CN100393456C - Hollow ball granular chain of nano-polycrystalline noble-metal and its production - Google Patents
Hollow ball granular chain of nano-polycrystalline noble-metal and its production Download PDFInfo
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- CN100393456C CN100393456C CNB2006100881090A CN200610088109A CN100393456C CN 100393456 C CN100393456 C CN 100393456C CN B2006100881090 A CNB2006100881090 A CN B2006100881090A CN 200610088109 A CN200610088109 A CN 200610088109A CN 100393456 C CN100393456 C CN 100393456C
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Abstract
A chain of hollow nanoparticles made of polycrystal noble metal (Au, Pd, or Pt) is prepared through dissolving polyvinyl pyrrolidone in inertial gas and uniform magnetic field while stirring, adding hexahydrated cobalt chloride powder, dropping the aqueous solution of sodium bromohydride, adding the solution of AuCl3, PdCl6 or PtCl6 to obtain coarse product, and purifying.
Description
Technical field:
The invention belongs to the nano particle technical field, particularly nano-polycrystalline noble-metal gold, palladium or platinum hollow ball particle chain and preparation method thereof.
Background technology:
Noble metal nano particles has very strong local surface plasma oscillation characteristic at visible light wave range, makes its prospect that has a very wide range of applications at aspects such as biochemistry sensing, biomarker, nanometer waveguides.In recent years, the research of noble metal nano particles has caused more and more researchers' interest, particularly more with rapid changepl. never-ending changes and improvements to the research of the hollow Nano particle of noble metal, reason is that there is far-reaching application potential in hollow-core construction in fields such as medicine delivery, microfabricated chemical reactor, efficient catalytics.For example U.S.'s " science " (Science 298.2176-2179,2002) has reported the technology of preparing of noble metal hollow ball particle, promptly electric displacement reaction (galvanic replacement reactions) technology; Germany's " applied chemistry " (Angew.Chem.Int.Ed.43.1540-1543,2004) report can be applied to this electric displacement reaction technology the system that the reaction of cobalt granule effect predecessor generates precious metal palladium hollow ball particle; Remarkable red shift takes place with the local surface plasma oscillation peak of the silver nano-grain golden hollow Nano particle that reaction obtains as predecessor in Germany's " high material " (Adv.Mater.17,2255-2261,2005) report.Yet, because the factor that does not exist direction to induce in the existing preparation noble metal hollow nano particle process, the noble metal hollow nano particle that the electric displacement reaction of above bibliographical information is prepared all is single decentralized system, on using, there is common limitation, for example badly controls, do not have ordered structure, poor, the medicine carrying ability of electronic transmission performance.Up to the present, do not see the senior nanostructured that bibliographical information noble metal hollow ball nano particle forms as yet, for example chain-like nanometer structure.
Summary of the invention:
The purpose of this invention is to provide a kind of nano-polycrystalline noble-metal gold, palladium or platinum hollow ball particle chain and preparation method thereof, to overcome the shortcoming that in the prior art hollow ball nano particle is difficult to control, lack order, obtain the orderly chain structure of Precious Metals-Gold, palladium or platinum hollow ball nano particle.
The preparation method of nano-polycrystalline noble-metal hollow ball particle chain of the present invention is included under 500～1500 revolutions per seconds the mixing speed and inert atmosphere, and (PVP) is dissolved in the water with polyvinylpyrrolidone, adds cobalt chloride hexahydrate powder (CoCl again
26H2O), make PVP concentration in the solution be 0.125～0.25 mM/liter, cobalt chloride concentration be 1.5～3.5 mMs/liter; Contain 3～6 milligrams of sodium borohydride (NaBH with 8～12 milliliters
4) the aqueous solution join in the above-mentioned solution with 3～10 droplets/second speed; It is characterized in that: said process is in the uniform magnetic field of 100～300 milli teslas; The pH value that adds content then and be 0.3～0.7 mM is this noble metal source AuCl of 6～8
3 -, PdCl
6 4 -Or PtCl
6 2-Solution; Crude product is purified, promptly obtain the nano-hollow ball particle chain of its Precious Metals-Gold (Au), palladium (Pd) or platinum (Pt).
This product can be dissolved in the ethanol and be preserved.
Nano-polycrystalline noble-metal hollow ball particle chain of the present invention is characterized in that by diameter being that the polycrystalline noble-metal particle of 25nm～70nm connects into the chain structure that chain length is 500nm～5000nm; Described noble metal comprises gold (Au), palladium (Pd) or platinum (Pt).
The inventive method is different from prior art and does not have the noble metal hollow particle of preparing under the externally-applied magnetic field effect: because NaBH
4The cobalt colloidal solution predecessor that the reduction cobalt chloride forms is not having can not form chain-like nanometer structure under the external magnetic field, but single dispersing morphology, noble metal Au, the Pd or the Pt hollow ball particle that form in the feasible further reaction also present monodisperse status, rather than chain structure; And the present invention is when preparation predecessor cobalt colloidal solution, induce the cobalt colloidal solid to form the chain-like nanometer structure predecessor by externally-applied magnetic field, thereby make noble metal Au, the Pd of formation in further reacting or the chain feature that Pt hollow ball particle can keep predecessor; This noble metal hollow ball particle chain-like nanometer structure is not reported so far, and this externally-applied magnetic field that utilizes is not reported to the structure regulating of noble metal hollow ball nano particle yet.Compare with single decentralized noble metal hollow ball nano particle, this noble metal hollow variole pellet chain has the potential performance of a lot of uniquenesses, for example better structurally ordered property, easily handling, enhanced electron transmission performance, bigger medicine carrying ability, these potential characteristics make it in nano electron device, molecule sensor and biological medicine carrying field profound application prospect be arranged.
Description of drawings:
Fig. 1 is the transmission electron microscope photo of the embodiment of the invention 1 product gold hollow ball particle chain;
Fig. 2 is the single transmission electron microscope photo of golden hollow ball particle chain;
Fig. 3 is the high-resolution-ration transmission electric-lens photo of golden hollow ball particle chain;
Fig. 4 is the electronic diffraction photo of golden hollow ball particle chain;
Fig. 5 is the X ray energy dispersive spectrogram of golden hollow ball particle chain.
Fig. 6 is the single transmission electron microscope photo of the embodiment of the invention 2 product palladium hollow ball particle chains;
Fig. 7 is the high-resolution-ration transmission electric-lens photo of palladium hollow ball particle chain;
Fig. 8 is the electronic diffraction photo of palladium hollow ball particle chain;
Fig. 9 is the X ray energy dispersive spectrogram of palladium hollow ball particle chain.
Figure 10 is the single transmission electron microscope photo of the embodiment of the invention 3 product platinum hollow ball particle chains;
Figure 11 is the high-resolution-ration transmission electric-lens photo of platinum hollow ball particle chain;
Figure 12 is the electronic diffraction photo of platinum hollow ball particle chain;
Figure 13 is the X ray energy dispersive spectrogram of platinum hollow ball particle chain.
Figure 14 is the transmission electron microscope photo of comparative example 1 product list decentralized gold hollow ball particle;
Figure 15 is the high-resolution-ration transmission electric-lens photo of single decentralized gold hollow ball particle.
Figure 16 is the transmission electron microscope photo of comparative example 2 product list decentralized palladium hollow ball particles;
Figure 17 is the high-resolution-ration transmission electric-lens photo of single decentralized palladium hollow ball particle.
Figure 18 is the transmission electron microscope photo of comparative example 3 product list decentralized platinum hollow ball particles;
Figure 19 is the high-resolution-ration transmission electric-lens photo of single decentralized platinum hollow ball particle.
The specific embodiment:
Embodiment 1: the preparation average-size is the polycrystalline attitude Au hollow ball particle chain of 50 nanometers
At first configuration is used to prepare the predecessor colloidal solution A of noble metal hollow ball chain, and step is: under inert atmosphere-adopt nitrogen in the present embodiment, with 200mg PVP through ultrasonic dissolution in 20ml water, take by weighing 11.9mgCoCl again
26H2O dissolves in this solution.This solution is transferred in the three-neck flask of 100ml capacity, from the stirring piece of middle bottleneck insertion mechanical agitator, a nitrogen bottleneck from the side feeds, and another bottleneck is put dropping funel.Whole reaction system is placed in the uniform magnetic field of 200 milli teslas.Under the mechanical agitation speed of 1000rpm, kept 15 minutes.Other gets 5mg NaBH
4Be dissolved in the 10ml water, and transfer in the dropping funel rapidly.Then in 1 minute with this NaBH
4The aqueous solution at the uniform velocity is added dropwise in the three-neck flask, has obtained dark brown colloidal solution, and continues to stir 5 minutes under nitrogen protection, stirs standby under blanket of nitrogen.
Dispose golden source solution C then, step is: the HAuCl that gets 5ml 0.1M
3Solution is neutralized to pH=7.0 with the KOH solution of 1M, is diluted to 20ml then.
After washing above-mentioned dropping funel 3 times with low amounts of water, in 1 minute, will prepare golden source solution C with it and join among the above-mentioned predecessor colloidal solution A, obtain navy blue colloidal solution, and continue under blanket of nitrogen, to stir 30 minutes, after leaving standstill 5 minutes, product is purified.
Purification step is: the navy blue colloidal solution that obtains is used centrifuge with 2400rpm centrifugal 10 minutes, discard supernatant liquor, its precipitation is dissolved again with water of equivalent, with 2400rpm centrifugal 10 minutes again; 3 times so repeatedly, the precipitation that obtains 1ml anhydrous alcohol solution still is a navy blue colloidal solution.
Above-mentioned colloidal solution is dripped 2～3 to be dripped on the plating carbon film copper mesh that testing electronic microscope uses, after treating that solvent volatilizees fully, it is to take pictures under 200,000 volts the JOEL2100 type high resolution transmission electron microscopy that the plating carbon film copper mesh that is loaded with product is put as for accelerating potential.Fig. 1 is the transmission electron microscope photo of golden hollow ball particle chain, and the average length of visible golden hollow ball chain is 2 microns; Fig. 2 is the single transmission electron microscope photo of golden hollow ball particle chain, and visible hollow ball particle is spherical in shape, big or small basically identical, and diameter is at 50 ± 10nm; Fig. 3 is the high-resolution photo of a hollow ball inside on the chain, and Fig. 4 is its electron diffraction diagram, and the lattice fringe picture of the Au of a plurality of directions that occur among Fig. 3 and the ring-type diffraction pattern among Fig. 4 have shown that product is the nano material of polycrystalline attitude; Fig. 5 is its X ray energy dispersive analysis chart, and is visible except the background signal (i.e. the position of the mark Cu of institute among the figure) of substrate copper mesh among the figure, only contains the signal (i.e. the position of the mark Au of institute among the figure) of single-element Au.Hence one can see that, and the present embodiment product is that average-size is the polycrystalline attitude Au hollow ball particle chain of 50 nanometers.As seen, predecessor colloidal solution A makes the product of electric displacement reaction embody orderly chain-like nanometer structure under the inducing action of externally-applied magnetic field.
Embodiment 2: the preparation average-size is the polycrystalline attitude Pd hollow ball particle chain of 50 nanometers
Configuration palladium source solution D: take by weighing 88.66mg PdCl
2, be dissolved into it among the HCl of 10ml 1M after, be neutralized to pH=7.0 with the KOH solution of 1M, be diluted to 20ml again.
Adopt and embodiment 1 identical operations and method, the palladium source solution D that configures is added drop-wise among the colloid predecessor A that is used for the preparation of hollow ball chain, continued under inert atmosphere mechanical agitation 30 minutes, obtain black colloidal solution.Purification step is dissolved in the 1ml absolute ethyl alcohol at last with embodiment 1, is black colloidal solution.
Sample test and data processing method are with embodiment 1.Fig. 6 is the transmission electron microscope photo of single Pd hollow ball chain, and Pd hollow ball particle is spherical in shape on the visible chain from photo, big or small basically identical, and diameter is at 50 ± 10nm; Fig. 7 is the high-resolution photo of a hollow ball inside on the chain, and Fig. 8 is its electron diffraction diagram, and the lattice fringe picture of the Pd of a plurality of directions that occur among Fig. 7 and the ring-type diffraction pattern among Fig. 8 have shown that product is the nano material of polycrystalline attitude; Fig. 9 is its X ray energy dispersive analysis chart, and is visible except the background signal (i.e. the position of the mark Cu of institute among the figure) of substrate copper mesh among the figure, only contains the signal (i.e. the position of the mark Pd of institute among the figure) of single-element Pd.Hence one can see that, and the present embodiment product is that average-size is the polycrystalline attitude Pd hollow ball particle chain of 50 nanometers.
Embodiment 3: the preparation average-size is the polycrystalline attitude Pt hollow ball particle chain of 40 nanometers
Configuration platinum source solution E: take by weighing 0.24g H
2PtCl
66H
2O is dissolved in the 10ml water, and the KOH solution that drips 1M is neutralized to pH=7.0, is diluted to 20ml again.
Adopt and embodiment 1 identical operations and method, the platinum source solution E that configures is added drop-wise to the colloid precursor solution A that is used for the preparation of hollow ball chain, continued under inert atmosphere mechanical agitation 30 minutes, obtain black colloidal solution.Method of purification is dissolved in the 1ml absolute ethyl alcohol at last with embodiment 1, is black colloidal solution.
Sample test and data processing method are with embodiment 1.Figure 10 is the transmission electron microscope photo of single Pd hollow ball chain, and Pt hollow ball particle is spherical in shape on the visible chain from photo, most of granular size unanimity, and diameter is at 40 ± 10nm, and utmost point individual particles diameter surpasses 60nm; Figure 11 is the high-resolution photo at two hollow ball overlapping places on the chain, and Figure 12 is its electron diffraction diagram, and the lattice fringe picture of the Pt of a plurality of directions that occur among Figure 11 and the ring-type diffraction pattern among Figure 12 have shown that product is the nano material of polycrystalline attitude; Figure 13 is its X ray energy dispersive analysis chart, as seen except the background signal (i.e. the position of the mark Cu of institute among the figure) of substrate copper mesh and substrate copper on the net the background signal (i.e. the position of the mark C of institute among the figure) of the carbon film that plates, only contain the signal (i.e. the position of the mark Pt of institute among the figure) of single-element Pt among the figure.Conclusion is that product is that average-size is the polycrystalline attitude Pt hollow ball particle chain of 40 nanometers.
In the above embodiments of the invention, in the process of configuration predecessor colloidal solution, all used externally-applied magnetic field.Presentation of results exists under the situation of externally-applied magnetic field, utilizes product that the cobalt colloid prepares for the predecessor of the electric displacement reaction chain-like nanometer structure for polycrystalline noble-metal gold, palladium or platinum hollow ball particle.Below by three groups of comparative examples situation when not adding magnetic field in the process of configuration predecessor colloidal solution is described.
Comparative example 1: the preparation average-size is single decentralized polycrystalline attitude Au hollow ball particle of 50 nanometers
Configuration is used to prepare the predecessor colloidal solution B of single decentralized noble metal hollow ball, step is: cancel the uniform magnetic field around the reaction unit in the process for preparing predecessor A among the embodiment 1, other operations are with embodiment 1, can obtain the colloidal solution of dark brown, continue under inert atmosphere mechanical agitation 5 minutes.
With with embodiment 1 in identical method prepare golden source solution, and use and embodiment 1 identical operations and method, the golden source drips of solution that configures is added to the predecessor colloidal solution B that is used for noble metal hollow ball preparation, continued under inert atmosphere mechanical agitation 30 minutes, obtain black colloidal solution.After leaving standstill 5 minutes, product is purified.
Purification step is: use centrifuge with 3000rpm centrifugal ten minutes in the navy blue colloidal solution that obtains, discard supernatant liquor, its precipitation is dissolved again with water of equivalent, again with 3000rpm centrifugal ten minutes; 3 times so repeatedly, the precipitation that obtains 1ml anhydrous alcohol solution still is a navy blue colloidal solution.
Above-mentioned colloidal solution is dripped 2～3 to be dripped on the plating carbon film copper mesh that testing electronic microscope uses, after treating that solvent volatilizees fully, it is to take pictures under 200,000 volts the JOEL2100 type high resolution transmission electron microscopy that the plating carbon film copper mesh that is loaded with product is put as for accelerating potential.Figure 14 is its transmission electron microscope photo, and Au hollow ball particle is single decentralized as can be seen from photo, and average diameter is at 50 ± 20nm; Figure 15 is the high-resolution photo at an Au hollow ball grain edges place, and the lattice fringe of the Au of a plurality of directions that occur in the photo looks like to show that it is the nano material of polycrystalline attitude.Conclusion is that product is that average-size is single decentralized polycrystalline attitude Au hollow ball particle of 50 nanometers.As seen, under the situation that does not have externally-applied magnetic field, predecessor colloidal solution B can not induced in layoutprocedure, and then makes next step the product of electric displacement reaction embody unordered single decentralized nanostructured.
Comparative example 2: the preparation average-size is single decentralized polycrystalline attitude Pd hollow ball particle of 35 nanometers
Press the method preparation Pd source of embodiment 2, use and comparative example 1 identical operations and method, it is added drop-wise to the predecessor colloidal solution B that is used for preparing the noble metal hollow ball, continued under inert atmosphere mechanical agitation 30 minutes, obtain black colloidal solution.Method of purification is with comparative example 1, and product is dissolved in the 1ml absolute ethyl alcohol, is black colloidal solution.
Sample test and data processing method are with comparative example 1.Figure 16 is its transmission electron microscope photo, and Pd hollow ball particle is single decentralized as can be seen from photo, and average diameter is at 35 ± 10nm; Figure 17 is the high-resolution photo of a Pd hollow ball granule interior, and the lattice fringe of the Pd of a plurality of directions that occur in the photo looks like to show that it is the nano material of polycrystalline attitude.As can be known, product is that average-size is single decentralized polycrystalline attitude Pd hollow ball particle of 35 nanometers.
Comparative example 3: the preparation average-size is single decentralized polycrystalline attitude Pt hollow ball particle of 30 nanometers
Press the method preparation Pt source of embodiment 3, use and comparative example 1 identical operations and method, it is added drop-wise to the predecessor colloidal solution B that is used for preparing the noble metal hollow ball, continued under inert atmosphere mechanical agitation 30 minutes, obtain black colloidal solution.Method of purification is with comparative example 1, and product is dissolved in the 1ml absolute ethyl alcohol, is black colloidal solution.
Sample test and data processing method are with comparative example 1.Figure 18 is its transmission electron microscope photo, and Pt hollow ball particle is single decentralized as can be seen from photo, and average diameter is at 30 ± 10nm; Figure 19 is the high-resolution photo of a Pd hollow ball granule interior, and the lattice fringe of the Pt of a plurality of directions that occur in the photo looks like to show that it is the nano material of polycrystalline attitude.Hence one can see that, and product is that average-size is single decentralized polycrystalline attitude Pt hollow ball particle of 30 nanometers.
Above-mentioned three comparative examples explanation under the situation that does not have externally-applied magnetic field, utilizes product that the cobalt colloid prepares for the predecessor of the electric displacement reaction single decentralized nanostructured for polycrystalline noble-metal gold, palladium or platinum hollow ball particle.
The analysis-by-synthesis explanation:
In reaction of the present invention, utilize the cobalt colloid to prepare granular nanometer polycrystalline noble-metal gold, palladium or platinum hollow ball and the hollow ball chain nano material of hollow-core construction for the predecessor of electric displacement reaction.The endocorpuscular form of cobalt colloid has directly determined the formalness of end product.When having externally-applied magnetic field, the particle in the cobalt colloid can be subjected to inducing of externally-applied magnetic field, forms ordered structure, and the noble metal hollow variole pellet chain that the product of electric displacement reaction just can be arranged in order embodies the inductive effect of external magnetic field; If when not having externally-applied magnetic field, the particle in the cobalt colloid can not be subjected to inducing of outfield, the product of electric displacement reaction just can obtain the noble metal hollow ball nano particle of single decentralized, has kept the disordered state of particle in the cobalt colloid.
Claims (2)
1. the preparation method of a nano-polycrystalline noble-metal hollow ball particle chain, be included under 500～1500 revolutions per seconds the mixing speed and inert atmosphere, polyvinylpyrrolidone is dissolved in the water, add the cobalt chloride hexahydrate powder again, make polyvinylpyrrolidone concentration in the solution be 0.125～0.25 mM/liter, cobalt chloride concentration be 1.5～3.5 mMs/liter; The speed of 8～12 milliliters of aqueous solution that contain 3～6 milligrams of sodium borohydrides with 3～10 droplets/second is joined in the above-mentioned solution; It is characterized in that: said process is in the uniform magnetic field of 100～300 milli teslas; The pH value that adds content then and be 0.3～0.7 mM is 6～8 noble metal source AuCl
3 -, PdCl
6 4-Or PtCl
6 2-Solution; Crude product is purified, promptly obtain the nano-hollow ball particle chain of its Precious Metals-Gold, palladium or platinum.
2. nano-polycrystalline noble-metal hollow ball particle chain is characterized in that by diameter being that the polycrystalline noble-metal particle of 25nm～70nm connects into the chain structure that chain length is 500nm～5000nm; Described noble metal comprises gold, palladium or platinum.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI307297B (en) | 2006-12-14 | 2009-03-11 | Ind Tech Res Inst | Method for manufacturing metal nano particles having hollow structure |
| CN101288909B (en) * | 2007-04-18 | 2011-10-12 | 财团法人工业技术研究院 | Preparation method of metal nano particle with hollow structure and metal nano particle |
| CN101775638A (en) * | 2010-03-24 | 2010-07-14 | 中国科学院长春应用化学研究所 | Preparation method of palladium nano crystal |
| CN104971737B (en) * | 2014-04-09 | 2017-12-01 | 中国科学院大连化学物理研究所 | A kind of PtCo nano-hollow balls, its preparation method and application |
| CN104625088B (en) * | 2015-03-20 | 2017-02-01 | 广东工业大学 | Environment-friendly synthesis method of 1D chain structure nano particles |
| CN111318721B (en) * | 2020-03-19 | 2022-04-15 | 四川省疾病预防控制中心 | Preparation method of platinum nano-chain |
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