CN103132143B - Gold nanorod and preparing method thereof - Google Patents
Gold nanorod and preparing method thereof Download PDFInfo
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- CN103132143B CN103132143B CN201110391939.1A CN201110391939A CN103132143B CN 103132143 B CN103132143 B CN 103132143B CN 201110391939 A CN201110391939 A CN 201110391939A CN 103132143 B CN103132143 B CN 103132143B
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Abstract
The invention provides a preparing method of a gold nanorod. The preparing method of the gold nanorod is characterized in that a growth solution of the gold nanorod further contains soluble copper salt, and the added quantity, relative to each mole of gold seed crystal, of the soluble copper salt is 16-400 moles. The length-diameter ratio of the gold nanorod obtained through the method is in a range of 2.3 +/- 0.3 to 3.7 +/- 0.4, the value of full wave at half maximum (FWHM) of an absorption peak of a longitudinal surface plasmon resonance is 0.20-0.22eV, and the ratio of absorbance of absorption peak positions of the longitudinal surface plasmon resonance and a transverse surface plasmon resonance (ALSPR/ATSPR) is 2.3 to 4.9. According to the preparing method of the gold nanorod, cupric ions are used for the first time to catalyze forming of the gold nanorod of high quality. The preparing method of the gold nanorod is simple in operating step, monodispersity of the size of the obtained gold nanorod is good, and performance of the gold nanorod is obviously improved. In addition, the preparing method of the gold nanorod is high in repeatability and moderate in reaction condition, and a used reagent is cheap and nontoxic.
Description
Technical field
The preparation method that the present invention relates to a kind of gold nanorods and the gold nanorods prepared by the method.
Background technology
At present, wet chemical mainly contains three kinds for the method for gold nanorods, wherein, the growth method (Seed-mediated Growth) that the most widely used seed being the people such as Murphy propose is modulated, namely by regulating correlated response parameter as the gold nanorods to obtain different-shape and size such as reactant concn, seed concentration, kinds of surfactants.Now generally adopt Ag
+auxiliary seed mediated growth method synthesizes the gold nanorods of different length-to-diameter ratio.Ag
+add the productive rate that can significantly improve gold nanorods and the length-to-diameter ratio realizing gold nanorods regulates and controls within the specific limits.The people such as Zhu (Jing Zhu, Ken-Tye Yong, Indrajit Roy, Rui Hu, Hong Ding, Lingling Zhao, Mark T Swihart, Guang S He, Yiping Cuiand Paras N Prasad, " Additive controlled synthesis of gold nanorods (GNRs) fortwo-photon luminescence imaging of cancer cells. " Nanotechnology, 2010,21:285106-285113) size and shape that also can be regulated and controled gold nanorods by the concentration of adjustment HCl is proposed.
In addition, conventional xitix (AA) and Au
3+ratio have two kinds.One is the people such as Liu (Mingzhao Liu and Philippe Guyot-Sionnest, " Mechanism of silver (I)-assistedgrowth of gold nanorods and bipyramids. " Journal of Physical Chemistry B, 2005,109 (47): 22192-22200.) [AA]/[Au is proposed
3+]=1.6, [seed]/[Au
3+]=0.0012, and in the growth solution of gold nanorods, separately add appropriate amount of acid to reduce growth velocity, Au in the method
3+reduce completely, Au
3+utilization ratio is higher.Another kind is the people such as Alkilany (Alaaldin M.Alkilany, Pratik K.Nagaria, Cole R.Hexel, Timothy J.Shaw, Catherine J.Murphy, and Michael D.Wyatt, " Cellular Uptake and Cytotoxicity of Gold Nanorods:Molecular Origin ofCytotoxicity and Surface Effects. " Small, 2009,5:701-708.) [AA]/[Au is proposed
3+]=1.1, [seed]/[Au
3+]=0.0006, does not add other acid, in the method, only has the Au of 1/5
3+be reduced, Au
3+utilization ratio is lower.These two kinds of methods are all mainly through regulating Ag
+concentration regulate the length-to-diameter ratio of gold nanorods, the size monodisperse of the gold nanorods obtained is good not.
2009, the people such as Khanal (Bishnu P. Khanal and Eugene R.Zubarev, " Polymer-functionalized platinum-on-gold bimetallic nanorods. " Angew.Chem.Int.Ed, 2009,48:6888-6891.) propose the method that multistep adds AA synthesis gold nanorods, this method significantly improves the size monodisperse of gold nanorods, also improves the utilization ratio of gold simultaneously.But the increase of number of times is added with AA, long wave surface plasmon resonance (longitudinal surfaceplasmon resonance, LSPR) absorption peak peak position changes greatly (can reach about 180nm), the bad control of length-to-diameter ratio, and repeatedly interpolation AA makes preparation process show slightly loaded down with trivial details.At present, this method uses less.
Summary of the invention
The object of the invention is to overcome the shortcoming that complex operation in prior art is bad with obtained gold nanorods size monodisperse, a kind of gold nanorods and preparation method thereof is provided.
The improvement of gold nanorods quality, usually by reducing its speed of growth to realize, being added a small amount of acid as above-mentioned, being reduced the reducing power of xitix further, repeatedly add reductive agent etc. on a small quantity in growth solution.The present inventor finds, in gold nanorods growth solution, add a certain amount of Cu
2+significantly accelerate the growth kinetics of gold nanorods.Cu
2+the catalyzer of gold nanorods growth, can obviously shorten the growth time of gold nanorods, although Cu
2+add and accelerate speed of response, and the quality of the gold nanorods obtained does not have corresponding reduction, but also significantly improve the distribution of sizes of gold nanorods, record peak width at half height (the full wave at half maximum of long wave surface plasmon resonance absorption peak, FWHM) the most I of value reaches 0.20eV, and gold nanorods LSPR peak position is also by Cu
2+the impact of concentration, high density Cu
2+make LSPR absorption peak blue shift (the nanometer rod blue shift that length-to-diameter ratio is large is more).So, use Cu
2+regulate the growth kinetics of gold nanorods, the quality of gold nanorods can be improved further.
The present inventor also finds, different Ag
+under concentration conditions (namely during different length-to-diameter ratio), obtain the Cu needed for top-quality gold nanorods
2+concentration different, such as Ag
+when concentration is 40 μMs, the Cu of obtained top-quality gold nanorods
2+concentration is 160 μMs, Ag
+when concentration is 70 μMs, the Cu of obtained top-quality gold nanorods
2+concentration is 100 μMs.
Thus, the invention provides a kind of preparation method of gold nanorods, the method comprises mixing gold nanorods growth solution and Jin Jing's kind, mixing gained mixture is placed under the condition of golden seeded growth to make described golden seeded growth, described gold nanorods growth solution contains tensio-active agent, reductive agent, tetra chlorauric acid and soluble silver salt, it is characterized in that, described gold nanorods growth solution is also containing soluble copper salt, Jin Jing's kind relative to every mole, the add-on of soluble copper salt is 16-400mol.
The present invention also provides a kind of gold nanorods obtained by aforesaid method, the length-to-diameter ratio of described gold nanorods is in 2.3 ± 0.3 to 3.7 ± 0.4 scope, peak width at half height (FWHM) value of long wave surface plasmon resonance absorption peak is 0.20-0.22eV, and long wave surface plasmon resonance absorption peak position and shortwave surface plasmon resonance absorb the ratio (A of peak position absorption value
lSPR/ A
tSPR) be 2.3-4.9.
By technique scheme, the present invention utilizes the formation of copper ions catalyze high quality gold nanorods first, and the method operation steps is simple, and obtained gold nanorods size monodisperse is good, significantly optimizes the performance of gold nanorods.And method repeatability of the present invention is high, reaction conditions is gentle, agents useful for same non-toxic inexpensive.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is the UV-visible-near infrared absorption figure of gold nanorods solution, wherein a-d is respectively the UV-visible-near infrared absorption figure of the gold nanorods solution that embodiment of the present invention 1-4 obtains, and a '-d ' is respectively the UV-visible-near infrared absorption figure of the gold nanorods solution that comparative example 1-4 obtains;
Fig. 2 is the gold nanorods transmission electron microscope shape appearance figure that embodiment of the present invention 1-4 obtains, and wherein A-D is respectively the obtained gold nanorods transmission electron microscope shape appearance figure of embodiment of the present invention 1-4.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The preparation method of gold nanorods provided by the invention comprises mixing gold nanorods growth solution and Jin Jing's kind, mixing gained mixture is placed under the condition of golden seeded growth to make described golden seeded growth, described gold nanorods growth solution contains tensio-active agent, reductive agent, tetra chlorauric acid and soluble silver salt, it is characterized in that, described gold nanorods growth solution is also containing soluble copper salt, Jin Jing's kind relative to every mole, the add-on of soluble copper salt is 16-400mol, is preferably 50-267mol.
The present inventor finds, when the soluble copper salt added is in above-mentioned preferred scope, can improves the quality of gold nanorods, thus improve the size monodisperse of gold nanorods further while remarkable fast reaction speed.
Wherein, as long as the solubleness of described soluble copper salt under Jin Jing plants growth temperature in water is greater than 25g/100g water can realize object of the present invention, preferably, described soluble copper salt is one or more in cupric chloride, copper sulfate and cupric nitrate.
According to the present invention, described Jin Jing plants and can contact with described gold nanorods growth solution with the form of golden seed-solution, described golden seed-solution can obtain according to method well-known to those skilled in the art, such as by adding the tetra chlorauric acid aqueous solution in the cetyl trimethylammonium bromide aqueous solution, then under the condition stirred, sodium borohydride and/or the POTASSIUM BOROHYDRIDE aqueous solution is added, continue to stir 3-5min, leave standstill 2-5h to obtain, wherein, cetyl trimethylammonium bromide, the mol ratio of sodium borohydride and/or POTASSIUM BOROHYDRIDE and tetra chlorauric acid is 295-305: 2.2-2.5: 1.
According to the present invention, in described gold nanorods growth solution, the add-on of each component can be selected in relative broad range, under preferable case, Jin Jing's kind relative to every mole, the add-on of described tensio-active agent, reductive agent, tetra chlorauric acid and soluble silver salt can be 125000-208334mol, 920-1334mol, 831-835mol and 33-250mol.
Described tensio-active agent, reductive agent and soluble silver salt can select this area common agents, and under preferable case, described tensio-active agent is cetyl trimethylammonium bromide.Described reductive agent is sodium borohydride and/or POTASSIUM BOROHYDRIDE.Described soluble silver salt is Silver Nitrate.
In the present invention, described Jin Jing plants the concentration that in growth solution, Jin Jing plants and is preferably 0.2-0.3mM.
According to the present invention, in described mixture, the concentration of described soluble silver salt is 30-50 μM, and the concentration of described soluble copper salt is 150-200 μM; Or the concentration of described soluble silver salt is 60-100 μM, the concentration of described soluble copper salt is 50-120 μM.The present inventor finds, when the concentration of soluble silver salt and soluble copper salt meets above-mentioned relation in described mixture, further improves the quality of gold nanorods.
The present inventor finds, the adjustment that Jin Jing plants growth velocity can be realized by adding acid while add soluble copper salt in described gold nanorods growth solution, the size monodisperse of gold nanorods improves further, therefore preferably, also acid is contained in described gold nanorods growth solution.Described acid can be sulfuric acid and/or hydrochloric acid, the Jin Jing's kind relative to every mole, and with pH meter, the add-on of described acid is 8332-58334mol.
The compound method of described gold nanorods growth solution can be the conventional method in this area, preferably, the method for described gold nanorods growth solution preparation comprises and in surfactant soln, adds tetra chlorauric acid, soluble silver salt, soluble copper salt, acid and reductive agent successively.
According to the present invention, planted to contact by described gold nanorods growth solution can realize object of the present invention with described Jin Jing, under preferable case, making the condition of described golden seeded growth comprise temperature is 25-35 DEG C, and the time is 12-16h.
The ratio that the inventive method prepares gold nanorods can reach 92-96%.
The present invention also provides a kind of gold nanorods prepared by aforesaid method, and the length-to-diameter ratio of described gold nanorods is in the scope of 2.3 ± 0.3 to 3.7 ± 0.4, and FWHM value is 0.20-0.22eV, A
lSPR/ A
tSPRvalue is 2.3-4.9.
Below will be described the present invention by embodiment.In following examples, agents useful for same is as follows: cetyl trimethylammonium bromide (Amresco), sodium borohydride (Alfa Aesar), tetra chlorauric acid (Chemical Reagent Co., Ltd., Sinopharm Group), xitix (Research chemicals Ltd); LSPR peak position and A
lSPR/ A
tSPRobtained by UV-visible-near infrared absorption figure, corresponding Energy value is calculated according to UV-visible-near infrared absorption figure and formula " E (energy)=h (quantum of action) v (frequency of light)=hc (light velocity)/λ (wavelength of light) ", the peak width at half height at the peak obtained is FWHM value, UV-visible-near infrared absorption is recorded when 25-35 DEG C by ultraviolet spectrophotometer (Varian Cary 50, the U.S.); The length-to-diameter ratio of gold nanorods is by transmission electron microscope (Tecnai G
220S-TWIN, U.S.) characterize and record, statistics number is 900; The calculating of length-to-diameter ratio theoretical value (R) is with reference to formula λ
max=(53.71R-42.29) ε
m+ 495.14, wherein, λ
maxfor LSPR peak position (nm), ε
mfor the specific inductivity of gold nanorods surrounding medium, get 1.77; Random statistics arbitrarily 1000 gold nano grains (comprise bar-shaped with non-bar-shaped), the ratio between the quantity of wherein bar-shaped gold nano grain and total gold nano grain quantity is ratio.
In following examples, Jin Jing plants and prepares by the following method: getting 7.5mL concentration is the 0.1M cetyl trimethylammonium bromide aqueous solution, add the tetra chlorauric acid aqueous solution that 55.1 μ L concentration are 45.4mM wherein, after mixing by volume dilution to 9.4mL, sodium borohydride aqueous solution that 0.6mL concentration is 0.01M (before using Extemporaneous be placed in frozen water preserve) is added under the condition of magnetic agitation, obtained mixing solutions (cetyl trimethylammonium bromide, the mol ratio of sodium borohydride and tetra chlorauric acid is 300: 2.4: 1), 2-5h is left standstill after stirring 3min, obtain the golden seed-solution of planting containing Jin Jing, the concentration that Jin Jing plants GOLD FROM PLATING SOLUTION is 0.25mM.
Embodiment 1
Get the cetyl trimethylammonium bromide aqueous solution that 100mL concentration is 0.1M, add the tetra chlorauric acid aqueous solution that 1.1mL concentration is 45.4mM wherein, 0.4mL concentration is the silver nitrate aqueous solution of 10mM, 1.6mL concentration is the copper chloride solution of 10mM, 2mL concentration is the aqueous sulfuric acid of 0.5M, after mixing, adding 800 μ L concentration is again the aqueous ascorbic acid of 0.1M, the mixing solutions obtained becomes colorless, then the golden seed-solution that 240 μ L are prepared by above-mentioned steps is added, mix rear 30 DEG C of waters bath with thermostatic control 12 hours, obtain gold nanorods solution.Measure the UV-visible-near infrared absorption characteristic parameter of gold nanorods solution, measurement result is as shown in a of Fig. 1 and table 1; Observe the images of transmissive electron microscope of gold nanorods, as shown in the A in Fig. 2.
Embodiment 2-4
Gold nanorods solution is prepared according to the method for embodiment 1, replaced by " 0.7mL concentration is the silver nitrate aqueous solution of 10mM; 1mL concentration is the copper chloride solution of 10mM ", " 1mL concentration is the silver nitrate aqueous solution of 10mM; 0.6mL concentration is the copper chloride solution of 10mM " and " 1.5mL concentration is the silver nitrate aqueous solution of 10mM, and 0.3mL concentration is the copper chloride solution of 10mM " respectively unlike " 0.4mL concentration is the silver nitrate aqueous solution of 10mM and 1.6mL concentration is the copper chloride solution of 10mM ".Measure the UV-visible-near infrared absorption characteristic parameter measurement result of gold nanorods solution as shown in the b-d in Fig. 1 and table 1; Observe the images of transmissive electron microscope of gold nanorods, as shown in the B-D in Fig. 2.
Comparative example 1-4
Gold nanorods solution is prepared respectively according to the method for embodiment 1-4, unlike, in the cetyl trimethylammonium bromide aqueous solution, do not add soluble copper salt.Measure the UV-visible-near infrared absorption characteristic parameter measurement result of gold nanorods solution as shown in a '-d ' in Fig. 1 and table 1; Observe the images of transmissive electron microscope of gold nanorods.
Table 1
Embodiment 5-11
Gold nanorods solution is prepared according to the method for embodiment 2, but the amount of the xitix added is different, addition and the correlation parameter measurement result of xitix are as shown in table 2, in table 2, "--" represents that the UV-visible-near infrared absorption of the gold nanorods solution that this embodiment obtains only has unimodal, calculate this parameter value meaningless, therefore omit.
Comparative example 5-11
Prepare gold nanorods solution according to the method for comparative example 2, but the amount of the xitix added is different, addition and the correlation parameter measurement result of xitix are as shown in table 2.
Table 2
Embodiment 12-19
Prepare gold nanorods solution according to the method for embodiment 3, but the amount of the sulfuric acid added is different, addition and the correlation parameter measurement result of sulfuric acid are as shown in table 3.
Comparative example 12-19
Gold nanorods solution is prepared according to the method for comparative example 3, but the amount of the sulfuric acid added is different, addition and the correlation parameter measurement result of sulfuric acid are as shown in table 3, in table 3, "--" expression does not form gold nanorods, UV-visible-near infrared absorption figure is a curve not having obvious peak shape, therefore does not do further statistics.
Table 3
As can be seen from above-described embodiment and comparative example, the LSPR peak position of the gold nanorods that the present invention prepares is adjustable between 645-800nm, length-to-diameter ratio in 2.3 ± 0.3 to 3.7 ± 0.4 scope, FWHM value within the scope of 0.20-0.22eV, A
lSPR/ A
tSPRvalue is greater than 2.3, and the gold nanorods size monodisperse obtained is good and quality is high.
As can be seen from embodiment 5-11 and comparative example 5-11, no matter Cu
2+whether exist, present the trend of blue shift after first red shift with the increase LSPR peak position of amount of adding AA, high density AA causes the particle of spheroidal particle and other shapes significantly to increase.When not adding cupric chloride, the FWHM value of gold nanorods obtained under the AA of high density is minimum; When adding cupric chloride, the quality of gold nanorods is all improved in varying degrees, and when lower AA concentration, FWHM value can reach 0.19eV, improves more obvious.
As can be seen from embodiment 12-19 and comparative example 12-19, when not adding cupric chloride, adding of acid makes the FWHM value of gold nanorods increase; When adding cupric chloride, with the increase of the amount of the acid added, LSPR peak position presents blue shift trend, and FWHM value first reduces to increase afterwards, when acid concentration is higher, cannot form gold nanorods.But at specific Cu
2+under the condition of concentration and acid concentration, high-quality gold nanorods can be obtained.
Below the preferred embodiment of the present invention is described in detail by reference to the accompanying drawings; but; the present invention is not limited to the detail in above-mentioned embodiment; within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method of a gold nanorods, the method comprises gold nanorods growth solution to plant with Jin Jing and mixes, mixing gained mixture is placed under the condition of golden seeded growth to make described golden seeded growth, described gold nanorods growth solution contains tensio-active agent, reductive agent, tetra chlorauric acid and soluble silver salt, it is characterized in that, described gold nanorods growth solution is also containing soluble copper salt, and the Jin Jing's kind relative to every mole, the add-on of soluble copper salt is 16-400mol.
2. method according to claim 1, wherein, the Jin Jing's kind relative to every mole, the add-on of soluble copper salt is 50-267mol.
3. method according to claim 1 and 2, wherein, described soluble copper salt is one or more in cupric chloride, copper sulfate and cupric nitrate.
4. method according to claim 1, wherein, Jin Jing's kind relative to every mole, the add-on of described tensio-active agent, reductive agent, tetra chlorauric acid and soluble silver salt is respectively 125000-208334mol, 920-1334mol, 831-835mol and 33-250mol.
5. the method according to claim 1 or 4, wherein, described tensio-active agent is cetyl trimethylammonium bromide, and described reductive agent is sodium borohydride and/or POTASSIUM BOROHYDRIDE, and described soluble silver salt is Silver Nitrate.
6. method according to claim 1, wherein, the concentration that in described mixture, Jin Jing plants is 0.2-0.3mM.
7. method according to claim 1, wherein, in described mixture, the concentration of described soluble silver salt is 30-50 μM, and the concentration of described soluble copper salt is 150-200 μM; Or the concentration of described soluble silver salt is 60-100 μM, the concentration of described soluble copper salt is 50-120 μM.
8. method according to claim 1, wherein, also containing acid in described gold nanorods growth solution, described acid is sulfuric acid and/or hydrochloric acid, the Jin Jing's kind relative to every mole, and with pH meter, the add-on of described acid is 8332-58334mol.
9. method according to claim 1, wherein, making the condition of described golden seeded growth comprise temperature is 25-35 DEG C, and the time is 12-16h.
10. a gold nanorods, it is characterized in that, described gold nanorods is prepared by the method in claim 1-9 described in any one, the length-to-diameter ratio of described gold nanorods is in 2.3 ± 0.3 to 3.7 ± 0.4 scope, the half-value width of long wave surface plasmon resonance absorption peak is 0.20-0.22eV, and the ratio that long wave surface plasmon resonance absorption peak position and shortwave surface plasmon resonance absorb peak position absorption value is 2.3-4.9.
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| CN103962545B (en) * | 2013-01-30 | 2016-06-15 | 国家纳米科学中心 | A kind of processing method of nanometer rods |
| CN103487378B (en) * | 2013-10-09 | 2016-06-15 | 国家纳米科学中心 | A kind of circular dichroism based on gold nanorod aggregation detects the method for DNA |
| CN105618730B (en) * | 2014-10-28 | 2018-03-13 | 深圳先进技术研究院 | A kind of preparation method of small size gold nanorods |
| CN106770049B (en) * | 2016-12-22 | 2020-04-14 | 南京邮电大学 | Method for constructing Dolmen structure based on DNA paper folding template and nano gold rod |
| CN107252896B (en) * | 2017-06-15 | 2018-12-04 | 山东大学 | A kind of synthetic method of monodisperse thorn-like gold nano grain |
| US10758983B1 (en) | 2018-04-17 | 2020-09-01 | Government Of The United States, As Represented By The Secretary Of The Air Force | Concentrated synthesis of monodispersed gold nanorods |
| CN111659903B (en) * | 2020-07-14 | 2022-10-21 | 国家纳米科学中心 | Gold nanorod and preparation method thereof |
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