sheet self-assembled microspheres2O3And (3) nano materials. Referring to FIG. 1, the microspheres have a diameter of about 8 microns and the surface of the microspheres is made of ultra-thin Ti2O3The nano-sheet is composed of nano-sheets, and the thickness of the nano-sheets is about 3-8 nanometers.
Example 2
0.4g of titanium acetylacetonate is added to 75mL of butanol, stirred for 1 hour on a magnetic stirrer, then transferred to a reaction kettle, heated to 180 ℃ and maintained for 20 hours, then naturally cooled to room temperature, the supernatant in the reaction kettle is poured off, the precipitate is centrifuged at 10000r/min, and the precipitate is washed with water and ethanol for three times.
And centrifugally collecting the precipitate obtained by the reaction, placing the precipitate in a tubular furnace, heating the precipitate to 500 ℃ in a hydrogen atmosphere, keeping the temperature for 5 hours, and naturally cooling the precipitate to room temperature.
The obtained product is determined to be Ti with nano-sheet self-assembled microspheres after SEM characterization2O3And (3) nano materials.
Example 3
Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembly microsphere comprises the following steps:
mixing diisopropyl titanate and ethanol with the mass ratio of 1:100, placing the mixture in a reaction kettle for heating reaction, heating the mixture to 240 ℃ for 12 hours, naturally cooling the mixture to room temperature, and separating a solid product from a system after the reaction;
the obtained solid product was heated in a tube furnace under gas protection at 400 ℃ for 9 hours, and then naturally cooled to room temperature.
The obtained product is determined to be Ti with nano-sheet self-assembled microspheres after SEM characterization2O3And (3) nano materials.
Example 4
Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembly microsphere comprises the following steps:
mixing diisopropyl titanate and ethylene glycol in a mass ratio of 1:200, placing the mixture in a reaction kettle, heating the mixture for reaction, heating the mixture to 210 ℃, keeping the temperature for 16 hours, naturally cooling the mixture to room temperature, and separating a solid product from a system after the reaction;
the obtained solid product is heated in a tube furnace under the protection of gas, the heating temperature is 420 ℃, the solid product is kept for 8 hours, and then the solid product is naturally cooled to the room temperature.
The obtained product is determined to be Ti with nano-sheet self-assembled microspheres after SEM characterization2O3And (3) nano materials.
Application examples
Ti prepared in example 12O3The nano-sheet self-assembly microspheres are suspended in an ethanol solution, a drop of the nano-sheet self-assembly microspheres is absorbed and dropped on a carrying fragment, and a round spot is formed after drying. Will 10-7Dripping the rhodamine 6G solution of M on the circular spots of the glass slide, and drying. The glass slide is placed on a confocal laser Raman spectrometer, 532nm laser is used as a light source, and the surface enhanced Raman spectroscopy test is carried out under the condition that the laser power is 1%. The results are shown in FIG. 2.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (8)
1. Ti with SERS effect2O3The synthesis method of the nano-sheet self-assembly microsphere is characterized by comprising the following steps: the method comprises the following steps:
s1: dispersing a titanium source in an organic solvent, placing the organic solvent in a reaction kettle for heating reaction, and separating a solid product from a system after the reaction;
s2: heating the solid product obtained in the step S1 under the protection of gas;
the titanium source is acetylacetone titanium and/or diisopropyl titanate; the organic solvent is one or more of ethanol, glycol, propanol, butanol and methanol;
the mass ratio of the titanium source to the organic solvent is 1 (100-200).
2. Ti with SERS effect according to claim 12O3The synthesis method of the nano-sheet self-assembly microsphere is characterized by comprising the following steps: the organic solvent is prepared from the following components in a mass ratio of 3: (10-15) a mixed solvent of propanol and methanol.
3. Ti with SERS effect according to claim 22O3The synthesis method of the nano-sheet self-assembly microsphere is characterized by comprising the following steps: heating the mixture to 180-240 ℃ in the reaction kettle, keeping the mixture for 12-20 hours, and then naturally cooling the mixture to room temperature.
4. Ti with SERS effect according to claim 32O3The synthesis method of the nano-sheet self-assembly microsphere is characterized by comprising the following steps: and step S2, heating in a tube furnace at 400-500 deg.C for 5-9 hr, and naturally cooling to room temperature.
5. The Ti having SERS Effect of any one of claims 1 to 42O3Ti prepared by synthesis method of nanosheet self-assembled microspheres2O3The nano-sheet self-assembly microsphere.
6. Ti according to claim 52O3The nano-sheet self-assembly microsphere is applied to high-sensitivity surface-enhanced Raman spectrum detection.
7. A surface-enhanced Raman spectroscopy method for detecting a surface-enhanced Raman spectrum, comprising the step of using the Ti of claim 52O3The nano-sheet self-assembly microsphere is used as a substrate, probe molecules are uniformly adsorbed on the surface of the substrate material, and surface enhanced Raman spectroscopy test is carried out under the action of a detection excitation light source.
8. The method of claim 7, wherein: the probe molecule is 10-7The rhodamine 6G solution of M uses 532nm laser as a light source, and the laser power is 1 percent.
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Citations (4)
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| CN102491413A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for preparing titanium sesquioxide material |
| CN104591273A (en) * | 2014-12-31 | 2015-05-06 | 上海师范大学 | Preparation method of synthesizing Ti<3+>-doped titanium dioxide by using alcohol thermal method |
| CN107324384A (en) * | 2017-07-21 | 2017-11-07 | 中国科学院合肥物质科学研究院 | One kind utilizes isopropanol etherification reaction generation TiO2The alcohol process for thermosynthesizing of micron ball |
| CN108525651A (en) * | 2018-03-21 | 2018-09-14 | 广州大学 | A kind of reduction titanium dioxide process with highlight catalytic active |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491413A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Method for preparing titanium sesquioxide material |
| CN104591273A (en) * | 2014-12-31 | 2015-05-06 | 上海师范大学 | Preparation method of synthesizing Ti<3+>-doped titanium dioxide by using alcohol thermal method |
| CN107324384A (en) * | 2017-07-21 | 2017-11-07 | 中国科学院合肥物质科学研究院 | One kind utilizes isopropanol etherification reaction generation TiO2The alcohol process for thermosynthesizing of micron ball |
| CN108525651A (en) * | 2018-03-21 | 2018-09-14 | 广州大学 | A kind of reduction titanium dioxide process with highlight catalytic active |
Non-Patent Citations (2)
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| Black TiO2 Nanotubes: Cocatalyst-Free Open-Circuit Hydrogen Generation;Ning Liu等;《Nano Lett.》;20140505;3309-3313 * |
| Formation and stability of reduced TiOx layers on anatase TiO2(101): Identification of a novel Ti2O3 phase;Xunhua Zhao等;《PHYSICAL REVIEW MATERIALS》;20180110;015801-1至015801-5 * |
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