CN109650392B - Preparation method of sensitive and stable TiC surface enhanced Raman scattering nano particles - Google Patents
Preparation method of sensitive and stable TiC surface enhanced Raman scattering nano particles Download PDFInfo
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- CN109650392B CN109650392B CN201910024212.6A CN201910024212A CN109650392B CN 109650392 B CN109650392 B CN 109650392B CN 201910024212 A CN201910024212 A CN 201910024212A CN 109650392 B CN109650392 B CN 109650392B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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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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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- 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 preparation method of a sensitive and stable TiC surface enhanced Raman scattering nano particle, which comprises the following steps: and (3) uniformly stirring anhydrous titanium chloride and ethanol, adding lithium powder, putting the uniformly stirred solution into a stainless steel autoclave, and reacting at high temperature to obtain the high-stability TiC nano material. The preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particles has strong operability and easy popularization, the synthesized material has high sensitivity and can be directly used for surface enhanced Raman spectrum detection, and the obtained surface enhanced Raman spectrum can be used for detecting pesticide residues on the surface of fruits and vegetables.
Description
Technical Field
The invention relates to the technical field of inorganic advanced materials, in particular to a preparation method of a sensitive and stable TiC surface enhanced Raman scattering nano particle.
Background
People take food as the day, and along with the improvement of living standard, people attach more and more importance to the food safety problem, thereby attaching more importance to the quality and safety of food, and the research of strengthening the food detection technology under the background has important meaning for the supervision of the food market.
In the past 40 years, Surface Enhanced Raman Spectroscopy (SERS) has been widely used in the fields of material science, chemistry, engineering science, bioscience, medicine, and the like as a new spectral analysis technique. Since the last 90 s of the century, SERS technology has also been applied to the detection of toxic chemical and microbial contamination in food in order to develop a rapid and sensitive method for the detection of food additives. At present, the SERS technology has the advantages of in-situ no damage, no water interference and the like, and is widely applied to detection of pesticide residues, illegal additives and transgenosis in food. With the research and the rapid development of nanotechnology in recent years, it is found that the SERS substrate with high sensitivity and high stability is a prerequisite for the SERS technology to successfully detect pesticide residue, and thus, the SERS substrate becomes another hot point of attention.
Disclosure of Invention
The invention aims to provide a preparation method of a TiC surface enhanced Raman scattering nano particle, which is sensitive and stable.
A method for preparing sensitive and stable TiC surface enhanced Raman scattering nano particles takes anhydrous titanium chloride and lithium powder as precursors and ethanol as a structural template, and synthesizes the TiC surface enhanced Raman scattering nano particles under the high-temperature condition, which specifically comprises the following steps: and (3) uniformly stirring anhydrous titanium chloride and ethanol, adding lithium powder, putting the uniformly stirred solution into a stainless steel autoclave, and reacting at high temperature to obtain the high-stability TiC nano material.
The preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particle comprises the following steps of mixing anhydrous titanium chloride, ethanol and lithium powder according to a mass ratio of 1:2: 1-1: 2: 1.5.
The preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particle comprises the steps of placing the solution into a stainless steel autoclave, reacting for 10-15 hours at 500-700 ℃, cooling to room temperature, centrifuging and washing for multiple times, and drying in vacuum at 50 ℃.
The preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particle comprises the step of stirring the anhydrous titanium chloride and the ethanol on a magnetic stirrer for 0.5 hour.
The preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particle comprises the step of adding the lithium powder and then continuing stirring for 0.5 hour.
The TiC obtained by the invention conforms to a nano structure with a shape similar to a sphere, and the diameter of the sphere is about 20nm (figures 1 and 2).
Compared with the prior art, the preparation method of the sensitive and stable TiC surface enhanced Raman scattering nano particle is characterized in that:
the invention is sensitive and stable TiC surface enhancementThe preparation method of the Raman scattering nanoparticles has strong operability and easy popularization, the synthesized material has high sensitivity and can be directly used for surface enhanced Raman spectroscopy detection, the obtained surface enhanced Raman spectroscopy can be used for detecting pesticide residues on the surfaces of fruits and vegetables, and the detection limits of rhodamine 6G (figure 3), malachite green and methyl parathion respectively reach 1.6ng/cm2、0.4ng/cm2、25ng/cm2。
The preparation method of the sensitive and stable TiC surface enhanced raman scattering nanoparticles of the present invention is further described with reference to the accompanying drawings.
Drawings
FIG. 1 is a scanning electron microscope photograph of TiC nanoparticles obtained by the synthesis method of the present invention;
FIG. 2 is a TEM image of TiC nanoparticles obtained by the synthesis method of the present invention;
FIG. 3 shows 10 obtained on a TiC quantum dot SERS substrate obtained by the synthesis method of the present invention-7M rhodamine 6G molecular signal.
Detailed Description
Example 1
A preparation method of sensitive and stable TiC surface enhanced Raman scattering nano particles comprises the following steps: 0.758g of anhydrous titanium chloride and 1.516g of ethanol are stirred for 0.5 hour on a magnetic stirrer, 0.758g of lithium powder is added into the solution and stirred for 0.5 hour, the obtained solution is transferred into a stainless steel autoclave and heated to 500 ℃ for 10 hours, and then the solution is cooled to room temperature, centrifugally washed for a plurality of times and dried in vacuum. The obtained product has highly stable TiC nano particles with the spherical diameter of about 20nm after being characterized by XRD, laser particle size analyzer, SEM, TEM, EDX and the like.
Example 2
A preparation method of sensitive and stable TiC surface enhanced Raman scattering nano particles comprises the following steps: anhydrous titanium chloride TiCl4Stirring with ethanol in a magnetic stirrer for 0.5 hr, adding lithium powder, stirring for 0.5 hr, placing the uniformly stirred solution into a stainless steel autoclave, and reacting at 600 deg.C for 10 hr to obtain the final productThen cooling to room temperature, centrifuging and washing for many times, and drying in vacuum at 50 ℃ to obtain the high-stability TiC nano material. Wherein, TiCl4And the mass ratio of the ethanol to the lithium powder is 1:2:1.
Example 3
The difference from example 2 is that: TiCl (titanium dioxide)4Ethanol and lithium powder in a mass ratio of 1:2:1.5, and reacting at 700 ℃ for 15 hours in a stainless steel autoclave.
The above examples are only for describing the preferred embodiments of the present invention, and are not intended to 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 be made within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (3)
1. A preparation method of sensitive and stable TiC surface enhanced Raman scattering nano particles is characterized by comprising the following steps: the method comprises the following steps: uniformly stirring anhydrous titanium chloride and ethanol, adding lithium powder, putting the uniformly stirred solution into a stainless steel autoclave, and reacting at high temperature to obtain a high-stability TiC nano material;
wherein the mass ratio of the anhydrous titanium chloride to the ethanol to the lithium powder is 1:2: 1-1: 2:1.5, and the anhydrous titanium chloride is TiCl4(ii) a Putting the solution into the stainless steel autoclave, reacting at 500-700 ℃ for 10-15 hours, cooling to room temperature, centrifuging and washing for multiple times, and drying in vacuum at 50 ℃.
2. The method of claim 1, wherein the TiC nanoparticle is characterized in that: the anhydrous titanium chloride and the ethanol were stirred on a magnetic stirrer for 0.5 hour.
3. The method of claim 1, wherein the TiC nanoparticle is characterized in that: the lithium powder was added and stirring was continued for 0.5 hour.
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| US6306343B1 (en) * | 1996-11-25 | 2001-10-23 | Ecodevice Laboratory Co., Ltd | Photocatalyst having visible light activity and uses thereof |
| KR20040074828A (en) * | 2003-02-19 | 2004-08-26 | 한국기계연구원 | Method for manufacturing nanophase tic composite powders by metallothermic reduction |
| WO2011119227A2 (en) * | 2010-03-25 | 2011-09-29 | Columbia Northwest Pharmaceuticals, Llc | Compositions for the treatment of central nervous system disorders including depression employing novel drug combination therapy to reduce suicidality in patients |
| CN103275327B (en) * | 2013-06-15 | 2015-05-13 | 厦门大学 | Method for preparing liquid anaerobic polytitanocarbosilane |
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