CN103639407B - A kind of Tri-metal nanoparticle and preparation method thereof - Google Patents
A kind of Tri-metal nanoparticle and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Tri-metal nanoparticle and preparation method thereof.The pattern of Tri-metal nanoparticle is dumbbell shaped, and waist is golden bipyramid, and the head at waist two ends is silver palladium alloy dendroid.With golden bipyramid for seed, liquor argenti nitratis ophthalmicus is metal precursor, is coated on the templating nanoparticles particle of the bar-shaped nucleocapsid structure outside golden bipyramid, is dispersed in ultra-pure water after centrifugal by the method preparation silver of seed growth; Utilize the electricity displacement of modification in conjunction with coreduction reaction, in the aqueous solution of the templating nanoparticles particle obtained, add chlorine palladium acid solution, take ascorbic acid as reducing agent, left at room temperature; By regulating the mol ratio of silver nitrate and the acid of chlorine palladium and standing time, obtain dumbbell shaped Tri-metal nanoparticle.The present invention is by the selective growth of silver-colored palladium dendroid alloy nano particle on golden bipyramid, and physicochemical properties diversification, the adjustability of the nano structural material of three metal components are strong.
Description
Technical field
The present invention relates to a kind of metal nanoparticle and preparation method thereof, particularly a kind of Tri-metal nanoparticle and preparation method thereof of dumbbell shaped, belongs to field of nanometer material technology.
Background technology
In recent years, the technology based on nano particle is widely used, because it has optics, electric field, the magnetic signature of the uniqueness depending on nanostructured.Except monometallic nano particle, increasing people pays close attention to the preparation of multi-metal nanoparticles.Due to cooperative effect, multi-metal nanoparticles show renewal better than monometallic, the physicochemical properties of diversification, such as, magnetic, superconductivity, SME, catalytic activity, hydrogen storage ability and structural rigidity etc., have very large application prospect in fields such as optics, electrochemical device and catalysis.Such as, polymetallic nano particle has the character of the plasma being different from monometallic component, such as at the coated certain thickness silver-colored shell in outside of gold rod, can produce four different plasma resonance peaks; Multi-metal nanoparticles shows the catalytic activity higher than monometallic, and as Xia Younan seminar utilizes a step seed mediated growth method to prepare Pd-Pt bimetal nano dendritic structure, its catalytic activity is 5 times of first generation platinum black catalyst; In addition, the characteristic of some novelties can realize by regulating the structure of multi-metal nanoparticles.
At present, existing research mainly focuses mostly in the preparation and regulation and control of bimetal nano particles.The structure of bimetal nano particles mainly contains nucleocapsid structure and alloy structure, and its preparation method has two kinds usually.The first is seed mediated growth method, and a kind of metal nanoparticle is as seed, and another kind of metal precursor is as growth-promoting media; The second is the precursor solution of coreduction two kinds of metals, regulates the mol ratio of two kinds of metals, the activity of co-conducer, can obtain different from the nano particle of structure.Document NanoRes, 2010(3), 69-80 utilizes the octahedral Pd nano particle in 9-nm cross section as seed, and chloroplatinic acid is as growth-promoting media, and ascorbic acid, as reducing agent, has prepared the dendritic structure of core-shell structure copolymer (Pd-Pt) structure by a step seed mediated growth method; And for example document J.Phys.Chem.C, 2010, (114), 7689 – 7693 utilize active stronger hydrazine as reducing agent, by the precursor solution of coreduction gold chloride and the acid of chlorine palladium, regulate the mol ratio of gold and palladium to obtain the Au-Pd alloy nano particle of dendritic structure.For Tri-metal nanoparticle, existing research mainly nucleocapsid structure, as document ACSNano, 2013(9), 7945-7955 utilizes ascorbic acid and hydrazine to be reducing agent, has prepared that octahedra golden nanometer particle is core, the dendritic Pd-Pt alloy of highly crystalline is the nano particle of shell.The shape of bimetal nano particles mainly contains spherical, bar-shaped, cube and dendroid etc.
At present, the alloy nano particle of dendritic structure also rare report in the literature, and existing report also mainly concentrates in the research of bimetallic component, has no the report of the dendritic nanostructures of three metal components.
Summary of the invention
The present invention is directed to the deficiency that prior art only can provide the nano particle of bimetallic component, there is provided a kind of physicochemical properties diversification, adjustability by force, and dumbbell shaped three metal component nano particle of preparation method simple golden bipyramid two ends Propagating Tree dendritic silver palladium alloy and preparation method thereof.
The technical solution adopted in the present invention is: provide a kind of Tri-metal nanoparticle, and its pattern is dumbbell shaped, and waist is golden double cone structure, and the head at waist two ends is silver palladium alloy dendritic structure.
Technical solution of the present invention also comprises the preparation method of Tri-metal nanoparticle as above, and step is as follows:
1, being joined by liquor argenti nitratis ophthalmicus in golden bipyramid nano particle, take ascorbic acid as reducing agent, obtains the rod-like nano particle of golden bipyramid/silver-colored nucleocapsid structure;
2, in the rod-like nano particle of the golden bipyramid obtained/silver-colored nucleocapsid structure, chlorine palladium acid solution is added, take ascorbic acid as reducing agent, mix rear left at room temperature 1 ~ 6 hour, again through centrifugal treating, obtain one with golden bipyramid for waist, two ends Propagating Tree dendritic silver palladium alloy is the dumbbell shaped Tri-metal nanoparticle of head.
A preferred version of the present invention is: liquor argenti nitratis ophthalmicus concentration is 0.01M, and chlorine palladium acid solutions is 0.01M, and ascorbic acid concentrations is 0.1M.By in molar ratio, silver nitrate: chlorine palladium acid: ascorbic acid is 3 ~ 5:1 ~ 2:5 ~ 10.
In technical solution of the present invention, described golden bipyramid nano particle is the proof gold bipyramid nano particle through purification processes.
Silver-colored palladium dendroid alloy nano particle in the present invention be selective growth on another structure (i.e. golden bipyramid) nano particle, and be not core-shell structure copolymer nano particle structure.Its principle is: utilize golden bipyramid nano particle to be five twin crystal structures, and there is the feature of two acute vertex, its electric-field intensity and Extinction Cross all have superiority than other particles, and by the two ends of silver-colored preferred growth at golden bipyramid, the final nucleocapsid structure formed is bar-shaped; On the basis of this core-shell structure particle, add the third metal precursor and the acid of chlorine palladium further, with ascorbic acid as reducing agent, electricity puts exchange reaction (Ag+Pd
2+→ Ag
++ Pd) and coreduction reaction (Ag
++ Pd
2+→ Ag+Pd) carry out simultaneously, according to the difference in reaction time, the dumbbell shaped metal nanoparticle of golden bipyramid two ends Propagating Tree dendritic silver palladium alloy can be obtained.
Owing to implementing technique scheme, compared with prior art, the obvious advantage of the present invention is:
1. bimetallic dendroid alloy nano particle of the prior art mainly concentrates on palladium and platinum two kinds of metals, and the present invention obtains is silver and palladium two kinds of metals.The selective growth of silver palladium dendroid alloy nano particle is on golden bipyramid, and the physicochemical properties more diversification of the nano structural material of three metal components, adjustability are stronger.
2. the process conditions of technical solution of the present invention are simple, as long as at room temperature place certain hour, just can obtain through centrifugal treating, do not need the condition that hydrothermal solution assists coreduction complicated like this; Use active gentle ascorbic acid as reducing agent in the present invention, do not need with the very strong reducing agent of reproducibility.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure and the ultraviolet spectrogram of golden core-Yin shell (AuBPs Ag) nano particle obtained by the embodiment of the present invention 1 technical scheme;
Fig. 2 is that the dendroid silver palladium alloy length prepared by the embodiment of the present invention 1 is at transmission electron microscope (TEM) figure, high resolution TEM (HRTEM) figure and linescan figure of the nano particle at golden bipyramid two ends;
Fig. 3 is transmission electron microscope (TEM) figure of the nano particle of dendroid silver palladium alloy length on golden bipyramid by the embodiment of the present invention 2 preparation.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical solution of the present invention is further elaborated.
Embodiment 1
By the Chinese invention patent " a kind of method of purification of golden double cone structure nano particle " that publication number is CN103240420A, prepare proof gold bipyramid nano particle.
By proof gold bipyramid nano-particle solution centrifugal 10min under 8000rpm rotating speed of three parts of 1ml, be dispersed in cetyltriethylammonium bromide (CTAC) solution of 1ml80mM respectively after concentrated, add the ascorbic acid solution of the liquor argenti nitratis ophthalmicus of 60 μ L0.01M, 15 μ L0.1M, shake up, 6h is placed under the condition of 65 DEG C, centrifugal rear concentrated, obtain golden core-Yin shell (AuBPs Ag) nano particle.
Getting two parts of obtained golden core-Yin shell (AuBPs Ag) nano particles is dispersed in 1ml ultra-pure water respectively, add the chlorine palladium acid solution of 40 μ L0.01M, the ascorbic acid solution of 20 μ L, shake up, left at room temperature 1h, the long nano particle having dendroid silver palladium alloy in centrifugal rear obtained golden bipyramid two ends.
Obtained nano particle is done morphology analysis, is transmission electron microscope (TEM) figure of the highly purified golden bipyramid nano particle used in the present embodiment technical scheme see accompanying drawing 1, a figure; B and c figure is transmission electron microscope (TEM) figure of golden core-Yin shell (AuBPs Ag) nano particle; D figure is elementary analysis (STEM-EDS) figure of (AuBPsAg) nano particle linescan, can see by figure, and along the long axis direction of particle, mid portion is gold, and two end portions is silver, thus confirms that silver is preferential length at the two ends of golden bipyramid; E figure is the ultraviolet spectrogram before and after golden bipyramid contracted payment, can see by figure, has occurred silver-colored plasma characteristics peak after contracted payment at 400nm place, and golden bipyramid is in the characteristic peak generation red shift at 822nm place, after 1000nm.
See accompanying drawing 2, a and b figure is long transmission electron microscope (TEM) figure having dendroid silver palladium alloy nano particle in golden bipyramid two ends, c and d figure is long high resolution TEM (HRTEM) figure having dendroid silver palladium alloy nano particle in golden bipyramid two ends, as can be seen from High-Resolution Map, the two ends of golden bipyramid are dendritic structures; E figure is linescan elementary analysis (STEM-EDS) figure, can see by figure, and along the long axis direction of particle, mid portion is gold, and two ends are alloys of silver and palladium.
Embodiment 2
The highly purified golden bipyramid solution of 1ml, centrifugal 10min under 8000rpm rotating speed, be dispersed in cetyltriethylammonium bromide (CTAC) solution of 1ml80mM respectively after concentrated, add the ascorbic acid solution of the liquor argenti nitratis ophthalmicus of 80 μ L0.01M, 20 μ L0.1M, shake up, 6h is placed under the condition of 65 DEG C, centrifugal rear concentrated, golden core-Yin shell (AuBPs Ag) nanoparticle dispersion obtained is in 1ml ultra-pure water, add the chlorine palladium acid solution of 40 μ L0.01M, the ascorbic acid solution of 20 μ L, shakes up, and is left at room temperature 3h.
Obtained nano particle is done pattern molecule, is long ESEM (SEM) figure having dendroid silver palladium alloy nano particle in golden bipyramid two ends that the present embodiment technical scheme obtains see accompanying drawing 3, a figure; B, c and d figure is long transmission electron microscope (TEM) figure having dendroid silver palladium alloy nano particle in golden bipyramid two ends; Can see by figure, other conditions are constant, and the amount of silver nitrate is increased to 80 μ L from 60 μ L, leave standstill 3h, and can obtain golden bipyramid two ends length has dendroid silver palladium alloy nano particle.
Claims (4)
1. a preparation method for Tri-metal nanoparticle, is characterized in that comprising the steps:
(1) being joined by liquor argenti nitratis ophthalmicus in golden bipyramid nano particle, is reducing agent with ascorbic acid, obtains the rod-like nano particle of golden bipyramid/silver-colored nucleocapsid structure;
(2) in the rod-like nano particle of the golden bipyramid obtained/silver-colored nucleocapsid structure, chlorine palladium acid solution is added, take ascorbic acid as reducing agent, mix rear left at room temperature 1 ~ 6 hour, again through centrifugal treating, obtain one with golden bipyramid for waist, two ends Propagating Tree dendritic silver palladium alloy is the dumbbell shaped Tri-metal nanoparticle of head.
2. the preparation method of a kind of Tri-metal nanoparticle according to claim 1, is characterized in that: liquor argenti nitratis ophthalmicus concentration is 0.01M, and chlorine palladium acid solutions is 0.01M, and ascorbic acid concentrations is 0.1M.
3. the preparation method of a kind of Tri-metal nanoparticle according to claim 1, is characterized in that: in molar ratio, silver nitrate: chlorine palladium acid: ascorbic acid is 3 ~ 5:1 ~ 2:5 ~ 10.
4. the preparation method of a kind of Tri-metal nanoparticle according to claim 1, is characterized in that: described golden bipyramid nano particle is the proof gold bipyramid nano particle through purification processes.
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| CN104741603B (en) * | 2015-04-11 | 2017-08-01 | 苏州大学 | A kind of dissymmetrical structure Tri-metal nanoparticle, preparation method and applications |
| CN104907557B (en) * | 2015-05-12 | 2017-04-19 | 济南大学 | Preparation method for flower-like gold palladium heterogeneous nano particle with good electro-catalytic property |
| CN106670495A (en) * | 2015-11-06 | 2017-05-17 | 南京大学 | Preparation method of network-state Ag-Au-Pd trimetal porous material |
| CN106735291B (en) * | 2016-12-01 | 2019-01-08 | 苏州大学 | A kind of dendroid two dimension palladium-silver nanometer sheet and preparation method thereof |
| CN107052359B (en) * | 2017-02-09 | 2018-11-20 | 安徽师范大学 | A kind of Au-AgPd core/bimetallic mount structure nano material, preparation method and applications |
| CN108855060A (en) * | 2017-05-16 | 2018-11-23 | 中国科学院上海硅酸盐研究所 | A kind of catalysis material and preparation method thereof of gold nanorods both ends cladding nanoparticle palladium |
| CN107894675A (en) * | 2017-12-28 | 2018-04-10 | 深圳市华星光电技术有限公司 | Liquid crystal display panel and liquid crystal display device |
| CN108927151A (en) * | 2018-06-08 | 2018-12-04 | 南京邮电大学 | The method for preparing golden platinum core-shell nanostructure material |
| CN108746595B (en) * | 2018-06-22 | 2020-04-07 | 黄河科技学院 | Gold nanometer bipyramid-gold and silver nanometer composite material with different morphologies and preparation method thereof |
| CN109365831A (en) * | 2018-12-19 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method of new infrared photodetection substrate based on tip deposition Pd/Ag gold nano double cone structure |
| CN110006976B (en) * | 2019-05-14 | 2021-06-15 | 黄河科技学院 | Electrochemical immunosensor for detecting Alzheimer's disease marker, and preparation method and application thereof |
| CN110076348B (en) * | 2019-05-14 | 2020-11-20 | 南京航空航天大学 | Superfine metal nano frame and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101623762A (en) * | 2008-07-09 | 2010-01-13 | 国家纳米科学中心 | Island-shaped porous tri-metal nano rod with gold core/silver-platinum alloy shell structure and method for preparing same |
| CN103240420A (en) * | 2013-05-24 | 2013-08-14 | 苏州大学 | Purification method for gold nano-particles with double-cone structures |
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| GB0227738D0 (en) * | 2002-11-28 | 2003-01-08 | Univ Liverpool | Nanoparticle conjugates and method of production thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101623762A (en) * | 2008-07-09 | 2010-01-13 | 国家纳米科学中心 | Island-shaped porous tri-metal nano rod with gold core/silver-platinum alloy shell structure and method for preparing same |
| CN103240420A (en) * | 2013-05-24 | 2013-08-14 | 苏州大学 | Purification method for gold nano-particles with double-cone structures |
Non-Patent Citations (3)
| Title |
|---|
| Crystalline structure-dependent growth of bimetallic nanostructures;Qian Li et. al.;《Nanoscale》;20120925(第4期);7070-7077 * |
| Nucleation and growth mechanisms for Pd-Pt bimetallic nanodendrites and their electrocatalytic properties;Lim B. et. al.;《Nano Research》;20100327(第3期);69-80 * |
| Synthesis and electrocatalytic activity of Au-Pd alloy nanodendrites for ethanol oxidation;Lee Y. W. et. al.;《The Journal of Physical Chemistry C》;20100412(第114期);7689-7693 * |
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