CN101077526A - Adjustable plasma wave gold nano bar preparation method - Google Patents
Adjustable plasma wave gold nano bar preparation method Download PDFInfo
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- CN101077526A CN101077526A CNA2007100352513A CN200710035251A CN101077526A CN 101077526 A CN101077526 A CN 101077526A CN A2007100352513 A CNA2007100352513 A CN A2007100352513A CN 200710035251 A CN200710035251 A CN 200710035251A CN 101077526 A CN101077526 A CN 101077526A
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Abstract
The process of preparing plasma wave adjustable nanometer gold rod is process of preparing nanometer gold rod with selective red shift. The process is one heating process with sodium thiosulfate or soluble sulfide added to obtain cutworm-shaped nanometer gold rod in obviously raised diameter and slightly increase length. The nanometer gold rod has increased plasma wave, and the process is simple and repeatable.
Description
Technical field
The present invention relates to the preparation method of the novel gold nanorods of a kind of similar caterpillar, particularly a kind of method of adjustable gold nanorods plasma wave is more specifically said so and is made the plasma resonance ripple generation red shift of gold nanorods with the method that adds related reagent.
Background technology
The about diameter of gold nanorods is approximately 10-20nm, length is the solid gold cylinder of 40-200nm.Being moulded material bar-shaped is the very important point, because clavate has determined the energy size of the light of electron excitation.So, can excite the light of different wave length by the nanometer rods of different length.Can characterize the plasma resonance absorption curve of gold nanorods with UV-Vis spectrum, traditional gold nanorods generally has an absworption peak at 520nm and another bigger wavelength place, corresponds respectively to the horizontal plasma wave and the longitudinal plasma wave of gold nanorods.Gold nanorods excites caused horizontal plasma wavelength (TPW) not obvious with the variation of transverse width along the transverse width direction, and nanometer rods longitudinal length direction excites the longitudinal plasma wave long (LPW) that causes, but change along with the variation of nanometer rods aspect ratio very sensitively, promptly the longitudinal plasma wave that the nanometer rods of different aspect ratios is corresponding different is long.
Scientific research shows that the plasma resonant vibration of nanometer rods can strengthen two-photon luminous (TPL) signal.The longitudinal mode of gold nanorods is at visible and near infrared wavelength region generation resonance, for bio-imaging, this frequency is desirable, because in this scope, the absorption of water and biomolecule is very low, and laser lighting gold nanorods technology is brought the hypersensitive medical imaging technology into a unprecedented sensitive level.Experiment shows that this technology is injected into blood vessel with small golden rod, sees through skin and illuminates them with laser, and the gold nanorods of taking in the intravital mouse blood vessel sends red light.The image that utilizes the method to generate is much brighter than the conventional fluorescent dye method.
At present develop the multiple method for preparing gold nanorods, comprised electrochemical method, photochemistry synthetic method and gold nano seed reduction preparation method.Especially in gold nano seed reducing process, introduce silver nitrate, can roughly control nanometer rods aspect ratio (aspect ratio of gold nanorods be meant the rod longitudinal length and the ratio of transverse width).But in the above-mentioned several method, than being easier to prepare less than the gold nanorods of 850 nanometers and having favorable reproducibility.But the preparation longitudinal plasma wave is during greater than the gold nanorods of 850 nanometers, and general reappearance is relatively poor, wants accurately to obtain longitudinal plasma wave greater than the unusual difficulty of the nanometer rods of 850 nanometers.In addition, the horizontal plasma wave of traditional gold nanorods of preparation is not also prepared the adjustable gold nanorods of a kind of horizontal plasma wave about 520nm at present.
Summary of the invention
Purpose of the present invention aims to provide a kind of novel gold nanorods, but the vertical wavelength of this gold nanorods plasma wave of accuracy controlling also, obtain accurate plasma resonance wavelength, and preparation process is simple and convenient, easy operating, prospect has a very wide range of applications at aspects such as magnetic, heat, light, electricity, catalysis, medical treatment, bio-sensings.
Method of the present invention is on gold nanorods (initial gold nanorods) basis by existing document preparation, by related reagent and technical finesse, obtains required novel gold nanorods at traditional gold nanorods dispersion.
The objective of the invention is to realize by following manner:
In the gold nanorods dispersion of need regulation and control plasma resonance wavelength, add sodium thiosulfate or dissolvable sulfide, regulating and controlling temperature obtains required plasma resonance wavelength with visible near-infrared real-time monitoring.
Described sulfide comprises vulcanized sodium, potassium sulfide, ammonium sulfide.
By controlling the formation speed that temperature can be regulated novel gold nanorods.At the gold nanorods that adds sodium thiosulfate or dissolvable sulfide, at room temperature can be than stable existence, but the rising of dispersion temperature can cause the plasma wave red shift of nanometer rods, the surface forms one deck loft layer simultaneously, pattern is similar to the novel gold nanorods of caterpillar, and temperature High variation speed more is fast more.Described regulating and controlling temperature, obtaining required plasma resonance wavelength with visible near-infrared real-time monitoring is: the gold nanorods dispersion is heated, with the real-time vertical absorbing wavelength of monitoring of visible near-infrared absorption, put into ice-water bath cooling a moment, centrifugation immediately then when arriving required wavelength.The temperature of heating can be: 25-100 ℃.
Described dispersion is an aqueous surfactant solution, mainly comprises cetyltrimethyl ammonium cationoid surfactant, as softex kw, hexadecyldimethyl benzyl ammonium phenyl ammonium bromide, the cetyltriethylammonium bromide aqueous solution.
But change between the concentration 0.001-0.1mol/L behind sodium thiosulfate of the present invention or the dissolvable sulfide adding gold nanorods solution in solution.
Described aqueous surfactant solution concentration gets final product between 0.01～0.2mol/L scope.
The present invention is on the basis of the gold nanorods that has prepared, and the plasma wave wavelength of this nanometer rods after by chemical treatment regulated.
Method one: heating gold nanorods and sodium thiosulfate mixed system, with visible near-infrared enforcement monitoring, vertical absorbing wavelength red shift of its correspondence then stops heating during to required wavelength, and place it in ice-water bath cooling, centrifugation immediately then obtains the gold nanorods of required similar caterpillar profile.
Method two: in the gold nanorods dispersion, add dissolvable sulfide, with this mixed system heating, with visible near-infrared enforcement monitoring, vertical absorbing wavelength red shift of its correspondence places it in the ice-water bath cooling during to required wavelength immediately, centrifugation then obtains the gold nanorods of required similar caterpillar profile.
Can obtain the novel gold nanorods of various accurate plasma waves---the gold nanorods of similar caterpillar profile by above method.
The present invention adopts and to add that sodium thiosulfate and methods of heating treatment make the significant chap of traditional gold nanorods and length slightly increases, thereby obtains the novel gold nanorods of a kind of similar caterpillar; Or add dissolvable sulfide and the traditional gold nanorods of heat treated and obtain that rod is long to be strengthened slightly, and the remarkable gold nanorods of chap.Handle by two kinds of methods in this invention, can acquire a kind of novel gold nanorods of similar caterpillar profile, the plasma wave of gold nanorods can increase arbitrarily, and simple to operate, the favorable reproducibility of this invention is easy to penetration and promotion.
The novel nano rod of preparation is compared with former nanometer rods, and photoluminescent property remains unchanged.Along with the variation of the loft layer thickness of novel nano rod, certain variation takes place in resonant light scattering character, develops into single resonant light scattering peak gradually by typical double resonance light scattering peak.
Owing to the invention provides the preparation method of the gold nanorods that a kind of horizontal and vertical plasma wave that makes gold nanorods can both regulate, resulting gold nanorods shows the longitudinal length direction and excites the longitudinal plasma wave long (LPW) that causes, no longer the variation along with the nanometer rods aspect ratio has linear relationship, it is different from the peculiar property of traditional gold nanorods, at aspects such as light, electricity, catalysis, medical treatment, bio-sensings very tempting application prospect is arranged.
Description of drawings
Fig. 1 is the transmission electron microscope picture of traditional gold nanorods.
Fig. 2 is the visible near-infrared absorption spectrum of traditional gold nanorods.
Fig. 3 is the novel gold nanorods transmission electron microscope picture of sodium thiosulfate after handling.
Fig. 4 is the visible near-infrared absorption spectrum of the novel gold nanorods of sodium thiosulfate after handling.
Fig. 5 is the transmission electron microscope picture of the novel gold nanorods of vulcanized sodium after handling.
Fig. 6 is the transmission electron microscope picture of another kind of traditional gold nanorods.
Fig. 7 is the transmission electron microscope picture of the novel gold nanorods of ammonium sulfide after handling.
The transmission electron microscope picture of Fig. 8 novel gold nanorods that to be the 1mol/L sodium thiosulfate that adds 0.02ml obtain to the 3ml nanometer rods.
Fig. 9 is the graph of a relation that adds temperature and LPW red shift speed behind the sodium thiosulfate in the gold nanorods.
The specific embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Get a gold nanorods 3ml by the preparation of gold nano seed reducing process, gold nanorods is long to be 55nm, width is 17nm (Fig. 1), vertical plasma resonance wavelength of its correspondence is at 784nm (Fig. 2), gold nanorods is dispersed in the 0.1mol/L softex kw solution, add 0.2ml hypo solution (0.1mol/L), and heat constant at 50 ℃, implement monitoring with near-infrared absorption spectrum, putting into frozen water after 10 minutes cools off, centrifugation then, acquisition length is 60nm, the novel gold nanorods (Fig. 3) of the similar caterpillar of width 30nm, the gold nanorods that vertical plasma resonance absorbing wavelength of its correspondence is 865nm (Fig. 4).
Embodiment 2
Get a gold nanorods 3ml by the preparation of gold nano seed reducing process, gold nanorods is long to be 55nm, width is 17nm (Fig. 1), vertical plasma resonance wavelength of its correspondence is at 784nm (Fig. 2), gold nanorods is dispersed in the 0.1mol/L vulcanized sodium that 0.1mol/L hexadecyldimethyl benzyl ammonium phenyl bromination ammonium salt solution adds 0.2ml, heating is also constant in 50 ℃, implement monitoring with near-infrared absorption spectrum, putting into frozen water after 10 minutes cools off, obtaining length then is 60nm, width 30nm nanometer rods (Fig. 5), vertical absorbing wavelength of its correspondence is the gold nanorods of 651nm.
Embodiment 3
Get a gold nanorods 3mL by the preparation of gold nano seed reducing process, gold nanorods is long to be that 40nm, width are 12nm (Fig. 6), vertical plasma resonance wavelength of its correspondence is at 732nm, gold nanorods is dispersed in the 0.1mol/L softex kw solution, the gold nanorods dispersion adds the 0.1mol/L ammonium sulfide of 0.2mL, heating is also constant in 50 ℃, putting into frozen water after 10 minutes cools off, centrifugation then, acquisition length is 50nm, width 24nm nanometer rods (Fig. 7), vertical absorbing wavelength of its correspondence is the gold nanorods of 721nm.
Embodiment 4
Get a gold nanorods 3ml by the preparation of gold nano seed reducing process, gold nanorods is long to be that 55nm, width are 17nm (Fig. 1), gold nanorods is dispersed in the 1mol/L sodium thiosulfate that 0.1mol/L softex kw solution adds 0.02ml, heating is also constant in 50 ℃, implement monitoring with near-infrared absorption spectrum, put into frozen water after 20 minutes and cool off, gained novel nano rod is seen (Fig. 8).
Get a gold nanorods 3ml by the preparation of gold nano seed reducing process, gold nanorods is long to be that 55nm, width are 17nm (Fig. 1), gold nanorods is dispersed in 0.1mol/L softex kw solution, the 0.5mol/L hypo solution that adds 0.02ml again, heating is also constant in 25 ℃, with per 5 minutes red shift speed of the LPW of near-infrared absorption spectrum monitoring gold nanorods and time relation, use the same method, measure 30,50,70,80,90,100 ℃ of red shift speed and time relation, the relation of temperature and red shift speed is seen Fig. 9.
Claims (5)
1, a kind of preparation method of gold nanorods of adjustable plasma wave, it is characterized in that, in the dispersion of gold nanorods, adopt to add sodium thiosulfate or dissolvable sulfide, regulating and controlling temperature obtains required plasma resonance wavelength with visible near-infrared real-time monitoring.
2, the preparation method of the gold nanorods of a kind of adjustable plasma wave according to claim 1, it is characterized in that, described regulating and controlling temperature, obtaining required plasma resonance wavelength with visible near-infrared real-time monitoring is: the gold nanorods dispersion is heated, monitor vertical absorbing wavelength in real time with visible near-infrared absorption, put into ice-water bath cooling a moment, centrifugation immediately then when arriving required wavelength.
3, the preparation method of the gold nanorods of a kind of adjustable plasma wave according to claim 1 is characterized in that, described sulfide comprises vulcanized sodium, potassium sulfide, ammonium sulfide.
4, the preparation method of the gold nanorods of a kind of adjustable plasma wave according to claim 1 is characterized in that, described dispersion is an aqueous surfactant solution.
5, the preparation method of the gold nanorods of a kind of adjustable plasma wave according to claim 4, it is characterized in that, described surfactant is a cetyltrimethyl ammonium cationoid surfactant, or softex kw or hexadecyldimethyl benzyl ammonium phenyl ammonium bromide or cetyltriethylammonium bromide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105880623A (en) * | 2016-04-13 | 2016-08-24 | 同济大学 | Precious metal nanocrystalline with adjustable plasma resonance absorption characteristic in visible wave band and preparation method of precious metal nanocrystalline |
| CN106092973A (en) * | 2016-06-23 | 2016-11-09 | 大连理工大学 | A kind of photo-thermal detection method based on double noble metal nano probes |
| CN109676128A (en) * | 2019-02-28 | 2019-04-26 | 湖南科技大学 | A kind of preparation method and application of four vulcanization, three molybdenums cladding gold nanorods |
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2007
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105880623A (en) * | 2016-04-13 | 2016-08-24 | 同济大学 | Precious metal nanocrystalline with adjustable plasma resonance absorption characteristic in visible wave band and preparation method of precious metal nanocrystalline |
| CN105880623B (en) * | 2016-04-13 | 2018-04-13 | 同济大学 | It is a kind of to have in noble metal nanocrystalline of the adjustable plasma resonance absorption characteristic of visible waveband and preparation method thereof |
| CN106092973A (en) * | 2016-06-23 | 2016-11-09 | 大连理工大学 | A kind of photo-thermal detection method based on double noble metal nano probes |
| CN106092973B (en) * | 2016-06-23 | 2019-06-25 | 大连理工大学 | A kind of photo-thermal detection method based on double noble metal nano probes |
| CN109676128A (en) * | 2019-02-28 | 2019-04-26 | 湖南科技大学 | A kind of preparation method and application of four vulcanization, three molybdenums cladding gold nanorods |
| CN109676128B (en) * | 2019-02-28 | 2021-05-04 | 湖南科技大学 | Preparation method and application of molybdenum trisulfide coated gold nanorods |
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