CN103639407A - Tri-metal nanoparticle and preparation method thereof - Google Patents
Tri-metal nanoparticle and preparation method thereof Download PDFInfo
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- CN103639407A CN103639407A CN201310677533.9A CN201310677533A CN103639407A CN 103639407 A CN103639407 A CN 103639407A CN 201310677533 A CN201310677533 A CN 201310677533A CN 103639407 A CN103639407 A CN 103639407A
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Abstract
The invention discloses a tri-metal nanoparticle and a preparation method thereof. The tri-metal nanoparticle is dumbbell-shaped in morphology, a gold bipyramid is arranged at the waist, and heads at two ends of the waist are in sliver-palladium alloy branch shapes. The gold bipyramid is taken as a seed, a silver nitrate solution is taken as a metal precursor, a clubbed template nanoparticle adopting a core-shell structure and with the gold bipyramid covered with sliver is prepared with a seed growing method, and the template nanoparticle is scattered in ultrapure water after centrifugation; by using modified electric displacement in combination with a co-reduction reaction, a palladium chloride acid solution is added into an aqueous solution of the obtained template nanoparticle, ascorbic acid is taken as a reducing agent, and standing is performed at a room temperature; and the dumbbell-shaped tri-metal nanoparticle is obtained through adjusting the molar ratio of silver nitrate to palladium chloride acid and standing time. According to the tri-metal nanoparticle and the preparation method thereof, the nanoparticle in the sliver-palladium alloy branch shape is selectively grown on the gold bipyramid, and a tri-metal nanostructured material is diversified in physicochemical property and high in adjustability.
Description
Technical field
The present invention relates to a kind of metal nanoparticle and preparation method thereof, particularly tri-metal nano particle of a kind of dumbbell shaped and preparation method thereof, belongs to field of nanometer material technology.
Background technology
In recent years, the technology based on nano particle is widely used, because it has unique optics, electric field, the magnetic signature of the nanostructured of depending on.Except monometallic nano particle, increasing people pays close attention to the preparation of multi-metal nanoparticles.Due to cooperative effect, multi-metal nanoparticles shows than the physicochemical properties better renewal of monometallic, 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.For example, polymetallic nano particle has the character of the plasma that is different from monometallic component, such as the coated certain thickness silver-colored shell in the outside at gold rod, can produce four different plasma resonance peaks; Multi-metal nanoparticles shows the catalytic activity higher than monometallic, and Ru Xiayounan seminar utilizes a step seed mediated growth method to prepare Pd-Pt bimetal nano dendritic structure, and its catalytic activity is 5 times of first generation platinum black catalyst; In addition, some novel characteristics can be by regulating the structure of multi-metal nanoparticles to realize.
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 conventionally.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 two kinds of metals of coreduction, regulates the mol ratio of two kinds of metals, the activity of co-conducer can obtain different from the nano particle of structure.Document Nano Res, 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 been prepared the dendritic structure of core-shell (Pd-Pt) structure by a step seed mediated growth method; Document J. Phys. Chem. C and for example, 2010, (114), 7689 – 7693 utilize active stronger hydrazine as reducing agent, the precursor solution by coreduction gold chloride and the acid of chlorine palladium, regulate the mol ratio of gold and palladium to make the Au-Pd alloy nano particle of dendritic structure.For tri-metal nano particle, existing research is mainly nucleocapsid structure, as document ACS Nano, 2013(9), it is reducing agent that 7945-7955 utilizes ascorbic acid and hydrazine, the nano particle that the dendritic Pd-Pt alloy of having prepared octahedra golden nanometer particle and be core, highly crystalline is shell.That the shape of bimetal nano particles mainly contains is spherical, bar-shaped, cube and dendroid etc.
At present, the alloy nano particle of dendritic structure is rare report also in the literature, and existing report also mainly concentrates in the research of bimetallic component, has no the report of the dendroid nanostructured of three metal components.
Summary of the invention
The present invention is directed to prior art and only can provide the deficiency of the nano particle of bimetallic component, provide a kind of physicochemical properties diversification, adjustability strong, and dumbbell shaped three metal component nano particles of the simple golden bipyramid of preparation method two ends growth dendroid silver palladium alloy and preparation method thereof.
The technical solution adopted in the present invention is: a kind of tri-metal nano particle is provided, and its pattern is dumbbell shaped, and waist is golden bipyramid 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 nano particle as above, and step is as follows:
1, liquor argenti nitratis ophthalmicus is joined in golden bipyramid nano particle, take ascorbic acid as reducing agent, obtain the rod-like nano particle of golden bipyramid/silver-colored nucleocapsid structure;
2, in the rod-like nano particle of the golden bipyramid/silver-colored nucleocapsid structure obtaining, add chlorine palladium acid solution, take ascorbic acid as reducing agent, mix under rear room temperature standing 1～6 hour, again through centrifugal treating, obtain a kind ofly take golden bipyramid as waist the dumbbell shaped tri-metal nano particle that two ends growth dendroid silver palladium alloy is 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 (being golden bipyramid) nano particle, and be not core-core/shell nanoparticles structure.Its principle is: utilizing golden bipyramid nano particle is five twin crystal structures, and there is the feature on two sharp-pointed summits, its electric-field intensity and Extinction Cross all have superiority than other particles, the two ends by silver-colored preferred growth at golden bipyramid, and the final nucleocapsid structure forming is bar-shaped; On the basis of this core-shell structure particle, further adding the third metal precursor is the acid of chlorine palladium, and with ascorbic acid, as reducing agent, electricity is put 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, can obtain the dumbbell shaped metal nanoparticle of golden bipyramid two ends growth dendroid silver palladium alloy.
Owing to having implemented 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 two kinds of metals of platinum, and the present invention obtains, is silver and two kinds of metals of palladium.The selective growth of silver palladium dendroid alloy nano particle is on golden bipyramid, and the more diversification of the physicochemical properties 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, through centrifugal treating, just can obtain, and do not need the complicated like this condition of the auxiliary coreduction of hydrothermal solution; In the present invention, use active gentle ascorbic acid as reducing agent, 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 of obtaining by the embodiment of the present invention 1 technical scheme;
Fig. 2 is transmission electron microscope (TEM) figure, high-resolution transmission electron microscope (HRTEM) figure and the linescan figure at the nano particle at golden bipyramid two ends by the dendroid silver palladium alloy length of the embodiment of the present invention 1 preparation;
Fig. 3 is transmission electron microscope (TEM) figure of the nano particle on golden bipyramid by the dendroid silver palladium alloy length of the embodiment of the present invention 2 preparations.
The specific embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further elaborated.
The Chinese invention patent that is CN103240420A by publication number " a kind of method of purification of golden bipyramid structure nano particle ", prepares proof gold bipyramid nano particle.
By proof gold bipyramid nano-particle solution centrifugal 10min under 8000rpm rotating speed of three parts of 1ml, after concentrated, be dispersed in respectively in cetyltriethylammonium bromide (CTAC) solution of 1ml 80mM, add the liquor argenti nitratis ophthalmicus of 60 μ L 0.01M, the ascorbic acid solution of 15 μ L 0.1M, shake up, under the condition of 65 ℃, place 6h, centrifugal rear concentrated, obtain golden core-Yin shell (AuBPs Ag) nano particle.
Getting two parts of golden core-Yin shell (AuBPs Ag) nano particles that make is dispersed in respectively in 1ml ultra-pure water, the chlorine palladium acid solution that adds 40 μ L 0.01M, the ascorbic acid solution of 20 μ L, shake up, standing 1h under room temperature, makes the nano particle that golden bipyramid two ends length has dendroid silver palladium alloy after centrifugal.
The nano particle making is done to morphology analysis, and referring to accompanying drawing 1, a figure is transmission electron microscope (TEM) figure of the highly purified golden bipyramid nano particle that uses in the present embodiment technical scheme; B and c figure are transmission electron microscope (TEM) figure of golden core-Yin shell (AuBPs Ag) nano particle; D figure is elementary analysis (STEM-EDS) figure of (AuBPs@Ag) nano particle linescan, in figure, can see, along the long axis direction of particle, mid portion is gold, and two end portions is silver, thereby confirmation silver is the preferential long two ends at golden bipyramid; E figure is the ultraviolet spectrogram before and after golden bipyramid contracted payment, in figure, can see, occurred silver-colored plasma characteristics peak, and golden bipyramid is in the characteristic peak generation red shift at 822nm place, after 1000nm after contracted payment at 400nm place.
Referring to accompanying drawing 2, a and b figure are transmission electron microscope (TEM) figure that golden bipyramid two ends length has dendroid silver palladium alloy nano particle, c and d figure are high-resolution transmission electron microscope (HRTEM) figure that golden bipyramid two ends length has dendroid silver palladium alloy nano particle, from High-Resolution Map, can find out, the two ends of golden bipyramid are dendritic structures; E figure is linescan elementary analysis (STEM-EDS) figure, in figure, can see, along the long axis direction of particle, mid portion is gold, and two ends are alloys of silver and palladium.
The highly purified golden bipyramid solution of 1ml, centrifugal 10min under 8000rpm rotating speed, after concentrated, be dispersed in respectively in cetyltriethylammonium bromide (CTAC) solution of 1ml 80mM, add the liquor argenti nitratis ophthalmicus of 80 μ L 0.01M, the ascorbic acid solution of 20 μ L 0.1M, shake up, under the condition of 65 ℃, place 6h, centrifugal rear concentrated, golden core-Yin shell (AuBPs Ag) nano particle obtaining is dispersed in 1ml ultra-pure water, the chlorine palladium acid solution that adds 40 μ L 0.01M, the ascorbic acid solution of 20 μ L, shakes up, and is standing 3h under room temperature.
The nano particle making is done to pattern molecule, and referring to accompanying drawing 3, a figure is that the golden bipyramid two ends length that the present embodiment technical scheme makes has the ESEM (SEM) of dendroid silver palladium alloy nano particle to scheme; B, c and d figure are transmission electron microscope (TEM) figure that golden bipyramid two ends length has dendroid silver palladium alloy nano particle; In figure, can see, other conditions are constant, and the amount of silver nitrate is increased to 80 μ L from 60 μ L, standing 3h, and can obtain golden bipyramid two ends length has dendroid silver palladium alloy nano particle.
Claims (5)
1. a tri-metal nano particle, is characterized in that: its pattern is dumbbell shaped, and waist is golden bipyramid structure, and the head at waist two ends is silver palladium alloy dendritic structure.
2. a preparation method for tri-metal nano particle, is characterized in that comprising the steps:
(1) liquor argenti nitratis ophthalmicus is joined in golden bipyramid nano particle, take ascorbic acid as reducing agent, obtain the rod-like nano particle of golden bipyramid/silver-colored nucleocapsid structure;
(2) in the rod-like nano particle of the golden bipyramid/silver-colored nucleocapsid structure obtaining, add chlorine palladium acid solution, take ascorbic acid as reducing agent, mix under rear room temperature standing 1～6 hour, again through centrifugal treating, obtain a kind ofly take golden bipyramid as waist the dumbbell shaped tri-metal nano particle that two ends growth dendroid silver palladium alloy is head.
3. the preparation method of a kind of tri-metal nano particle according to claim 2, 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.
4. the preparation method of a kind of tri-metal nano particle according to claim 2, is characterized in that: in molar ratio, and silver nitrate: chlorine palladium acid: ascorbic acid is 3～5:1～2:5～10.
5. the preparation method of a kind of tri-metal nano particle according to claim 2, is characterized in that: described golden bipyramid nano particle is the proof gold bipyramid nano particle through purification processes.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104741603A (en) * | 2015-04-11 | 2015-07-01 | 苏州大学 | Tri-metal nano particle with asymmetric structure, preparation method and application thereof |
| CN104907557A (en) * | 2015-05-12 | 2015-09-16 | 济南大学 | Flower-like gold palladium heterogeneous nano particle with good electro-catalytic property and preparing method thereof |
| CN106670495A (en) * | 2015-11-06 | 2017-05-17 | 南京大学 | Preparation method of network-state Ag-Au-Pd trimetal porous material |
| CN106735291A (en) * | 2016-12-01 | 2017-05-31 | 苏州大学 | A kind of dendroid two dimension palladium-silver nanometer sheet and preparation method thereof |
| CN107052359A (en) * | 2017-02-09 | 2017-08-18 | 安徽师范大学 | A kind of Au AgPd cores/bimetallic mount structure nano material, preparation method and applications |
| 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 |
| CN108746595A (en) * | 2018-06-22 | 2018-11-06 | 黄河科技学院 | A kind of different-shape gold nano bipyramid-gold and silver nanocomposite and preparation method thereof |
| 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 |
| CN108927151A (en) * | 2018-06-08 | 2018-12-04 | 南京邮电大学 | The method for preparing golden platinum core-shell nanostructure material |
| 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 |
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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 |
| CN104741603A (en) * | 2015-04-11 | 2015-07-01 | 苏州大学 | Tri-metal nano particle with asymmetric structure, preparation method and application thereof |
| CN104907557A (en) * | 2015-05-12 | 2015-09-16 | 济南大学 | Flower-like gold palladium heterogeneous nano particle with good electro-catalytic property and preparing method thereof |
| CN106670495A (en) * | 2015-11-06 | 2017-05-17 | 南京大学 | Preparation method of network-state Ag-Au-Pd trimetal porous material |
| CN106735291A (en) * | 2016-12-01 | 2017-05-31 | 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 |
| CN107052359A (en) * | 2017-02-09 | 2017-08-18 | 安徽师范大学 | A kind of Au AgPd cores/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 |
| CN108746595A (en) * | 2018-06-22 | 2018-11-06 | 黄河科技学院 | A kind of different-shape gold nano bipyramid-gold and silver nanocomposite 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 |
| CN110006976A (en) * | 2019-05-14 | 2019-07-12 | 黄河科技学院 | A kind of electrochemical immunosensor, preparation method and application detecting Alzheimer's disease marker |
| CN110076348A (en) * | 2019-05-14 | 2019-08-02 | 南京航空航天大学 | A kind of superfine metal nanometer frame and preparation method thereof |
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