CN104308179A - Method for quickly preparing high-yield gold triangular nanoprisms - Google Patents
Method for quickly preparing high-yield gold triangular nanoprisms Download PDFInfo
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Abstract
The invention relates to a method for quickly preparing high-yield gold triangular nanoprisms. The method comprises the following steps of adding chloroauric acid solution and soluble iodide ion solution into a cationic surface active agent, namely quaternary ammonium chloride solution, taking ascorbic acid as a reducing agent, and adding aqueous alkali to regulate a pH value to induce the growth of the gold triangular nanoprisms with ascorbic acid as a reducing agent . According to the method for synthesizing the gold triangular nanoprisms, the gold triangular nanoprisms can be prepared in a very short time (about eight minutes), while for seed growth method-based synthesis of the gold triangular nanoprisms, synthesis steps are complicated, conditions are not easy to control, the repeatability is poor and three to four hours are required for completing the growth of the gold triangular nanoprisms. Therefore, the method has the advantages that the time for synthesizing the gold triangular nanoprisms is greatly shortened, the yield and the morphology uniformity of the obtained gold triangular nanoprisms are improved, the sizes of the gold triangular nanoprisms are adjustable, and a foundation is provided for widely applying the gold nanoprisms.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of fast preparation method of high yield gold nano triangular plate.
Background technology
When the size of material narrows down to below 100 nanometers, due to the appearance of quantum effect, small-size effect and skin effect etc., nano material can present the distinct excellent properties with body phase material in all many-sides such as mechanics, optics, magnetics.Such as, for gold, silver nano material, because it has very excellent surface plasma resonance (Surface plasmon resonance, SPR) character, has thus shown huge application potential in fields such as catalysis, information storage, nanosecond medical science, bio-sensing, photothermal technique and image enhancements.Research shows, the SPR effect of noble metal nanometer material and the pattern of metal material itself and size closely related, the controlledly synthesis how realizing noble metal nanometer material is the key realizing its application.In the past few decades, although people have developed the multiple method preparing noble metal nano particles, but still have many problems demand to solve, such as synthesis mechanism is unclear, productive rate is lower, poor repeatability, cannot synthesize on a large scale, and these problems seriously constrain the large-scale application of nano material.As modal noble metal, synthesis and the application of gold nano-material have been a great concern always, up to the present, people can prepare the gold nano grain of different-shape, such as gold nanorods, nanowires of gold, gold nano band, gold nano cube, gold-nano-piece etc.Wherein gold nano triangular plate is very typical two-dimensional structure, the SPR effect very strong because of its three summits place and having been a great concern.In the time of more than ten years in the past, people are devoted to the synthesis of gold-nano-piece and the research of application always, have developed multiple synthetic method at present to prepare gold nano triangular plate.2004, Murali Sastry prepared the gold nano grain of triangular plate shape by lemon grass extract reduction chloroaurate based on bioanalysis.Subsequently, Mirkin seminar uses seed-mediated growth to synthesize the homogeneous gold nano triangular plate of shape, and achieves the size regulation and control of gold nano triangular plate.Develop again electrochemistry, hydro-thermal and photocatalysis method synthesis gold nano triangular plate subsequently gradually.But the general size of gold nano triangular plate that these synthetic methods obtain comparatively large (being greater than 100nm) and productive rate lower (lower than 40).2014, Luis M.Liz-Marz á n seminar obtains higher yields by the purification of products obtained by the seed-mediated growth of improvement and the gold nano triangular plate of size uniformity, but formed without still there being a large amount of erose nano particles in the product of purifying, and also there is complex steps in seed synthetic method, experimental repeatability and the shortcoming such as poor controllability, length consuming time, therefore developing a kind of efficient synthetic method is fast the basis of the practical application realizing triangle gold-nano-piece.
Summary of the invention
The object of this invention is to provide one and greatly shorten gold nano triangular plate generated time, and improve the quick method preparing gold nano triangular plate of gold nano triangular plate productive rate.
For reaching this technical purpose, the technical solution used in the present invention is:
A kind of fast preparation method of high yield gold nano triangular plate, in cationic surfactant quaternary ammonium chloride salting liquid, adding tetra chlorauric acid solution and iodine soluble solion, is reducing agent with ascorbic acid, adds aqueous slkali and regulates acid-base value to induce the growth of gold nano triangular plate.
The adjust ph that is adjusted to of described acid-base value is 7 ~ 8.
Fast preparation method of the present invention, preferably, concrete steps comprise:
(1) growth solution is prepared: in cationic surfactant quaternary ammonium chloride salting liquid, add tetra chlorauric acid solution, iodine soluble solion and aqueous slkali successively, rock and make it mix, make growth solution;
(2) growth of gold nano triangular plate: add ascorbic acid solution in the growth solution described in step (1), until solution by faint yellow fade to colourless after, then add aqueous slkali, adjust ph is 7 ~ 8, manually rocks 1-2 second, leaves standstill.
Above-mentioned quaternary ammonium chloride is preferably hexadecyltrimethylammonium chloride.
Above-mentioned iodine soluble solion is preferably liquor kalii iodide or IodineSodium Solution.
Above-mentioned aqueous slkali is preferably sodium hydroxide solution or potassium hydroxide solution.
According to a specific embodiment of the present invention, the most preferred step of one of fast preparation method of the present invention comprises:
(1) the hexadecyltrimethylammonium chloride solution of 1.6mL, 0.1M is pipetted in the ultra-pure water of 8mL, add the tetra chlorauric acid solution of 80 μ L, 25.4mM successively, the liquor kalii iodide of 75 μ L, 0.01M, and then the sodium hydroxide solution of 20.3 μ L, 0.1M is added, rock and make it mix, make growth solution;
(2) in growth solution, add the ascorbic acid solution of 100 μ L, 64mM, rock to reaction even, obtain colourless transparent solution; Add the sodium hydroxide solution of 5 μ L, 0.1M again, manually evenly rock 1-2 second, then left standstill.
Based on the above method, the present invention has prepared the gold nano triangular plate product of high yield.Wherein gold nano triangular plate productive rate is high, can reach more than 90%, and wherein spheric granules content is few, is less than 10%.This method can control by regulating the amount of ascorbic acid and the adjustment of acid-base value the gold nano triangular plate obtaining different size, and regulate size between 40-120nm, the dimensional homogeneity of the gold nano triangular plate at every turn prepared is good.
Technique effect of the present invention is:
The quick method preparing gold nano triangular plate of the present invention; adopt one step growth method; use cationic surfactant quaternary ammonium chloride as protective agent; in tetra chlorauric acid solution; by the booster action of iodide ion; taking ascorbic acid as reducing agent, regulating solution ph by adding aqueous slkali, induction gold-nano-piece Fast back-projection algorithm.Compare with traditional synthetic method, the method of synthesis gold nano triangular plate of the present invention can complete in the very short time (about 8 minutes), and use the synthesis of the gold nano triangular plate based on seed mediated growth method, usual synthesis step is loaded down with trivial details, condition is wayward, poor repeatability, and need the growth completely that just can complete gold nano triangular plate for 3 to 4 hours.Therefore this method not only substantially reduces the generated time of gold nano triangular plate, and the gold-nano-piece productive rate obtained and topography uniformity are obtained for raising, and size adjustable, for the extensive use of gold-nano-piece provides the foundation.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of description, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is the procedure schematic diagram of quick preparation gold nano triangular plate of the present invention;
Fig. 2 is the uv absorption spectra of gold nano triangular plate in growth course of the embodiment of the present invention 1;
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of the gold nano triangular plate of different size prepared by the embodiment of the present invention 2;
Fig. 4 is the transmission electron microscope figure of the gold nano triangular plate of different size prepared by the embodiment of the present invention 2 respectively.
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
See Fig. 1; the fast preparation method of high yield gold nano triangular plate of the present invention uses cationic surfactant quaternary ammonium chloride as protective agent, in tetra chlorauric acid solution; by the booster action of iodide ion, add ascorbic acid and tervalence gold ion is reduced into monovalence gold ion.Finally by the growth of aqueous slkali rapid induction gold nano triangular plate.Compare with traditional synthetic method, method of the present invention only needs the time of about 8 minutes can complete the synthesis of gold nano triangular plate, not only substantially reduce the generated time of gold nano triangular plate, for the practical application of gold nano triangular plate provides material base, and the gold nano triangular plate productive rate obtained is high, spherical particle is few.The method generated time is short, easily implements, and has great industry using value.By the size dimension regulating the value of ascorbic acid and acid-base value to regulate the gold nano triangular plate obtained, specific embodiment is:
Embodiment 1
In the present embodiment, quaternary ammonium chloride is hexadecyltrimethylammonium chloride, and iodine soluble solion is liquor kalii iodide, and aqueous slkali is sodium hydroxide solution.Step is:
(1) 1.6mL (0.1M) cationic surfactant quaternary ammonium chloride is pipetted in the ultra-pure water of 8mL, add 80 μ L (25.4mM) tetra chlorauric acid solution, add the liquor kalii iodide of 75 μ L (0.01M) subsequently, and then adding 20.3 μ L (0.1M) sodium hydroxide solutions, rocking to mixing.
(2) add 100 μ L (64mM) reducing agent ascorbic acid solutions in the solution obtained in step (1), rock to reaction evenly, obtain colourless transparent solution.And then add 5 μ L (0.1M) sodium hydroxide solutions, rock and within 1 ~ 2 second, make it even, leave standstill subsequently and treat that it reacts.
The growth change of the gold nano triangular plate adopting the gold nano triangular plate synthetic method of the present embodiment to prepare in CTAC as shown in Figure 2, can find out, at first 2 ~ 3 minutes, gold-nano-piece ramp, and the speed of growth slows down gradually in the time subsequently, finally reach home reaction in about 8 minutes, obtain the gold nano triangular plate of 90% productive rate.
Note: the concentration in above-mentioned bracket is the solubility adding solution.
Embodiment 2:
In the present embodiment, by regulating the amount of the ascorbic acid of 64mM between 60 μ L ~ 160 μ L, and the amount of the alkali of 0.1M needed for minimizing induced reaction is between 10 μ L ~ 5 μ L, and regulation and control obtain the gold nano triangular plate of different size.
Fig. 3 is the ultraviolet-visible absorption spectroscopy comparison diagram of the gold nano triangular plate of different size prepared by the present embodiment.As can be seen from Figure 3, the gold nano triangular plate characteristic plasma formant with different size be 620nm to 700nm not etc., show that the size of gold-nano-piece determines its SPR character.Fig. 4 a-4f is the transmission electron microscope figure of the gold nano triangular plate of different size prepared by the present embodiment respectively.
Can find out in conjunction with above-described embodiment, the fast preparation method of high yield gold nano triangular plate of the present invention, whole building-up process only needs the time of about 8 minutes, compare with prior synthesizing method, not only highly shortened generated time, and effectively improve the productive rate of gold-nano-piece, for the practical application of gold-nano-piece provides material base.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (10)
1. the fast preparation method of a high yield gold nano triangular plate, it is characterized in that: in cationic surfactant quaternary ammonium chloride salting liquid, add tetra chlorauric acid solution and iodine soluble solion, be reducing agent with ascorbic acid, add aqueous slkali and regulate acid-base value to induce the growth of gold nano triangular plate.
2. fast preparation method according to claim 1, is characterized in that: described adjustment acid-base value is adjust ph is 7 ~ 8.
3. fast preparation method according to claim 1 and 2, is characterized in that: comprise step:
(1) growth solution is prepared: in cationic surfactant quaternary ammonium chloride salting liquid, add tetra chlorauric acid solution, iodine soluble solion and aqueous slkali successively, rock and make it mix, make growth solution;
(2) growth of gold nano triangular plate: add ascorbic acid solution in the growth solution described in step (1), until solution by faint yellow fade to colourless after, then add aqueous slkali, adjust ph is 7 ~ 8, manually rocks 1-2 second, leaves standstill.
4. the fast preparation method according to claim 1 or 2 or 3, is characterized in that: described quaternary ammonium chloride is hexadecyltrimethylammonium chloride.
5. the fast preparation method according to claim 1 or 2 or 3, is characterized in that: described iodine soluble solion is liquor kalii iodide or IodineSodium Solution.
6. the fast preparation method according to claim 1 or 2 or 3, is characterized in that: described aqueous slkali is sodium hydroxide solution or potassium hydroxide solution.
7. fast preparation method according to claim 3, is characterized in that: comprise step:
(1) the hexadecyltrimethylammonium chloride solution of 1.6mL, 0.1M is pipetted in the ultra-pure water of 8mL, add the tetra chlorauric acid solution of 80 μ L, 25.4mM successively, the liquor kalii iodide of 75 μ L, 0.01M, and then the sodium hydroxide solution of 20.3 μ L, 0.1M is added, rock and make it mix, make growth solution;
(2) in growth solution, add the ascorbic acid solution of 100 μ L, 64mM, rock to reaction even, obtain colourless transparent solution; Add the sodium hydroxide solution of 5 μ L, 0.1M again, manually evenly rock 1-2 second, then left standstill.
8. the gold nano triangular plate product for preparing of claim 1-7 either method.
9. gold nano triangular plate product according to claim 8, is characterized in that: wherein the productive rate of gold nano triangular plate is more than 90%, is wherein less than 10% containing spheric granules.
10. gold nano triangular plate product according to claim 8, is characterized in that: wherein gold nano triangular plate size uniformity, size is between 40-120nm.
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Cited By (14)
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| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
| CN106860864A (en) * | 2017-01-10 | 2017-06-20 | 中国人民解放军南京军区南京总医院 | A kind of mesoporous organosilicon gold nano triangular plate composite for loading sensitising agent and preparation method thereof, application |
| CN107199349A (en) * | 2016-03-17 | 2017-09-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of simple and quick method for preparing gold nano star |
| CN108031860A (en) * | 2017-12-04 | 2018-05-15 | 浙江工业大学 | Preparation method of nano gold triangular plate |
| CN108788177A (en) * | 2018-06-18 | 2018-11-13 | 上海大学 | The preparation method of gold nano grain |
| CN109324045A (en) * | 2018-11-12 | 2019-02-12 | 安庆师范大学 | A kind of kit and its detection method of quick detection Cadmium In The Water Body ion |
| CN109837531A (en) * | 2017-11-27 | 2019-06-04 | 重庆科技学院 | Gold nano triangle piece preparation method with surface-enhanced Raman effects |
| CN110186858A (en) * | 2019-06-20 | 2019-08-30 | 盐城工学院 | A method of detection cysteine |
| CN110340375A (en) * | 2018-04-03 | 2019-10-18 | 中国科学院青岛生物能源与过程研究所 | A method of preparing mm-scale two dimension monocrystalline gold plaque |
| CN112972690A (en) * | 2021-02-22 | 2021-06-18 | 上海交通大学医学院附属第九人民医院 | Triangular nano-gold-based carrier, preparation method and application |
| CN113695584A (en) * | 2021-08-18 | 2021-11-26 | 杭州师范大学 | Method for rapidly synthesizing high-purity gold nano triangular plate |
| CN113828790A (en) * | 2021-08-25 | 2021-12-24 | 海南大学 | Preparation method of gold and core-shell nanocrystal thereof |
| CN114210994A (en) * | 2021-12-17 | 2022-03-22 | 中红外激光研究院(江苏)有限公司 | Preparation method of gold nanodisk |
| CN115740481A (en) * | 2022-11-17 | 2023-03-07 | 江苏师范大学 | Method for synthesizing flaky nano gold particles |
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| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
| CN107199349B (en) * | 2016-03-17 | 2019-10-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of method of simple and quick preparation gold nano star |
| CN107199349A (en) * | 2016-03-17 | 2017-09-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of simple and quick method for preparing gold nano star |
| CN106860864A (en) * | 2017-01-10 | 2017-06-20 | 中国人民解放军南京军区南京总医院 | A kind of mesoporous organosilicon gold nano triangular plate composite for loading sensitising agent and preparation method thereof, application |
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| CN108031860A (en) * | 2017-12-04 | 2018-05-15 | 浙江工业大学 | Preparation method of nano gold triangular plate |
| CN108031860B (en) * | 2017-12-04 | 2021-04-06 | 浙江工业大学 | Preparation method of nano gold triangular plate |
| CN110340375A (en) * | 2018-04-03 | 2019-10-18 | 中国科学院青岛生物能源与过程研究所 | A method of preparing mm-scale two dimension monocrystalline gold plaque |
| CN108788177A (en) * | 2018-06-18 | 2018-11-13 | 上海大学 | The preparation method of gold nano grain |
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| CN112972690A (en) * | 2021-02-22 | 2021-06-18 | 上海交通大学医学院附属第九人民医院 | Triangular nano-gold-based carrier, preparation method and application |
| CN113695584A (en) * | 2021-08-18 | 2021-11-26 | 杭州师范大学 | Method for rapidly synthesizing high-purity gold nano triangular plate |
| CN113695584B (en) * | 2021-08-18 | 2023-04-07 | 杭州师范大学 | Method for rapidly synthesizing high-purity gold nano triangular plate |
| CN113828790A (en) * | 2021-08-25 | 2021-12-24 | 海南大学 | Preparation method of gold and core-shell nanocrystal thereof |
| CN113828790B (en) * | 2021-08-25 | 2024-05-14 | 海南大学 | Gold and preparation method of core-shell nanocrystalline thereof |
| CN114210994A (en) * | 2021-12-17 | 2022-03-22 | 中红外激光研究院(江苏)有限公司 | Preparation method of gold nanodisk |
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Inventor after: Ji Fei Inventor after: Zhang Qiao Inventor after: Chen Lei Inventor after: Xu Yong Inventor after: Mi Yifan Inventor after: Sun Baoquan Inventor after: Ye Xingchen Inventor after: Zhang Xiaohong Inventor before: Zhang Qiao Inventor before: Chen Lei Inventor before: Ji Fei Inventor before: Xu Yong Inventor before: Mi Yifan Inventor before: Sun Baoquan Inventor before: Ye Xingchen Inventor before: Zhang Xiaohong |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: ZHANG QIAO CHEN LEI JI FEI XU YONG MI YIFAN SUN BAOQUAN YE XINGCHEN ZHANG XIAOHONG TO: JI FEI ZHANG QIAO CHEN LEI XU YONG MI YIFAN SUN BAOQUAN YE XINGCHEN ZHANG XIAOHONG |
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| CB03 | Change of inventor or designer information |
Inventor after: Zhang Qiao Inventor after: Chen Lei Inventor after: Ji Fei Inventor after: Xu Yong Inventor after: Mi Yifan Inventor after: Sun Baoquan Inventor after: Ye Xingchen Inventor after: Zhang Xiaohong Inventor before: Ji Fei Inventor before: Zhang Qiao Inventor before: Chen Lei Inventor before: Xu Yong Inventor before: Mi Yifan Inventor before: Sun Baoquan Inventor before: Ye Xingchen Inventor before: Zhang Xiaohong |
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| COR | Change of bibliographic data | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150128 |
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| RJ01 | Rejection of invention patent application after publication |