CN104999071A - Gold nanorod array and preparation method and application thereof - Google Patents
Gold nanorod array and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a gold nanorod array. The method includes the steps that a gold nanorod aqueous solution modified by cetyl trimethyl ammonium bromide (CATB) is prepared; the final concentration of gold nanorods and the final concentration of the CATB are adjusted to be 0.2-0.6 nmol/L and 0.5-2 mmol/l respectively; sulfhydryl compounds are added and stirred, and a mixed solution can be obtained; the final concentration of the sulfhydryl compounds is 0.01-0.2 mmol/L; after being concentrated, the mixed solution is dripped to a hydrophilic planar substrate; and the gold nanorod array is obtained after natural drying. The preparation method of the gold nanorod array is easy to operate and mild in condition. The prepared gold nanorod array is regular in structure and at the macroscopic millimeter level; and evenly-distributed SERS hot spots are arranged on the surface of the gold nanorod array, and therefore the gold nanorod array can serve as an SERS enhanced substrate easily. The invention further provides the gold nanorod array and application thereof.
Description
Technical field
The present invention relates to technical field of nano material, particularly a kind of gold nano stick array and its preparation method and application.
Background technology
Molecular Raman signal can be strengthened 1,000,000 times of even more high powers by SERS (SERS) effect, is good chemistry, biological detecting method.This superelevation strengthens and mainly depends on SERS " focus ": it mainly by surface plasma body resonant vibration at the adjacent noble metal nano particles as substrate contact position produces in gap etc. " point " with extremely strong local electric field.When detection molecules is adsorbed on " focus " position, its Raman signal can greatly be strengthened.But, due to the random distribution of " focus " position in detection architecture, the reappearance of SERS detection technique is restricted.Therefore, the SERS substrate that preparation a kind of " focus " is evenly distributed controlled, very important in the application aspect of SERS technology.
Strengthen the one in the noble metal nanometer material of substrate as SERS, gold nanorods has special physical anisotropy, and as along with the regulation and control to gold nanorods draw ratio, its intrinsic plasma resonance character can be regulated and controled.And gold nanorods shows the performance more excellent than single gold nanorods by the assembly that self assembly obtains, as regulatable obscurity, to each other plasma resonance are coupled the aggregating characteristic etc. brought, this makes gold nanorods assembly be widely used in fields such as high sensitive sensor (as SERS), optoelectronic devices.
But the small scale of existing gold nanorods assembly, (as CN103341623 only can obtain the assembling of pattern shoulder to shoulder of several gold nanorods), and the nano particle assembling of large area (i.e. micron level) can not be realized, when using it for SERS substrate, structure is taken a walk discontinuous on substrate, overall unordered, " focus " skewness must be caused.
In view of this, be necessary to provide a kind of extensive and gold nano stick array that array structure is regular and its preparation method and application.
Summary of the invention
Based on above-mentioned technical problem, the invention provides a kind of gold nano stick array and its preparation method and application, the scale of described gold nano stick array is at macroscopic grade, and compound with regular structure, described gold nano stick array is when strengthening substrate as SERS, its surface has equally distributed SERS " focus ", strengthens ability high, reproducible.The preparation method of described gold nano stick array is simple to operate, mild condition.
First aspect, the invention provides a kind of preparation method of gold nano stick array, comprises the following steps:
(1) prepare the aqueous solution of gold nanorods that softex kw is modified, and by centrifugal, remove supernatant, then with pure water dispersion, obtain gold nanorods dispersion liquid that concentration is 0.2-0.6nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, and softex kw is added in the precipitation after centrifugal, obtain gold nanorods twice dispersing liquid, the concentration of described softex kw in described gold nanorods twice dispersing liquid is 0.5-2mmol/L;
(3) in described gold nanorods twice dispersing liquid, sulfhydryl compound is added, obtain gold nanorods three dispersion liquids, then by described gold nanorods three dispersion liquids at room temperature stirred overnight, wherein, the concentration of described sulfhydryl compound in described gold nanorods three dispersion liquids is 0.01-0.2mmol/L, six (ethylene glycol) that described sulfhydryl compound comprises (11-mercapto-undecanoic base);
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating, obtain gold nanorods three dispersion liquids concentrated;
(5) by the surface of concentrated gold nanorods three dispersant liquid drops to hydrophily planar substrates, adopt solvent evaporated method dry, obtain gold nano stick array.
Preferably, in step (1), the described method preparing the aqueous solution of the gold nanorods that softex kw is modified is seed mediated growth method.
Preferably, in step (1), described centrifugal rotating speed is 8000-12000r/min.
Preferably, in step (1), the rod of described gold nanorods is long is 30-70nm, and its draw ratio is 3-5.
As described in the present invention, in step (1), described prepare the gold nanorods that softex kw (CTAB) modifies the method for the aqueous solution, the conventional method of this area can be adopted to carry out, such as, the seeded growth method of wet chemistry synthesis and non-crystal seed growth method etc. can adopt seed mediated growth method etc.
As described in the present invention; the gold nanorods adopting the CTAB that obtains of said method to modify the aqueous solution in; the concentration of CTAB is generally 0.5-2mol/L; outside the scope will protected in step of the present invention (2); therefore; the present invention adds CTAB in described gold nanorods dispersion liquid, makes the concentration of described CTAB in described gold nanorods twice dispersing liquid be 0.5-2mmol/L, and the concentration of gold nanorods in described gold nanorods twice dispersing liquid is still 0.2-0.6nmol/L.
Preferably, the volume of a gold nanorods dispersion liquid described in step (1) is identical with the volume of gold nanorods twice dispersing liquid described in step (2).
As described in the present invention, in step (2), the concentration of described softex kw (CTAB) in described gold nanorods twice dispersing liquid refers to the concentration of the CTAB be dissolved in water.
Preferably, in step (2), described centrifugal rotating speed 8000-12000r/min.
Preferably, in step (3), describedly in gold nanorods twice dispersing liquid, add sulfhydryl compound, be specially: be that the aqueous solution of the sulfhydryl compound of 0.1-0.4mmol/L mixes with step (2) gained gold nanorods twice dispersing liquid in the ratio of 1:2 by concentration.
Preferably, in step (4), described concentrated gold nanorods three dispersion liquids are 10-75 times of the concentration of described gold nanorods three dispersion liquids.
Preferably, in step (5), the silicon chip that described hydrophily planar substrates comprises polished silicon slice, there is silicon dioxide layer on surface, surface have the sheet glass of silicon dioxide layer and surface to have the quartz plate of silicon dioxide layer.
Preferably, in step (5), described solvent evaporated method is dry, and referring to surface to drip has the planar substrates horizontal stationary of concentrated gold nanorods three dispersion liquids to be the environment of 40%-95% in air humidity, till treating the natural drying of substrate surface liquid.
Preferably, in step (5), described gold nano stick array is made up of the compact arranged single layer of gold nanometer rods of the longitudinal direction being laid in substrate surface, in described gold nano stick array, the rod of gold nanorods is long is 30-70nm, and its draw ratio is 3-5, and the interrod spacing of gold nanorods is 1-3nm.
The preparation method of the gold nano stick array that first aspect present invention provides is simple to operate, mild condition, effectively can realize the efficient self assembly of gold nanorods, prepared gold nano stick array compound with regular structure, for macroscopic millimeter rank, be conducive to gold nano stick array and be used as SERS enhancing substrate.
Second aspect, the invention provides a kind of gold nano stick array, and described gold nano stick array adopts the preparation method described in first aspect present invention to obtain.
Preferably, described gold nano stick array is made up of the compact arranged gold nanorods of the longitudinal direction being laid in substrate surface, and in described gold nano stick array, the rod of gold nanorods is long is 30-70nm, and its draw ratio is 3-5, and the interrod spacing of gold nanorods is 1-3nm.
The third aspect, the invention provides the application of gold nano stick array in SERS (SERS) detects that the gold nano stick array described in second aspect or the preparation method described in first aspect obtain.
Described application, comprises the following steps:
(1) prepare the aqueous solution of gold nanorods that softex kw is modified, and by centrifugal, remove supernatant, then with pure water dispersion, obtain gold nanorods dispersion liquid that concentration is 0.2-0.6nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, and softex kw is added in the precipitation after centrifugal, obtain gold nanorods twice dispersing liquid, the concentration of described softex kw in described gold nanorods twice dispersing liquid is 0.5-2mmol/L;
(3) in described gold nanorods twice dispersing liquid, sulfhydryl compound is added, obtain gold nanorods three dispersion liquids, then by described gold nanorods three dispersion liquids at room temperature stirred overnight, wherein, the concentration of described sulfhydryl compound in described gold nanorods three dispersion liquids is 0.01-0.2mmol/L, six (ethylene glycol) that described sulfhydryl compound comprises (11-mercapto-undecanoic base);
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating to 10-75 times, obtain gold nanorods three dispersion liquids concentrated;
(5) by the surface of concentrated gold nanorods three dispersant liquid drops to hydrophily planar substrates, adopt solvent evaporated method dry, obtain gold nano stick array;
(6) on the surface of above-mentioned gold nano stick array, drip determinand solution, carry out Raman spectrum test.
Preferably, in step (6), described in carry out Raman spectrum test time, the excitation wavelength of use is 633nm or 785nm.
As described in the present invention, in step (6), the volume of determinand solution should be no more than the volume of gold nano stick array.
Preferably, in step (6), the volume of determinand solution is 0.5-2 μ l.
The concentration of determinand solution is not particularly limited.
The gold nano stick array that the present invention prepares is when strengthening substrate as SERS, because its surface has equally distributed SERS " focus ", not only high to the enhancing ability of determinand, and the reappearance detected might as well.Also the SERS (SERS) gold nano stick array being used for the fields such as food analysis, environmental analysis, Pharmaceutical Analysis, chemical analysis and bioanalysis detects.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.Specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Fig. 1 is transmission electron microscope (TEM) photo of the gold nanorods that in embodiment 1, six alkyl trimethyl ammonium bromides (CTAB) are modified;
Fig. 2 is the ultraviolet-visible absorption spectroscopy of the gold nanorods before and after assembling in embodiment 1;
Fig. 3 is the photo in kind of the gold nano stick array that embodiment 1 obtains;
Fig. 4 is SEM (SEM) photo (top view) of the gold nano stick array that embodiment 1 obtains;
Fig. 5 be gold nano stick array described in embodiment 1 as surface reinforced Raman active (SERS) substrate for detecting the Raman detection result of malachite green;
Fig. 6 is the TEM photo of the gold nanorods that in embodiment 2, CTAB modifies;
Fig. 7 is the SEM photo (top view) of the gold nano stick array that embodiment 2 obtains;
Fig. 8 is the SEM photo (side view) of the gold nano stick array that embodiment 2 obtains.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for gold nano stick array, comprises the following steps:
(1) gold seeds growth method is utilized to prepare the aqueous solution of the gold nanorods that softex kw (CTAB) is modified, specific as follows:
The synthesis of a, gold seeds: the gold chloride of the 0.0005M of 2.5mL is dissolved in the CTAB solution of the 0.2mol/L of 2.5mL, mix, 0.3mL is newly configured, the sodium borohydride solution of the 0.01M of precooling is added in above-mentioned solution fast, powerful mixing 2min, at room temperature 25 DEG C, place 2h, obtain gold seeds;
The configuration of the growth solution of b, gold nanorods: the silver nitrate of 0.15mL, 0.004mol/L, the chlorauric acid solution of 5mL, 0.001M are added in the CTAB of 5mL, 0.2mol/L, then the sodium ascorbate of the 0.0788M of 70 μ L is added, abundant reductase 12 min, add the gold seeds that 12 μ L above-mentioned steps (a) configure, after abundant stirring 20s, obtain mixed solution, and in 25 DEG C of set aside for use;
And by above-mentioned mixed solution by under the rotating speed of 10000rpm/min centrifugal resuspended 2-3 time (namely centrifugal, remove supernatant, again with the dispersion of 10ml pure water), remove unnecessary reaction residue, obtain gold nanorods dispersion liquid that concentration is 0.4nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, wherein centrifugal speed is 12000rpm/min, and softex kw is added in the precipitation after centrifugal, obtain the gold nanorods twice dispersing liquid of 10ml, the concentration of described CTAB in described gold nanorods twice dispersing liquid is 1.2mmol/L;
(3) be that (11-mercapto-undecanoic base) six (ethylene glycol) aqueous solution of 0.2mmol/L mixes with step (2) gained gold nanorods twice dispersing liquid in the ratio of 1:2 by concentration, and at room temperature stirred overnight, obtain gold nanorods three dispersion liquids, wherein, the concentration of described (11-mercapto-undecanoic base) six (ethylene glycol) in described gold nanorods three dispersion liquids is 0.1mmol/L;
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating to 50 times, obtain gold nanorods three dispersion liquids concentrated;
(5) by concentrated gold nanorods three dispersant liquid drops on the silicon chip of polishing, adopt solvent evaporated method dry, and silicon wafer horizontal be still in the environment that air humidity is 80%, till treating the natural drying of substrate surface liquid, obtain gold nano stick array.
Fig. 1 is the transmission electron microscope picture (TEM) of a gold nanorods dispersion liquid of the CTAB modification that in the embodiment of the present invention 1, step (1) is obtained, as can be seen from Figure 1, the particle diameter of described gold nanorods is more homogeneous, and monodispersity is good, rod is long is 65nm, and its draw ratio is 3.5.
Fig. 2 is the uv-visible absorption spectra of the gold nanorods before and after assembling in the embodiment of the present invention 1, " before self assembly gold nanorods " in figure refers to gold nanorods dispersion liquid that CTAB modifies, " after self assembly gold nanorods " refers to obtained gold nanorods three dispersion liquids of step (3), as can be seen from Figure 2, the absworption peak of " before self assembly gold nanorods " mainly concentrates on the peak centered by 810nm, few at the absworption peak of about 500nm, and the absworption peak of gold nanorods after self assembly is positioned at 540nm, about 650nm, this may be because the major surfaces dressing agent of gold nanorods becomes (11-mercapto-undecanoic base) six (ethylene glycol) by CTAB, therefore absworption peak has movement.
Fig. 3 is the macro morphology that photo figure, Fig. 3 in kind of the obtained gold nano stick array of the embodiment of the present invention 1 reflects this gold nano stick array; Fig. 4 is the scanning electron microscope diagram (SEM of gold nano stick array, top view), as can be seen from Figure 4, the compound with regular structure of described gold nano stick array, this gold nano stick array is made up of the compact arranged gold nanorods of the longitudinal direction being laid in substrate surface, and described gold nanorods arranges perpendicular to substrate surface, and the rod of gold nanorods is long is 65nm, its draw ratio is 3.5, and the interrod spacing of gold nanorods is 2nm.This gold nano stick array structurally ordered, regular, can strengthen substrate as SERS, its surface has equally distributed SERS " focus ".
Application Example 1
Gold nano stick array obtained for above-described embodiment 1 being used for SERS and strengthening substrate, for detecting malachite green, being specially:
The gold nano stick array that Example 1 step (5) is obtained, drips 5 μ L, 10 on this gold nano stick array surface
-6the malachite green aqueous solution of mol/L, after its drying, carries out Raman spectrum test.
It is 633nm that Raman tests the optical maser wavelength used, and integral number of times is 1 time.
Simultaneously in order to outstanding effect of the present invention, comparable sodium, unassembled gold nanorods are also used as SERS substrate, to 10
-6the malachite green aqueous solution of mol/L carries out Raman spectrum test.
Raman test result as shown in Figure 5: as ise apparent from FIG. 5, the gold nano stick array formed when assembling is used for SERS substrate (time in Fig. 5 a), have very high SERS active, the more unassembled gold nanorods of its intensification factor is (b) about high 5 times in Fig. 5.
Embodiment 2
A preparation method for gold nano stick array, comprises the following steps:
(1) gold seeds growth method is utilized to prepare the aqueous solution of the gold nanorods that softex kw (CTAB) is modified, specific as follows:
The chlorauric acid solution of 1mL, 5mM is added in the test tube or beaker of 50mL, the CTAB aqueous solution getting 5mL, 0.2M adds wherein, gentle agitation, add 4.5mL ultra-pure water, the sodium oleate solution of 500 μ L, 0.1M, the liquor argenti nitratis ophthalmicus of 250 μ L, 4mM, gentle agitation, add 8 μ L, 37% concentrated hydrochloric acid, gentle agitation, add the ascorbic acid 56 μ L of 0.1M, gentle agitation, treats that solution fades to colourless, adds the sodium borohydride solution of 15 μ L, 0.01M fast, in 35 DEG C of insulating boxs, leave standstill 2 ~ 3h, obtain mixed solution;
And by above-mentioned mixed solution by under the rotating speed of 12000rpm/min centrifugal resuspended 2-3 time (namely centrifugal, remove supernatant, again with the dispersion of 10ml pure water), remove unnecessary reaction residue, obtain gold nanorods dispersion liquid that concentration is 0.6nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, wherein centrifugal speed is 8000rpm/min, and softex kw is added in the precipitation after centrifugal, obtain the gold nanorods twice dispersing liquid of 10ml, the concentration of described CTAB in described gold nanorods twice dispersing liquid is 2mmol/L;
(3) be that (11-mercapto-undecanoic base) six (ethylene glycol) aqueous solution of 0.4mmol/L mixes with step (2) gained gold nanorods twice dispersing liquid in the ratio of 1:2 by concentration, and at room temperature stirred overnight, obtain gold nanorods three dispersion liquids, wherein, the concentration of described (11-mercapto-undecanoic base) six (ethylene glycol) in described gold nanorods three dispersion liquids is 0.2mmol/L;
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating to 75 times, obtain gold nanorods three dispersion liquids concentrated;
(5) by concentrated gold nanorods three dispersant liquid drops to surface have silicon dioxide layer silicon chip on, employing solvent evaporated method is dry, namely be that above-mentioned silicon wafer horizontal is still in the environment that air humidity is 95%, after the natural drying of substrate surface liquid, obtain gold nano stick array.
Fig. 6 is the transmission electron microscope picture (TEM) of a gold nanorods dispersion liquid of the CTAB modification that in the embodiment of the present invention 2, step (1) is obtained, as can be seen from Figure 6, the particle diameter of described gold nanorods is more homogeneous, and monodispersity is good, rod is long is 30nm, and its draw ratio is 3; Fig. 7, Fig. 8 are respectively SEM photo (top view), the SEM photo (side view) of the obtained gold nano stick array of embodiment 2, as can be seen from Figure 7, the compound with regular structure of described gold nano stick array, described gold nano stick array is made up of the compact arranged gold nanorods of the longitudinal direction being laid in substrate surface, as can be seen from Figure 8, gold nanorods arranges perpendicular to substrate surface, form gold nano stick array, in described gold nano stick array, the rod of gold nanorods is long is 30nm, its draw ratio is 3, and the interrod spacing of gold nanorods is 3nm.
Application Example 2
Gold nano stick array obtained for above-described embodiment 2 being used for SERS and strengthening substrate, for detecting malachite green, being specially:
The gold nano stick array that Example 2 step (5) is obtained, drips 5 μ L, 10 on this gold nano stick array surface
-5mol/L the malachite green aqueous solution, after its drying, carry out Raman spectrum test.
It is 633nm that Raman tests the optical maser wavelength used, and integral number of times is 1 time.
When described gold nano stick array is used for SERS substrate, have very high SERS active, the more unassembled gold nanorods of its intensification factor is about high 4 times.
Embodiment 3
A preparation method for gold nano stick array, comprises the following steps:
(1) gold seeds growth method is utilized to prepare the aqueous solution of the gold nanorods that softex kw (CTAB) is modified, specific as follows:
The synthesis of a, gold seeds: the gold chloride of the 0.0005M of 2.5mL is dissolved in the CTAB solution of the 0.2mol/L of 2.5mL, mix, 0.3mL is newly configured, the sodium borohydride solution of the 0.01M of precooling is added in above-mentioned solution fast, powerful mixing 2min, at room temperature 25 DEG C, place 2h, obtain gold seeds;
The configuration of the growth solution of b, gold nanorods: the silver nitrate of 0.10mL, 0.004mol/L, the chlorauric acid solution of 5mL, 0.001M are added in the CTAB of 5mL, 0.2mol/L, then the sodium ascorbate of the 0.0788M of 70 μ L is added, abundant reductase 12 min, add the gold seeds that 10 μ L above-mentioned steps (a) configure, after abundant stirring 20s, obtain mixed solution, and in 25 DEG C of set aside for use;
And by above-mentioned mixed solution by under the rotating speed of 8000rpm/min centrifugal resuspended 2-3 time (namely centrifugal, remove supernatant, again with the dispersion of 10ml pure water), remove unnecessary reaction residue, obtain gold nanorods dispersion liquid that concentration is 0.2nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, wherein centrifugal speed is 10000rpm/min, and softex kw is added in the precipitation after centrifugal, obtain the gold nanorods twice dispersing liquid of 10ml, the concentration of described CTAB in described gold nanorods twice dispersing liquid is 0.5mmol/L;
(3) be that (11-mercapto-undecanoic base) six (ethylene glycol) aqueous solution of 0.1mmol/L mixes with step (2) gained gold nanorods twice dispersing liquid in the ratio of 1:2 by concentration, and at room temperature stirred overnight, obtain gold nanorods three dispersion liquids, wherein, the concentration of described (11-mercapto-undecanoic base) six (ethylene glycol) in described gold nanorods three dispersion liquids is 0.01mmol/L;
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating to 10 times, obtain gold nanorods three dispersion liquids concentrated;
(5) concentrated gold nanorods three dispersant liquid drops are had on the quartz plate of silicon dioxide layer to surface, employing solvent evaporated method is dry, namely be the environment of 40% by above-mentioned quartz plate horizontal stationary in air humidity, treat the natural drying of substrate surface liquid, obtain gold nano stick array.
The gold nano stick array that embodiment 3 obtains is made up of the compact arranged single layer of gold nanometer rods of the longitudinal direction being laid in substrate surface, and in described gold nano stick array, the rod of gold nanorods is long is 70nm, and its draw ratio 5, the interrod spacing of gold nanorods is 1nm.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for gold nano stick array, is characterized in that, comprises the following steps:
(1) prepare the aqueous solution of gold nanorods that softex kw is modified, and by centrifugal, remove supernatant, then with pure water dispersion, obtain gold nanorods dispersion liquid that concentration is 0.2-0.6nmol/L;
(2) carry out centrifugal to described gold nanorods dispersion liquid, and softex kw is added in the precipitation after centrifugal, obtain gold nanorods twice dispersing liquid, the concentration of described softex kw in described gold nanorods twice dispersing liquid is 0.5-2mmol/L;
(3) in described gold nanorods twice dispersing liquid, sulfhydryl compound is added, obtain gold nanorods three dispersion liquids, then by described gold nanorods three dispersion liquids at room temperature stirred overnight, wherein, the concentration of described sulfhydryl compound in described gold nanorods three dispersion liquids is 0.01-0.2mmol/L, six (ethylene glycol) that described sulfhydryl compound comprises (11-mercapto-undecanoic base);
(4) described gold nanorods three dispersion liquids are carried out centrifugal concentrating, obtain gold nanorods three dispersion liquids concentrated;
(5) by the surface of concentrated gold nanorods three dispersant liquid drops to hydrophily planar substrates, adopt solvent evaporated method dry, obtain gold nano stick array.
2. the preparation method of gold nano stick array as claimed in claim 1, is characterized in that, in step (1), the described method preparing the aqueous solution of the gold nanorods that softex kw is modified is seed mediated growth method.
3. the preparation method of gold nano stick array as claimed in claim 1, it is characterized in that, the volume of a gold nanorods dispersion liquid described in step (1) is identical with the volume of gold nanorods twice dispersing liquid described in step (2).
4. the preparation method of gold nano stick array as claimed in claim 1, it is characterized in that, in step (2), described centrifugal rotating speed is 8000-12000r/min.
5. the preparation method of gold nano stick array as claimed in claim 1, is characterized in that, in step (4), described concentrated gold nanorods three dispersion liquids are 10-75 times of the concentration of described gold nanorods three dispersion liquids.
6. the preparation method of gold nano stick array as claimed in claim 1, it is characterized in that, in step (5), the silicon chip that described hydrophily planar substrates comprises polished silicon slice, there is silicon dioxide layer on surface, surface have the sheet glass of silicon dioxide layer and surface to have the quartz plate of silicon dioxide layer.
7. the preparation method of gold nano stick array as claimed in claim 1, it is characterized in that, in step (5), described solvent evaporated method is dry, referring to surface to drip has the planar substrates horizontal stationary of concentrated gold nanorods three dispersion liquids to be the environment of 40%-95% in air humidity, till treating the natural drying of substrate surface liquid.
8. the preparation method of gold nano stick array as claimed in claim 1, it is characterized in that, in step (5), described gold nano stick array is made up of the compact arranged gold nanorods of the longitudinal direction being laid in substrate surface, in described gold nano stick array, the rod of gold nanorods is long is 30-70nm, and its draw ratio is 3-5, and the interrod spacing of gold nanorods is 1-3nm.
9. a gold nano stick array, is characterized in that, adopts the preparation method described in claim 1-5 to obtain.
10. the application of gold nano stick array in SERS detects that obtain of preparation method as claimed in claim 1.
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| CN111060490A (en) * | 2019-12-25 | 2020-04-24 | 安徽中科赛飞尔科技有限公司 | SERS detection method of succinylcholine chloride |
| CN111198175A (en) * | 2018-11-19 | 2020-05-26 | 中国科学院宁波材料技术与工程研究所 | Macroscopic large-area nano gold rod two-dimensional array with controllable distribution of hot spots and application |
| CN113899732A (en) * | 2021-09-30 | 2022-01-07 | 长沙新材料产业研究院有限公司 | PH value sensitive ligand modified nano-gold and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153333A (en) * | 2007-09-27 | 2008-04-02 | 上海交通大学 | Method for producing gold nano stick array chip based on DNA molecule |
| WO2011021846A2 (en) * | 2009-08-18 | 2011-02-24 | 한국과학기술원 | Multi-spot metal-deposited nucleic acid chip with nanostructure arrays for diagnosing corneal dystrophy, and method for producing same |
| CN102397557A (en) * | 2010-09-07 | 2012-04-04 | 国家纳米科学中心 | Modification method for gold nanorods and gold nanorods-functional molecule composite |
| CN103506629A (en) * | 2012-06-18 | 2014-01-15 | 国家纳米科学中心 | Gold nanorod vertical array and preparing method thereof |
| CN103950891A (en) * | 2014-05-21 | 2014-07-30 | 江南大学 | Preparing method of high conductivity chain-shaped photoelectric nanometer bridge |
| CN104152897A (en) * | 2014-08-15 | 2014-11-19 | 国家纳米科学中心 | Method for manufacturing SERS substrate monolayer film and SERS substrate monolayer film |
-
2015
- 2015-06-24 CN CN201510354816.9A patent/CN104999071B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101153333A (en) * | 2007-09-27 | 2008-04-02 | 上海交通大学 | Method for producing gold nano stick array chip based on DNA molecule |
| WO2011021846A2 (en) * | 2009-08-18 | 2011-02-24 | 한국과학기술원 | Multi-spot metal-deposited nucleic acid chip with nanostructure arrays for diagnosing corneal dystrophy, and method for producing same |
| CN102397557A (en) * | 2010-09-07 | 2012-04-04 | 国家纳米科学中心 | Modification method for gold nanorods and gold nanorods-functional molecule composite |
| CN103506629A (en) * | 2012-06-18 | 2014-01-15 | 国家纳米科学中心 | Gold nanorod vertical array and preparing method thereof |
| CN103950891A (en) * | 2014-05-21 | 2014-07-30 | 江南大学 | Preparing method of high conductivity chain-shaped photoelectric nanometer bridge |
| CN104152897A (en) * | 2014-08-15 | 2014-11-19 | 国家纳米科学中心 | Method for manufacturing SERS substrate monolayer film and SERS substrate monolayer film |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105712293A (en) * | 2016-02-25 | 2016-06-29 | 国家纳米科学中心 | Gold nanosphere two-dimensional array structure, preparation method and application |
| CN105755463A (en) * | 2016-03-07 | 2016-07-13 | 东南大学 | Method for preparing hydrophobic surface solid monolayer uniform SERS substrate |
| CN106940310A (en) * | 2017-03-06 | 2017-07-11 | 宁波大学 | Substrate and preparation method thereof is immunized in a kind of self assembly gold nanorods SERS |
| CN106940310B (en) * | 2017-03-06 | 2019-08-23 | 宁波大学 | Substrate and preparation method thereof is immunized in a kind of self assembly gold nanorods SERS |
| CN107235471B (en) * | 2017-04-20 | 2019-06-14 | 广东工业大学 | A kind of surface enhanced Raman scattering substrate and its preparation method and application |
| CN107235471A (en) * | 2017-04-20 | 2017-10-10 | 广东工业大学 | A kind of surface enhanced Raman scattering substrate and its preparation method and application |
| CN106944615A (en) * | 2017-05-11 | 2017-07-14 | 洛阳理工学院 | A kind of preparation method of solid coated with silica gold nanorods composite nano materials |
| CN107290329A (en) * | 2017-05-17 | 2017-10-24 | 中国人民解放军第二军医大学 | A kind of preparation method and application of sulfydryl beta cyclodextrin functionalization SERS paper substrates |
| CN108356277A (en) * | 2018-02-24 | 2018-08-03 | 浙江大学 | A kind of preparation method of gold nanorods |
| CN108356277B (en) * | 2018-02-24 | 2020-08-11 | 浙江大学 | Preparation method of gold nanorods |
| CN111198175A (en) * | 2018-11-19 | 2020-05-26 | 中国科学院宁波材料技术与工程研究所 | Macroscopic large-area nano gold rod two-dimensional array with controllable distribution of hot spots and application |
| CN111198175B (en) * | 2018-11-19 | 2022-09-27 | 中国科学院宁波材料技术与工程研究所 | Macroscopic large-area nano gold rod two-dimensional array with controllable distribution of hot spots and application |
| CN109632723A (en) * | 2019-02-22 | 2019-04-16 | 东北大学 | A kind of optical fiber SPR sensor based on multilayer gold nanorods |
| CN110108697A (en) * | 2019-06-25 | 2019-08-09 | 北威(重庆)科技股份有限公司 | Surface enhanced Raman scattering micro-nano chip and preparation method thereof, application and Raman spectrum test macro |
| CN110108697B (en) * | 2019-06-25 | 2022-03-08 | 北威(重庆)科技股份有限公司 | Surface-enhanced Raman scattering micro-nano chip, preparation method and application thereof, and Raman spectrum testing system |
| CN110987915A (en) * | 2019-12-03 | 2020-04-10 | 泸州品创科技有限公司 | Method for rapidly identifying Chinese liquor based on gold nanorod colorimetric sensor array |
| CN110987915B (en) * | 2019-12-03 | 2022-04-01 | 泸州品创科技有限公司 | Method for rapidly identifying Chinese liquor based on gold nanorod colorimetric sensor array |
| CN111060490A (en) * | 2019-12-25 | 2020-04-24 | 安徽中科赛飞尔科技有限公司 | SERS detection method of succinylcholine chloride |
| CN113899732A (en) * | 2021-09-30 | 2022-01-07 | 长沙新材料产业研究院有限公司 | PH value sensitive ligand modified nano-gold and preparation method thereof |
| CN113899732B (en) * | 2021-09-30 | 2023-09-22 | 航天科工(长沙)新材料研究院有限公司 | PH value sensitive ligand modified nano gold and preparation method thereof |
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