CN102233434A - Method for preparing nano/micron gold hierarchical structure material - Google Patents
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Abstract
The invention discloses a method for preparing a gold hierarchical structure material. In the method, the nano/micron gold hierarchical structure material is prepared by reducing chloroauric acid at normal temperature, wherein a 'dendritic' surfactant C18N3 serves as a template and protective agent; and ascorbic acid serves as a reducing agent. Bubbles formed by the surfactant C18N3 serve as the template; and a C18N3 protected stable gold nano hierarchical structure is obtained through reduction by using the ascorbic acid. Compared with the conventional method, the method is simple and low in cost; and the hierarchical structure prepared by the method has high monodispersity, controllable appearance and the like. The nano/micron gold hierarchical structures with different appearances can be obtained by simply adjusting the amount of the surfactant, the chloroauric acid and the ascorbic acid, and comprise three-dimensional gold nanostructures such as a gold nanocrystal with a plurality of protrusions on the surface, nearly spherical hollow nanoparticles, a meatball-shaped structure, a spherical structure with rodlike protrusions on the surface, a nano/micron spherical structure with sheet-like surface and the like.
Description
Technical field
The present invention relates to a kind of method for preparing Nano/micron level gold grading structure material.
Background technology
In recent years, because noble metal micron and nano material have peculiar property and wide potential application foreground at aspects such as optics, electricity, acoustics, magnetics and mechanics, micro-nano noble metal synthesizes and has prepared concern widely.The nanometer hierarchy is the novel nano structural material that occurred in recent years, owing to have multi-level, various dimensions, multi-component coupling and cooperative effect, grading structure material becomes the strongest carrying person who satisfies the material demand for development undoubtedly.On broad sense, grading structure material had both comprised the two dimension of polyhedron (as polypody shape, starlike etc.), zero dimension or the 1-dimention nano particle of special construction, three-dimensional super the arrangement, the specific form multilevel hierarchy of nanometer primitive by interacting and forming that also comprises given shape is as nucleocapsid structure, junction structure and branched structure etc.The noble metal nano hierarchy all has potential application prospect at aspects such as catalysis, surface Raman enhancement, biologies, therefore enjoys chemist and physicist's concern.Because the character of noble metal micron and nano material determines pattern and size with itself to a great extent, the noble metal micron and the nano material of therefore synthetic pattern, controllable size have become a very important problem.Along with the development of nanometer science and technology, people have invented the method for many synthetic noble metal nano hierarchies, have summarized nanometer star and nanometer golden flower at the application aspect the surface Raman enhancement (Giannini, V. as S á nchez-Gil etc.; Rodr í guez-Oliveros, R.; S á nchez-Gil, J., Surface Plasmon Resonances of Metallic Nanostars/Nanoflowers for Surface-Enhanced Raman Scattering.Plasmonics 2010,5 (1), 99-104.); Rogach etc. have summarized the preparation of nanostructured colloid chemistry method (Sau, the T.K. of non-sphere; Rogach, A.L., Nonspherical Noble Metal Nanoparticles:Colloid-Chemical Synthesis and Morphology Control.Adv.Mater.2010,22 (16), 1781-1804.); Yang etc. have reported and have utilized prepared by electrodeposition gold/platinum bimetal nano golden flower (Qian, L.; Yang, X., Polyamidoamine Dendrimers-Assisted Electrodeposition of Gold-Platinum Bimetallic Nanoflowers.The Journal of Physical Chemistry B 2006,110 (33), 16672-16678.); Daniel etc. have reported synthesis of nano golden flower and the application aspect living imaging (Xie, J.; Zhang, Q.; Lee, J.Y.; Wang, D.I.C., The Synthesis of SERS-Active Gold Nanoflower Tags for In Vivo Applications.ACS Nano 2008,2 (12), 2473-2480.); Retna etc. have reported under the room temperature, fluorogold nm of gold floral structure (Jena, the B.K. of synthetic single crystal under the condition that does not have surfactant and seed; Raj, C.R., Seedless, Surfactantless Room Temperature Synthesis of Single Crystalline Fluorescent Gold Nanoflowers with Pronounced SERS and Electrocatalytic Activity.Chemistry of Materials 2008,20 (11), 3546-3548.); Peng etc. utilize the seed law to prepare stabilized nano golden flower (Zhao, L.; Ji, X.; Sun, X.; Li, J.; Yang, W.; Peng, X., Formation and Stability of Gold Nanoflowers by the Seeding Approach:The Effect of Intraparticle Ripening.The Journal of Physical Chemistry C 2009,113 (38), 16645-16651.); Liu etc. utilize the Gemini surfactant to induce and produce nanometer golden flower (Zhong, L.; Zhai, X.; Zhu, X.; Yao, P.; Liu, M., Vesicle-Directed Generation of Gold Nanoflowers by Gemini Amphiphiles and the Spacer-Controlled Morphology and Optical Property.Langmuir 2009,26 (8), 5876-5881.); Halas etc. have prepared meat ball-type nm of gold structure, and have carried out Raman and strengthen research and obtained very high enhancer (Wang, H.; Halas, N.J., Mesoscopic Au " Meatball " Particles.Adv.Mater.2008,20 (4), 820-825.); Huang etc. have reported and have utilized seed hair tonic preparation band ramiform and star-like nano hierarchy (Wu, H.-L.; Chen, C.-H.; Huang, M.H., Seed-Mediated Synthesis of Branched Gold Nanocrystals Derived from the Side Growth of Pentagonal Bipyramids and the Formation of Gold Nanostars.Chemistry of Materials 2008,21 (1), 110-114.).But there is the preparation process complexity in above method, and productive rate is less, shortcomings such as monodispersity difference.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing golden grading structure material.
The method of the golden grading structure material of preparation provided by the present invention is to use " branch " shape amphiphile, amphiphilic molecule C18N3 (two (amino-ethyl acyl Methylethyl) octadecylamine) as template and protective agent; utilize ascorbic acid to be reducing agent; make gold chloride carry out reduction reaction, obtain Nano/micron gold grading structure material.
The method is simple to operate, the controlled nanometer hierarchy of preparation pattern under the normal temperature condition, in the short time, and synthesis of nano utilizes the nm of gold structure and morphology of the method preparation to stablize good reproducibility to micron-sized golden hierarchy in a large number.
Applied amphiphile, amphiphilic molecule C18N3 among the present invention (two (amino-ethyl acyl Methylethyl) octadecylamine) is according to document (Wang, W.; Lu, W.S.; Jiang, L.Influence of pH on the Aggregation Morphology of a Novel Surfactant with Single Hydrocarbon Chain and Multi-Amine Headgroups.J.Phys.Chem.B.2008,112,1409-1413) prepare, method is simple, the productive rate height.
Application of the present invention " branch " type surfactant molecule C18N3 (two (amino-ethyl acyl Methylethyl) octadecylamine) prepares the method for Nano/micron gold hierarchy; it is that both agent prepared the hollow gold nanometer ball as template by amphiphile, amphiphilic molecule C18N3, and the while obtains grading structure material as the two-step method preparation of protective agent growth surface topology again.This method can be synthesized the gold nano hierarchy of various topological structures, and the surperficial branch of this hierarchy and projection all are monocrystalline, and it comprises structures such as bar-shaped, sheet and taper; The size of gold nano structure can be regulated from the nanometer to the micron.And resulting separation structure monodispersity is good, the productive rate height.
The present invention prepares the method for golden grading structure material, specifically comprise the steps: at ambient temperature, in the C18N3 aqueous solution of concentration, add gold chloride, ascorbic acid successively greater than the C18N3 critical micelle concentration, then with still aging at least 1 hour of mixed solution, centrifugal (rotating speed can be 3000-6000r/min), washing (available second distillation water washing), remove unnecessary C18N3, obtain described golden grading structure material.
The mol ratio of C18N3, gold chloride and ascorbic acid can be (0.245-2.45) in the described mixed solution: (1.44-7.2): (5-7).The concentration of C18N3 should be greater than the C18N3 critical micelle concentration in the described mixed solution.
The size of the golden grading structure material that the present invention is prepared can be regulated between the micron order at nanoscale.
Prepared golden grading structure material is a three-dimensional hierarchical structure, and it comprises: the gold nanocrystals of surperficial many projections, burger type, surface are for the ball-type structure of baculum and surperficially be the Nano/micron golden flower structure of sheet.
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in reaction system: (1.44-3.36): 5, and preferred molar ratio is 1.225: 1.44: 5, the golden grading structure material of gained is the burger type;
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in the reaction system of reaction: (3.36-3.84): (5-7), preferred molar ratio is 1.225: 3.36: 5 or 1.225: 3.84: (6-7); The golden grading structure material of gained is that the surface is the ball-type structure of baculum;
The mol ratio of C18N3, gold chloride and ascorbic acid is (0.245-1.47) in the reaction system of reaction: (3.84-7.2): 5; The golden grading structure material of gained is that the surface is the Nano/micron golden flower structure of sheet;
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in the reaction system of reaction: (0.48-1.44): 5; The golden grading structure material of gained is the gold nanocrystals of surperficial many projections.
The particle diameter of described burger type structure can be 200-300nm;
Described surface be the ball-type structure of baculum or surface for the particle diameter of ball-type in the Nano/micron golden flower structure of sheet be 200-1000nm; Described surface is that the length of protrusion of surface is 50-100nm in the ball-type structure of baculum, and the diameter of projection is 20-50nm; Described surface is that the thickness of surperficial sheet is 20-50nm in the Nano/micron golden flower structure of sheet.
By the mol ratio of gold chloride/C18N3 in the conditioned reaction system, can obtain the gold nano structure of multiple pattern; Mol ratio as C18N3/ gold chloride/ascorbic acid is: 1.225: 3.84: 5, it was scattered to obtain list, and the surface that productive rate is high is the nm of gold floral structure of sheet.
By regulating the ratio of gold chloride/ascorbic acid, the fixing amount of gold chloride, increase the amount of ascorbic acid, (particle diameter is 200nm～1000nm), and ascorbic acid is increased to the gold nano structure that obtains surperficial different projections after a certain amount of can to obtain the nanometer golden flower on the sheet surface of different sizes.
The present invention uses to have that condition is simple, easy to operate, product purity is high, monodispersity good and the colloid chemistry method of advantage such as surface texture is controlled, under normal temperature condition, prepares the nm of gold structure of kinds of surface topological structure.Resulting nm of gold structure can be passed through the capable adjusting of concentration ratio of surfactant/gold chloride/ascorbic acid, can obtain different sizes, the golden hierarchy of different surfaces topology.Because this method is to utilize C18N3 under normal temperature condition this " " the shape amphiphile, amphiphilic molecule is a template to branch, and the nm of gold structure monodispersity of preparation is good, and pattern is controlled.Surperficial branch and projection with the gold nano hierarchy of the synthetic Nano/micron level of the inventive method all are monocrystalline, and it comprises structures such as bar-shaped, sheet and taper.
The inventive method is compared with the existing method for preparing gold nano/micron grading structure material, have following advantage: normal temperature condition gets final product down, simple to operate, without any need for adding material, with low cost, the product productive rate is high and can synthesize in a large number, concentration ratio by reconciliation statement surface-active agent/gold chloride/ascorbic acid, can obtain the golden hierarchy of the nanometer of kinds of surface topology to micron, easy reaction, eliminated the influence of additional substances such as salt, can be good at realizing artificial adjustment the product surface topology.
Description of drawings
Fig. 1 (a) adds the sem photograph that 30 μ L aqueous solution of chloraurate obtain product among the embodiment 1, be burger type hollow-core construction as can be seen.
Fig. 1 (b) adds the sem photograph that 70 μ L aqueous solution of chloraurate obtain product among the embodiment 1, be that the surface is the gold nano structure of baculum structure as can be seen.
Fig. 1 (c) adds the sem photograph that 80 μ L aqueous solution of chloraurate obtain product among the embodiment 1, the surface that is monodispersed submicron order as can be seen is the gold nano hierarchy of laminated structure.
Fig. 1 (d) executes to add the transmission electron microscope picture that 80 μ L aqueous solution of chloraurate obtain product in the example 1, can be clear that the sheet topological structure on nanometer golden flower surface.
Fig. 2 is the sem photograph and the dynamic light scattering statistical chart of monodispersity of Jenner's popped rice of the sheet surface topology that obtains of embodiment 1.
Fig. 3 is the high-resolution-ration transmission electric-lens picture of Jenner's popped rice of the sheet surface topology that obtains of embodiment 1.
Fig. 4 is the stereoscan photograph of embodiment 2 products, as can be seen from the figure arrive the golden hierarchy of different topology.
Fig. 5 is the sem photograph of embodiment 3 products, is surperficial many projections gold nanocrystals as can be seen.
Fig. 6 is the sem photograph of embodiment 4 products, can obtain the nanometer golden flower of different surfaces topology density.
Fig. 7 is the sem photograph of embodiment 5 products, can obtain micron order golden flower.
Fig. 8 (a) is the XRD diffracting spectrum of the surperficial sheet structure nano golden flower of embodiment 1 preparation, (b) high-resolution of nanometer golden flower surface patch shape structure projection Electronic Speculum picture, and illustration is a SEAD, the gold that the surface patch shape can be described is a monocrystalline.
The specific embodiment
Below by specific embodiment method of the present invention is described, but the present invention is not limited thereto.
Experimental technique described in the following embodiment if no special instructions, is conventional method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Applied surfactant amphiphile, amphiphilic molecule C18N3 among the following embodiment (two (amino-ethyl acyl Methylethyl) octadecylamine) is according to document (Wang, W.; Lu, W.S.; Jiang, L.Influence of pH on the Aggregation Morphology of a Novel Surfactant with Single Hydrocarbon Chain and Multi-Amine Headgroups.J.Phys.Chem.B.2008,112,1409-1413) prepare, method is simple, the productive rate height.
Embodiment 1, preparation burger type, surperficial many projections type and surface are the ball-type gold grading structure material of laminated structure
(1) C18N3 is dissolved in the redistilled water, preparation obtains the C18N3 aqueous solution of 0.5mM.
(2) at ambient temperature, in the 2.45mL C18N3 aqueous solution, add the aqueous solution of chloraurate of 30 μ L (or 70 μ L or 80 μ L) mass concentration 2% (48mM), make that gold chloride concentration is 0.58Mm (or 1.33mM, 1.52mM) in the mixed solution
(3) the rapid aqueous ascorbic acid that adds 0.25mL (20mM) behind the above-mentioned mixed solution mixing 30s, light shaking left standstill 1 hour.
(4) with above-mentioned product solution centrifugal 5min under the rotating speed of 3000r/min, remove supernatant, with sedimentation products second distillation water washing.So circulation is 3 times.
(5) each sample with centrifuge washing drips on the silicon chip drying at room temperature.Add the product of 30 μ L aqueous solution of chloraurate preparation, its pattern is a burger type structure, and stereoscan photograph is seen Fig. 1 (a).From Fig. 1 (b)-(d) as can be seen, by changing the nm of gold structure that gold chloride concentration in the reaction system can obtain the kinds of surface topology, add 70 μ L aqueous solution of chloraurate, the product pattern be the surperficial gold nano structure of baculum structure that is; Add 80 μ L aqueous solution of chloraurate, the product pattern is that the surface of submicron order is the gold nano hierarchy of laminated structure.Fig. 2 is the sem photograph and the dynamic light scattering statistics of monodispersity of Jenner's popped rice of sheet surface topology; Fig. 3 is the high-resolution-ration transmission electric-lens picture, as can be seen the multistage hierarchy on nanometer golden flower surface.The laminated structure on nanometer golden flower surface all is a monocrystalline as seen in Figure 8.
(1) C18N3 is dissolved in the redistilled water, preparation obtains the C18N3 aqueous solution of 0.5mM.
(2) at ambient temperature, in the 2.45mL C18N3 aqueous solution, add the aqueous solution of chloraurate of 80 μ L mass concentrations 2% (48mM), make that gold chloride concentration is 1.52mM in the mixed solution.
(3) the rapid aqueous ascorbic acid that adds 0.25mL (or 0.3mL or 0.35mL) concentration 20mM behind the above-mentioned mixed solution mixing 30s, light shaking left standstill 1 hour.
(4) with above-mentioned product solution centrifugal 5min under the rotating speed of 3000r/min, remove supernatant, with sedimentation products second distillation water washing.So circulation is 3 times.
(5) sample with centrifuge washing drips on the silicon chip, drying at room temperature, the electromicroscopic photograph that obtains product as shown in Figure 4, the ascorbic acid that 4a-c is respectively adding is 0.25mL, 0.3mL and 0.35mL.
As seen from the figure, the fixing amount of gold chloride increases the amount of ascorbic acid, can obtain the nm of gold hierarchy of three kinds of different surfaces successively: the ball shaped nano gold of nanometer golden flower, surperficial kick, the nm of gold structure of surperficial baculum.
The preparation method of the gold nano monocrystalline of embodiment 3, surperficial many projections is as follows:
(1) C18N3 is dissolved in the redistilled water, preparation obtains the C18N3 aqueous solution of 0.5mM.
(2) at ambient temperature, the aqueous solution of chloraurate that in the 2.45mL C18N3 aqueous solution, adds 10 μ L (or 20 μ L or 30 μ L) mass concentration 2% (48mM).
(3) the rapid aqueous ascorbic acid that adds 0.25 (20mM) behind the above-mentioned mixed solution mixing 30s, light shaking left standstill 1 hour.
(4) with above-mentioned product solution centrifugal 5min under the rotating speed of 6000r/min, remove supernatant, with sedimentation products second distillation water washing.So circulation is 3 times.
(5) sample with centrifuge washing drips on the silicon chip drying at room temperature.Add 20 μ L chlorauric acid solutions product sem photograph as shown in Figure 5, be surperficial many projections gold nanocrystals as can be seen.
The nanometer golden flower of embodiment 4, the surperficial different topology density of preparation (petal density)
(1) C18N3 is dissolved in the redistilled water, preparation obtains the C18N3 aqueous solution of 0.1mM, 0.3mM, 0.4mM, 0.5mM and 0.6mM respectively.
(2) at ambient temperature, in the C18N3 of the 2.45mL variable concentrations aqueous solution, add the aqueous solution of chloraurate of 80 μ L mass concentrations 2% (48mM) respectively, make that gold chloride concentration is 1.52mM in the mixed solution.
(3) the rapid ascorbic acid that adds 0.25mL (20mM) behind the above-mentioned solution mixing 30s, light shaking left standstill 1 hour.
(4) with above-mentioned product solution centrifugal 5min under the rotating speed of 3000r/min, remove supernatant, with sedimentation products second distillation water washing.So circulation is 3 times.
(5) sample with centrifuge washing drips on the silicon chip; drying at room temperature; the electromicroscopic photograph that obtains product is shown in Fig. 6 (a-e); a-e is respectively corresponding C18N3 initial concentration 0.1,0.3,0.4,0.5,0.6mM; increase with C18N3 concentration; because protective agent quantity increases, can obtain the nanometer golden flower that surperficial sheet density increases.
Embodiment 5, preparation micron order golden flower
(1) C18N3 is dissolved in the redistilled water, preparation obtains the C18N3 aqueous solution of 0.5mM.
(2) at ambient temperature, the aqueous solution of chloraurate that in the 2.45mL C18N3 aqueous solution, adds 130-150 μ L mass concentration 2% (48mM).
(3) the rapid aqueous ascorbic acid that adds 0.25mL (20mM) behind the above-mentioned mixed solution mixing 30s, light shaking left standstill 1 hour.
(4) with above-mentioned product solution centrifugal 5min under the rotating speed of 3000r/min, remove supernatant, with sedimentation products second distillation water washing.So circulation is 3 times.
(5) each sample with centrifuge washing drips on the silicon chip drying at room temperature.Stereoscan photograph is seen Fig. 7.
Claims (8)
1. method for preparing golden grading structure material, be with surfactant C18N3 as template and protective agent, utilize ascorbic acid as reducing agent, make gold chloride carry out reduction reaction, obtain described golden grading structure material.
2. method according to claim 1, it is characterized in that: described method comprises the steps: at ambient temperature, in the C18N3 aqueous solution of concentration, add gold chloride, ascorbic acid successively greater than the C18N3 critical micelle concentration, then with still aging at least 1 hour of mixed solution, centrifugal, washing, remove unnecessary C18N3, obtain described golden grading structure material.
3. method according to claim 2 is characterized in that: the mol ratio of C18N3, gold chloride and ascorbic acid is (0.245-2.45) in the described mixed solution: (1.44-7.2): (5-7); The concentration of C18N3 is greater than the C18N3 critical micelle concentration in the described mixed solution.
4. according to each described method among the claim 1-3, it is characterized in that: described golden grading structure material is of a size of nanoscale to micron order.
5. according to each described method among the claim 1-4, it is characterized in that: described golden grading structure material is a three-dimensional hierarchical structure, and it comprises: the gold nanocrystals of surperficial many projections, subsphaeroidal hollow Nano particle, burger type, surface are for the ball-type structure of baculum and surperficially be the Nano/micron golden flower structure of sheet.
6. method according to claim 5 is characterized in that:
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in the reaction system of described reaction: (1.44-3.36): 5, and described golden grading structure material is the burger type;
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in the reaction system of described reaction: (3.36-3.84): (5-7); Described golden grading structure material is that the surface is the ball-type structure of baculum;
The mol ratio of C18N3, gold chloride and ascorbic acid is (0.245-1.47) in the reaction system of described reaction: (3.84-7.2): 5; Described golden grading structure material is that the surface is the Nano/micron golden flower structure of sheet;
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225 in the reaction system of described reaction: (0.48-1.44): 5; Described golden grading structure material is the gold nanocrystals of surperficial many projections.
7. method according to claim 6 is characterized in that: the mol ratio of C18N3, gold chloride and ascorbic acid is 1.225: 1.44: 5 in the reaction system of described reaction, and described golden grading structure material is the burger type;
The mol ratio of C18N3, gold chloride and ascorbic acid is 1.225: 3.36: 5 or 1.225: 3.84 in the reaction system of described reaction: (6-7); The golden grading structure material of gained is that the surface is the ball-type structure of baculum.
8. according to claim 6 or 7 described methods, it is characterized in that: the particle diameter of described burger type structure is 200-300nm; Described surface be the ball-type structure of baculum or surface for the particle diameter of ball-type in the Nano/micron golden flower structure of sheet be 200-1000nm; Described surface is that the length of protrusion of surface is 50-100nm in the ball-type structure of baculum, and the diameter of projection is 20-50nm; Described surface is that the thickness of surperficial sheet is 20-50nm in the Nano/micron golden flower structure of sheet.
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| CN103934467A (en) * | 2014-04-02 | 2014-07-23 | 南京邮电大学 | Hydrangea-shaped gold nanoparticle and preparation method thereof |
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| CN104308174A (en) * | 2014-09-25 | 2015-01-28 | 中国科学院化学研究所 | Method for dispersing and/or purifying gold nano-sheets |
| CN104439272A (en) * | 2014-11-04 | 2015-03-25 | 天津大学 | Method for manufacturing orderly-arranged gold particles through combination of dewetting method and template method |
| CN106141199A (en) * | 2015-03-24 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | Multi-stage nano JINHUA, its preparation method and application |
| CN106141199B (en) * | 2015-03-24 | 2018-02-27 | 中国科学院宁波材料技术与工程研究所 | Multi-stage nano golden flower, its preparation method and application |
| CN106112003A (en) * | 2016-06-07 | 2016-11-16 | 轻工业化学电源研究所 | A kind of size and the preparation method and application of the adjustable noble metal nano particles of pattern |
| CN106424752A (en) * | 2016-09-29 | 2017-02-22 | 清华大学深圳研究生院 | Silver powder with flower-shaped microstructure and preparation method thereof and electric conducting ink |
| CN110842213A (en) * | 2019-11-12 | 2020-02-28 | 广东羚光新材料股份有限公司 | High-activity silver powder and preparation method and application thereof |
| CN110842213B (en) * | 2019-11-12 | 2022-05-27 | 广东羚光新材料股份有限公司 | High-activity silver powder and preparation method and application thereof |
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