CN109650392A - The preparation method of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle - Google Patents
The preparation method of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle Download PDFInfo
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- CN109650392A CN109650392A CN201910024212.6A CN201910024212A CN109650392A CN 109650392 A CN109650392 A CN 109650392A CN 201910024212 A CN201910024212 A CN 201910024212A CN 109650392 A CN109650392 A CN 109650392A
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- enhanced raman
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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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- 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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- C—CHEMISTRY; METALLURGY
- 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 kind of preparation methods of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, include the following steps: anhydrous titanium chloride and ethyl alcohol after mixing evenly, lithium powder is added, uniform solution will be again stirring for be put into stainless steel autoclave, it is reacted under high temperature, obtains the TiC nano material of high stable.The preparation method strong operability of the sensitive and stable TiC Surface enhanced Raman scattering nanoparticle of the present invention, easily promote, the material synthesized has high sensitivity, can be directly used for Surface enhanced Raman spectroscopy detection, obtained Surface enhanced Raman spectroscopy can be to fruits and vegetables epidermis Detecting Pesticide.
Description
Technical field
The present invention relates to inorganic advanced material technical fields, and in particular to a kind of sensitive and stable TiC surface enhanced drawing
The preparation method of graceful scattering nanoparticle.
Background technique
" bread is the staff of life ", with the improvement of living standards, people increasingly pay attention to food-safety problem, thus to food
Quality and safety more pay attention to, in this context reinforce food inspection technology research for food products market supervision have
It is significant.
Between past 40 years, Surface enhanced Raman spectroscopy (SERS) technology is as a kind of emerging spectral analysis technique,
It is widely used in the fields such as material science, chemistry, engineering science, bioscience and medicine.From the nineties in last century with
Come, in order to develop a kind of food additives detection method of rapid sensitive, SERS technology has been applied equally to toxic in food
The detection of chemistry and microbial contamination.It is extensive at present since SERS technology has many advantages, such as lossless, anhydrous interference in situ
It is applied to the detection of Pesticide Residues, illegal additive and transgenosis.With going deep into and nanometer skill in recent years for research
The rapid development of art, it has been found that having highly sensitive and high stability SERS substrate is that SERS technology realizes pesticide residue
The premise that success detects, therefore it is increasingly becoming another hot spot concerned by people.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of sensitive and stable TiC Surface enhanced Raman scattering nanoparticles
The preparation method of son.
A kind of preparation method of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, with anhydrous titanium chloride,
Lithium powder is predecessor, and ethyl alcohol is stay in place form, is synthesized under the high temperature conditions, is specifically comprised the following steps: anhydrous titanium chlorination
Object and ethyl alcohol after mixing evenly, are added lithium powder, will be again stirring for uniform solution and be put into stainless steel autoclave, under high temperature
Reaction, obtains the TiC nano material of high stable.
The preparation method of of the present invention sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, wherein institute
Stating anhydrous titanium chloride, the ethyl alcohol and the lithium powder mass ratio is 1:2:1~1:2:1.5.
The preparation method of of the present invention sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, wherein will
The solution is put into the stainless steel autoclave, is reacted 10-15 hours at 500-700 DEG C, is finally being cooled to room temperature,
Multiple centrifuge washing is simultaneously dried in vacuo at 50 DEG C.
The preparation method of of the present invention sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, wherein institute
It states anhydrous titanium chloride and the ethyl alcohol stirs 0.5 hour on magnetic stirring apparatus.
The preparation method of of the present invention sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, wherein add
Continue stirring 0.5 hour after entering the lithium powder.
The obtained TiC of the present invention meets nanostructure with the spheroidal pattern of class, spherical diameter be about 20nm (Fig. 1 with
Fig. 2).
The preparation method of the sensitive and stable TiC Surface enhanced Raman scattering nanoparticle of the present invention is unlike the prior art
Place is:
The preparation method strong operability of the sensitive and stable TiC Surface enhanced Raman scattering nanoparticle of the present invention, easily
It promotes, the material synthesized has high sensitivity, can be directly used for Surface enhanced Raman spectroscopy detection, and obtained surface enhanced is drawn
Graceful spectrum can be to fruits and vegetables epidermis Detecting Pesticide, to the detection limit point of rhodamine 6G (Fig. 3), malachite green, parathion-methyl
1.6ng/cm is not reached2、0.4ng/cm2、25ng/cm2。
With reference to the accompanying drawing to the preparation side of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle of the invention
Method is described further.
Detailed description of the invention
Fig. 1 is the electron scanning micrograph for the TiC nanoparticle that synthetic method of the invention obtains；
Fig. 2 is the transmission electron microscope photo for the TiC nanoparticle that synthetic method of the invention obtains；
10 obtained in the TiC quantum dot SERS substrate that Fig. 3 obtains for synthetic method of the invention-7M rhodamine 6G molecule
Signal.
Specific embodiment
Embodiment 1
The preparation method of a kind of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, includes the following steps:
The anhydrous titanium chloride of 0.758g and 1.516g ethyl alcohol stir 0.5 hour on magnetic stirring apparatus, add in the lithium powder for taking 0.758g
Enter in the solution, stir 0.5 hour, resulting solution is transferred in stainless steel autoclave, is warming up to 500 DEG C and is kept for 10 hours,
It is then cooled to room temperature, multiple centrifuge washing is simultaneously dried in vacuo.Obtained product is through XRD, laser particle analyzer, SEM, TEM and EDX
After characterization, there is highly stable TiC nanoparticle, spherical diameter is about 20nm.
Embodiment 2
A kind of preparation method of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, include the following steps: by
Anhydrous titanium chloride TiCl4It is stirred on magnetic stirring apparatus 0.5 hour with ethyl alcohol, after mixing evenly, lithium powder is added, continues
Stirring 0.5 hour, the solution stirred evenly is put into stainless steel autoclave, is reacted 10 hours at 600 DEG C, finally cold
But room temperature is arrived, multiple centrifuge washing is simultaneously dried in vacuo at 50 DEG C, obtains the TiC nano material of high stable.Wherein, TiCl4、
Ethyl alcohol and lithium powder mass ratio are 1:2:1.
Embodiment 3
The difference from example 2 is that: TiCl4, ethyl alcohol and lithium powder mass ratio be 1:2:1.5, in stainless steel autoclave,
It is reacted 15 hours at 700 DEG C.
Above embodiment be only preferred embodiments of the present invention will be described, not to the scope of the present invention into
Row limits, and without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements out should all be fallen into the protection scope that claims of the present invention determines.
Claims (5)
1. a kind of preparation method of sensitive and stable TiC Surface enhanced Raman scattering nanoparticle, it is characterised in that: including such as
Lower step: after mixing evenly by anhydrous titanium chloride and ethyl alcohol, being added lithium powder, will be again stirring for uniform solution be put into it is stainless
It in steel autoclave, is reacted under high temperature, obtains the TiC nano material of high stable.
2. the preparation method of according to claim 1 sensitive and stable TiC Surface enhanced Raman scattering nanoparticle,
Be characterized in that: the anhydrous titanium chloride, the ethyl alcohol and the lithium powder mass ratio are 1:2:1~1:2:1.5, described anhydrous
Titanium chloride is TiCl4。
3. the preparation method of according to claim 2 sensitive and stable TiC Surface enhanced Raman scattering nanoparticle,
It is characterized in that: the solution is put into the stainless steel autoclave, reacted 10-15 hours at 500-700 DEG C, finally cold
But room temperature is arrived, multiple centrifuge washing is simultaneously dried in vacuo at 50 DEG C.
4. the preparation method of according to claim 2 sensitive and stable TiC Surface enhanced Raman scattering nanoparticle,
Be characterized in that: the anhydrous titanium chloride and the ethyl alcohol stir 0.5 hour on magnetic stirring apparatus.
5. the preparation method of according to claim 2 sensitive and stable TiC Surface enhanced Raman scattering nanoparticle,
It is characterized in that: continuing stirring 0.5 hour after the lithium powder is added.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244818A (en) * | 1996-11-25 | 2000-02-16 | 有限会社环境设备研究所 | Photocatalyst having visible light activity and use thereof |
| US7108840B2 (en) * | 2003-02-19 | 2006-09-19 | Korea Institute Of Machinery & Materials | Method for manufacturing nanophase TiC-based 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 |
| CN103275327A (en) * | 2013-06-15 | 2013-09-04 | 厦门大学 | Method for preparing liquid anaerobic polytitanocarbosilane |
| CN108584939A (en) * | 2018-07-09 | 2018-09-28 | 黑龙江科技大学 | A kind of titanium carbide of high dielectric/graphene composite thin film material preparation method |
-
2019
- 2019-01-10 CN CN201910024212.6A patent/CN109650392B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244818A (en) * | 1996-11-25 | 2000-02-16 | 有限会社环境设备研究所 | Photocatalyst having visible light activity and use thereof |
| US7108840B2 (en) * | 2003-02-19 | 2006-09-19 | Korea Institute Of Machinery & Materials | Method for manufacturing nanophase TiC-based 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 |
| CN103275327A (en) * | 2013-06-15 | 2013-09-04 | 厦门大学 | Method for preparing liquid anaerobic polytitanocarbosilane |
| CN108584939A (en) * | 2018-07-09 | 2018-09-28 | 黑龙江科技大学 | A kind of titanium carbide of high dielectric/graphene composite thin film material preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 刘平安等: "超细碳化钛粉体的制备及应用研究进展", 《兵器材料科学与工程》 * |
| 崔富晖: "熔盐电化学脱氧制备碳化钛", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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