CN110104679A - Ti with SERS effect2O3The synthetic method and application of nanometer sheet self-assembly microspheres - Google Patents
Ti with SERS effect2O3The synthetic method and application of nanometer sheet self-assembly microspheres Download PDFInfo
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- CN110104679A CN110104679A CN201910445035.9A CN201910445035A CN110104679A CN 110104679 A CN110104679 A CN 110104679A CN 201910445035 A CN201910445035 A CN 201910445035A CN 110104679 A CN110104679 A CN 110104679A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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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
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of Ti with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, includes the following steps: S1: titanium source is scattered in organic solvent, is placed in reaction kettle and is heated reaction, isolates solid product from the system after reaction；S2: the solid product that step S1 is obtained is heated under the conditions of gas shield.Synthetic method of the invention prepares nano particle using solvent thermal reaction, has the features such as easy to operate, repeatability height, pollution-free, easy to spread and production.The obtained Ti of synthetic method of the invention2O3Meet nano structure, the pattern with nanometer sheet self-assembly microspheres.The Ti of the nanometer sheet self-assembly microspheres2O3Nano material can be directly used as surface enhanced Raman substrate, and the surface-enhanced Raman effects of realization, enhancement factor is up to 106。
Description
Technical field
The invention belongs to detection fields, and in particular to a kind of synthesis of the titania meterial for Surface enhanced Raman spectroscopy
Method and its application.
Background technique
Surface enhanced Raman spectroscopy is a kind of very sensitive detection technique, is examined in chemical detection, bio-imaging and disease
It is disconnected that fields is waited to be widely used, but traditional Surface enhanced Raman spectroscopy technology is all made of noble metal gold and silver nanostructured material
Material is used as signal enhancing substrate, not only expensive, but also stability is not high, is unfavorable for Surface enhanced Raman scattering (SERS) skill
The popularization of art.It, not only can be with strong enhancement of Raman molecular signal, also using semiconductor as the substrate of Surface enhanced Raman scattering
With stability height, heat resistance is strong, more cheap etc. a variety of advantages of price, is conducive to pushing away on a large scale for surface enhanced Raman substrate
Extensively.
Different with traditional wide band gap semiconducter, metallicity semiconductor is due to a certain amount of free electron, so tool
There is certain electric conductivity.It, can be on its surface when incident light frequency is identical as the vibration frequency of metallicity semiconductor free electron
Local surface plasma resonance phenomenon is generated, and maximum absorption is generated to incident light.Local surface plasma resonance can be half
Conductive surface generates extremely strong electric field, square directly proportional due to surface-enhanced Raman signals and electric field strength, so being in half
The raman active molecule signal of conductive surface can be enhanced.And shaggy, the metallicity half of oxygen defect type nano-scale
Conductor material not only has very big specific surface area, moreover it is possible to stronger local surface plasma resonance effect is generated, on surface
Occupy great advantage in enhancing Raman scattering substrate.
The Ti of metallicity2O3Free electron with higher concentration, conductivity at room temperature rate is higher, can under the irradiation of visible light
To generate stronger surface plasmon resonance effect, and then it can produce excellent Raman scattering signal enhancement effect.But it is long
Since phase, the Ti with specific ultra-thin two-dimension nanostructure2O3It has not been reported.
Summary of the invention
The features such as the technical problem to be solved in the present invention is to provide a kind of easy to operate, repeatability is high, pollution-free, is easy to
The Ti with SERS effect for promoting and producing2O3The synthetic method of nanometer sheet self-assembly microspheres.
The material obtained it is another object of the present invention to propose the synthetic method.
A further object of the present invention is to propose the Ti2O3The application of nanometer sheet self-assembly microspheres.
A kind of Ti with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, includes the following steps:
S1: titanium source is scattered in organic solvent, is placed in reaction kettle and is heated reaction, is isolated from the system after reaction solid
Body product；
S2: the solid product that step S1 is obtained is heated under the conditions of gas shield.
Ti of the present invention with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, wherein the titanium
Source is titanium acetylacetone and/or metatitanic acid diisopropyl ester；The organic solvent is in ethyl alcohol, ethylene glycol, propyl alcohol, butanol and methanol
It is one or more.
Ti of the present invention with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, wherein the titanium
The mass ratio of source and the organic solvent is 1:(100~200).
Ti of the present invention with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, wherein described to have
Solvent is that mass ratio is 3:(10~15) methanol and propyl alcohol mixed solvent.
Ti of the present invention with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, wherein described
It is heated to 180~240 DEG C in reaction kettle to be kept for 12~20 hours, subsequent cooled to room temperature.
Ti of the present invention with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, wherein step S2
It is to be heated in tube furnace, heating temperature is 400~500 DEG C, is kept for 5~9 hours, subsequent cooled to room temperature.
Ti of the present invention with SERS effect2O3What the synthetic method of nanometer sheet self-assembly microspheres was prepared
Ti2O3Nanometer sheet self-assembly microspheres.
Ti of the present invention2O3Application of the nanometer sheet self-assembly microspheres in the detection of highly sensitive Surface enhanced Raman spectroscopy.
A kind of Raman spectrum method for detecting surface reinforcement, with Ti of the present invention2O3Nanometer sheet self-assembly microspheres are as base
Bottom carries out surface-enhanced Raman light under detection excitation light source effect by probe molecule uniform adsorption on substrate material surface
Spectrum test.
Raman spectrum method for detecting surface reinforcement of the present invention, wherein the probe molecule is 10-7The rhodamine of M
6G solution uses 532nm laser as light source, laser power 1%.
The present invention has the Ti of SERS effect2O3The synthetic method difference from prior art of nanometer sheet self-assembly microspheres
It is:
Synthetic method of the invention prepares nano particle using solvent thermal reaction, has easy to operate, repeatability height, nothing
The features such as pollution, easy to spread and production.
The obtained Ti of synthetic method of the invention2O3Meet nano structure, the pattern with nanometer sheet self-assembly microspheres.
The Ti of the nanometer sheet self-assembly microspheres2O3Nano material, can be directly used as surface enhanced Raman substrate, and the surface enhanced of realization is drawn
Graceful effect, enhancement factor is up to 106。
With reference to the accompanying drawing to the Ti with SERS effect of the invention2O3The synthetic method of nanometer sheet self-assembly microspheres and
Using being described further.
Detailed description of the invention
Fig. 1 is the Ti that synthetic method of the invention obtains2O3The electron scanning micrograph of nanometer sheet self-assembly microspheres；
Fig. 2 is the Ti obtained with synthetic method of the invention2O310 obtained in nanometer sheet SERS substrate-7M rhodamine 6G
Molecular signal.
Specific embodiment
Embodiment 1:
A kind of Ti2O3Nanometer sheet self-assembly microspheres are prepared by following steps:
0.5g titanium acetylacetone is added in the mixed solution of 60mL anhydrous propyl alcohol and 15mL anhydrous methanol, in magnetic agitation
It stirs 1 hour, is then continued in reaction kettle on device, be warming up to 220 DEG C and maintain 12 hours.
Reaction gained precipitating is collected by centrifugation, is placed in tube furnace, 450 DEG C are heated under hydrogen atmosphere and is kept for 6 hours, from
So it is cooled to room temperature.
Products obtained therefrom is determined as the Ti with nanometer sheet self-assembly microspheres after the characterization such as XRD, SEM, TEM and EDS2O3It receives
Rice material.Referring to Fig. 1, the diameter of microballoon is about 8 microns, and microsphere surface is by ultra-thin Ti2O3Nanometer sheet is constituted, nanometer sheet thickness
About 3-8 nanometers.
Embodiment 2
0.4g titanium acetylacetone is added in 75mL butanol, is stirred 1 hour on magnetic stirring apparatus, is then continued at reaction kettle
In, it is warming up to 180 DEG C and maintains 20 hours, subsequent cooled to room temperature outwells the supernatant in reaction kettle, precipitating warp
10000r/min centrifugation, is cleaned three times with water and ethyl alcohol.
Reaction gained precipitating is collected by centrifugation, is placed in tube furnace, 500 DEG C are heated under hydrogen atmosphere and is kept for 5 hours, from
So it is cooled to room temperature.
Products obtained therefrom is determined as the Ti with nanometer sheet self-assembly microspheres after SEM is characterized2O3Nano material.
Embodiment 3
A kind of Ti with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, includes the following steps:
It is that 1:100 metatitanic acid diisopropyl ester and ethyl alcohol mix by mass ratio, is placed in reaction kettle and heats reaction, be heated to 240
DEG C keep 12 hours, subsequent cooled to room temperature isolates solid product from the system after reaction；
Obtained solid product is heated under the conditions of gas shield in tube furnace, heating temperature is 400 DEG C, and holding 9 is small
When, subsequent cooled to room temperature.
Products obtained therefrom is determined as the Ti with nanometer sheet self-assembly microspheres after SEM is characterized2O3Nano material.
Embodiment 4
A kind of Ti with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, includes the following steps:
It is that 1:200 metatitanic acid diisopropyl ester and ethylene glycol mix by mass ratio, is placed in reaction kettle and heats reaction, be heated to
210 DEG C are kept for 16 hours, and subsequent cooled to room temperature isolates solid product from the system after reaction；
Obtained solid product is heated under the conditions of gas shield in tube furnace, heating temperature is 420 DEG C, and holding 8 is small
When, subsequent cooled to room temperature.
Products obtained therefrom is determined as the Ti with nanometer sheet self-assembly microspheres after SEM is characterized2O3Nano material.
Application Example
Ti made from embodiment 12O3Nanometer sheet self-assembly microspheres are suspended in ethanol solution, are drawn one after another drop of in load fragment
On, a round spot is formed after drying.By 10-7The rhodamine 6G solution of M drips in the round spot of glass slide, drying.Glass slide is put
On confocal laser Raman spectrometer, uses 532nm laser as light source, carry out table under conditions of laser power is 1%
Face enhances Raman spectrum test.As a result referring to fig. 2.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (10)
1. a kind of Ti with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, it is characterised in that: including walking as follows
It is rapid:
S1: titanium source is scattered in organic solvent, is placed in reaction kettle and is heated reaction, and solid production is isolated from the system after reaction
Object；
S2: the solid product that step S1 is obtained is heated under the conditions of gas shield.
2. the Ti according to claim 1 with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, feature
Be: the titanium source is titanium acetylacetone and/or metatitanic acid diisopropyl ester；The organic solvent is ethyl alcohol, ethylene glycol, propyl alcohol, fourth
One of pure and mild methanol is a variety of.
3. the Ti according to claim 2 with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, feature
Be: the mass ratio of the titanium source and the organic solvent is 1:(100~200).
4. the Ti according to claim 3 with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, feature
Be: the organic solvent is that mass ratio is 3:(10~15) propyl alcohol and methanol mixed solvent.
5. the Ti according to claim 4 with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, feature
It is: is heated to 180~240 DEG C in the reaction kettle and is kept for 12~20 hours, subsequent cooled to room temperature.
6. the Ti according to claim 5 with SERS effect2O3The synthetic method of nanometer sheet self-assembly microspheres, feature
Be: step S2 is heated in tube furnace, and heating temperature is 400~500 DEG C, is kept for 5~9 hours, is then naturally cooled to
Room temperature.
7. with the Ti of SERS effect described in any one of claim 1~62O3The synthesis side of nanometer sheet self-assembly microspheres
The Ti that method is prepared2O3Nanometer sheet self-assembly microspheres.
8. Ti as claimed in claim 72O3Nanometer sheet self-assembly microspheres answering in the detection of highly sensitive Surface enhanced Raman spectroscopy
With.
9. a kind of Raman spectrum method for detecting surface reinforcement, which is characterized in that with Ti as claimed in claim 72O3Nanometer sheet is from group
Microballoon is filled as substrate, by probe molecule uniform adsorption on substrate material surface, carries out table under detection excitation light source effect
Face enhances Raman spectrum test.
10. Raman spectrum method for detecting surface reinforcement according to claim 9, it is characterised in that: the probe molecule is
10-7The rhodamine 6G solution of M uses 532nm laser as light source, laser power 1%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113484302A (en) * | 2021-07-01 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | SnS with capillary effect2Microsphere SERS substrate and preparation method and application thereof |
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2019
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113484302A (en) * | 2021-07-01 | 2021-10-08 | 中国科学院上海硅酸盐研究所 | SnS with capillary effect2Microsphere SERS substrate and preparation method and application thereof |
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