CN103252501A - Method for preparing metal palladium nanowires of controllable size - Google Patents
Method for preparing metal palladium nanowires of controllable size Download PDFInfo
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- CN103252501A CN103252501A CN2013101558769A CN201310155876A CN103252501A CN 103252501 A CN103252501 A CN 103252501A CN 2013101558769 A CN2013101558769 A CN 2013101558769A CN 201310155876 A CN201310155876 A CN 201310155876A CN 103252501 A CN103252501 A CN 103252501A
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Abstract
The invention relates to a method for preparing metal palladium nanowires of controllable size. The method is characterized in that the method comprises the following steps of (1) preparation of palladium oxide nano-particles, namely a palladium chloride solution of certain concentration is prepared according to needs and hydrolysis is carried out; (2) preparation of azelon, namely an insulin solution is dropwise added on a mica sheet; (3) synthesis of palladium oxide nanowires, namely palladium oxide nano-particle solution is dropwise added on the mica sheet with azelon deposited, and then cultivation and blow-drying are carried out to obtain the palladium oxide nanowires; (4) reduction of palladium oxide, namely borane dimethyl amine is dropwise added on the mica sheet with the palladium oxide nanowires prepared, and after cultivation, washing and blow-drying, the one-dimension metal palladium nanowires are obtained. Compared with the prior art, the method can be used for preparing the environment-friendly metal palladium nanowires of controllable size and is simple.
Description
Technical field
The present invention relates to the preparation method of Metal Palladium nano wire, especially refer to a kind of preparation method of Metal Palladium nano wire of controllable size.
Background technology
The one-dimensional metal palladium nanometer wire is subjected to extensive concern because having unique functions such as optics, electricity and catalytic.Utilize the palladium nanometer wire general cost of way preparations such as physical etchings very high, so prepare with the method that adopts chemical self assembly usually at present.But chemical method often needs to use violent reaction conditions such as organic reagent and HTHP, and environment is had bigger negative effect.
Summary of the invention
Technical problem to be solved by this invention is the preparation method that the Metal Palladium nano wire of a kind of environmental friendliness and controllable size is provided at the present situation of prior art.
The present invention solves the problems of the technologies described above the technical scheme that adopts: the preparation method of the Metal Palladium nano wire of this controllable size is characterized in that comprising the steps:
1. the preparation of palladium oxide nano particle:
A certain amount of palladium bichloride pressed powder is dissolved in the water, is mixed with certain density palladium chloride solution as required; The palladium chloride solution for preparing 20～30 ℃ of following hydrolysis 2.5～4 days, is obtained the palladium oxide nanoparticles solution of certain size;
2. the preparation of azelon:
Configuration concentration is that 0.5～2mg/ml, pH value are 1～3 insulin solutions, solution is placed on to cultivate in 65～90 ℃ insulating box in the centrifuge tube takes out after 20～30 hours, obtains nutrient solution; Get 4～6 microlitre nutrient solutions and drip on the mica sheet of the 1cm * 1cm that newly peels off, obtain depositing the mica sheet of azelon;
3. the palladium oxide nano wire is synthetic:
Get the palladium oxide nanoparticles solution that 1. 20-30 microlitre step prepares, dropping was cultivated 8～15 minutes on the mica sheet that deposits azelon in advance, washed the residual solution on surface then gently with deionized water, then in air, dry up with nitrogen, obtain the palladium oxide nano wire;
4. the reduction of palladium oxide:
The borine dimethyl amine that to get a certain amount of 40-50 microlitre concentration be 3～8mM drips to be had on the mica sheet of oxidation palladium nanometer wire in preparation, cultivates 20～40 minutes, with reduction of palladium oxide into palladium; With deionized water lavage specimens product surface, remove unnecessary borine dimethyl amine then, both can obtain the one-dimensional metal palladium nanometer wire of preliminary dimension after drying up with nitrogen.
Among the above-mentioned preparation method, the concentration of palladium chloride solution can be specifically selected according to the size of required one-dimensional metal palladium nanometer wire, that is to say, the concentration of palladium chloride solution can be arbitrarily, when the size of required Metal Palladium nano wire is big, can the high palladium chloride solution of working concentration, otherwise, need be with the concentration configuration of palladium bichloride a little bit smaller.
Preferably, the concentration of described palladium chloride solution is 0.1～50mM.The Metal Palladium nano wire prepared with the palladium chloride solution in this concentration range can satisfy most of demand.
More preferably, the concentration of described palladium chloride solution is 1～30mM.
The invention provides a kind of preparation method of Metal Palladium nano wire of novel concept, its concentration by control hydrolysis palladium chloride solution obtains the palladium oxide metal nanoparticle of different size, prepare the azelon combination at substrate surface then and in advance, form the palladium oxide nano wire of different-diameter, with reducing agent reduction of palladium oxide into palladium is obtained the one-dimensional metal palladium nanometer wire at last; The present invention is the synthetic Metal Palladium nano wire of template with the large biological molecule azelon, because the degradability of azelon, so this method is a kind of preparation method of environmental protection, and simple to operate; And by changing the concentration of palladium chloride solution, can obtain the one-dimensional metal palladium nanometer wire of different size, thereby realize the size Control to palladium nanometer wire.The diameter of Metal Palladium nano wire is from adjustable from 1-30nm.
Description of drawings
Fig. 1 is the AFM shape appearance figure of palladium oxide nano particle in the embodiment of the invention 1, and the scale among the figure is 1 micron;
Fig. 2 is fibrinous AFM shape appearance figure in the embodiment of the invention 1;
Fig. 3 is the AFM shape appearance figure of palladium oxide nano wire in the embodiment of the invention 1, and the scale among the figure is 1 micron, and lower right corner part is the partial enlarged drawing of Fig. 3 middle part square frame part.
The specific embodiment
Describe in further detail below in conjunction with the present invention of accompanying drawing embodiment.
Embodiment 1
1. the preparation of palladium oxide nano particle:
The palladium bichloride pressed powder is dissolved in the water, is mixed with the 2.5mM palladium chloride solution; The palladium chloride solution for preparing 25 ℃ of following hydrolysis 3 days, is obtained particle diameter and be the palladium oxide nanoparticles solution about nanometer, and the AFM shape appearance figure of this palladium oxide nano particle as shown in Figure 1.White round dot among Fig. 1 is the palladium oxide particle.
2. the preparation of azelon:
Configuration concentration is that 1mg/ml, pH value are 1.6 insulin solutions, solution is placed in the centrifuge tube to cultivate in 70 ℃ insulating box takes out after 25 hours, obtains nutrient solution; Get 5 microlitre nutrient solutions and drip on the mica sheet of newly peeling off, obtain depositing the mica sheet of azelon, obtain the uniform one dimension azelon of size.Its AFM shape appearance figure as shown in Figure 2.The elongated filament bar of white is the azelon of one dimension among Fig. 2, and the filamentous azelon of this one dimension will be as the biological template of synthetic palladium nanometer wire.
3. the palladium oxide nano wire is synthetic:
Palladium oxide nanoparticles solution 25 microlitres that 1. step is prepared drip on the mica sheet that deposits azelon in advance, cultivated 10 minutes, wash the residual solution on surface then with deionized water gently, then in air, dry up with nitrogen, obtain the palladium oxide nano wire; Its AFM shape appearance figure as shown in Figure 3.By the analysis of the micro-height map of atomic force, the diameter that obtains the palladium oxide nano wire is the 10-12 nanometer.
4. the reduction of palladium oxide:
The borine dimethyl amine of getting 20 microlitre 5mM drips to be had on the mica sheet of oxidation palladium nanometer wire in preparation, cultivates 30 minutes, with reduction of palladium oxide into palladium; With deionized water lavage specimens product surface, remove unnecessary borine dimethyl amine then, both can obtain the one-dimensional metal palladium nanometer wire of preliminary dimension after drying up with nitrogen.
Embodiment 2 to embodiment 6
Change the concentration of the palladium chloride solution of preparing, embodiment 2 to embodiment 6 is followed successively by 0.1,1,5,10 and 30mM, obtained the palladium oxide nano particle of different-grain diameter in 3 days 25 ℃ of following hydrolysis, the palladium oxide nanoparticle size is as shown in table 1, the palladium oxide nano particle of these different sizes and azelon in conjunction with after just obtained the palladium oxide nano wire of different-diameter, this is because the palladium oxide nano particle can only be adsorbed on the azelon, particle can not be deposited in owing to electrostatic interaction between particle, so the diameter of palladium oxide nano wire only depends on the size of palladium oxide particle.At last, the one dimension palladium metal nano wire of corresponding size will can be obtained with the borine dimethyl amine after the palladium oxide reduction.
Table 1
| Embodiment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Palladium bichloride concentration (mM) | 0.1 | 1 | 5 | 10 | 30 |
| The average diameter of palladium oxide particle (nm) | 0.5 | 4.3 | 19.8 | 22.5 | 31.3 |
Other content of embodiment 2 to embodiment 6 is identical with embodiment 1.
Claims (3)
1. the preparation method of the Metal Palladium nano wire of a controllable size is characterized in that comprising the steps:
1. the preparation of palladium oxide nano particle:
A certain amount of palladium bichloride pressed powder is dissolved in the water, is mixed with certain density palladium chloride solution as required; The palladium chloride solution for preparing 20～30 ℃ of following hydrolysis 2.5～4 days, is obtained the palladium oxide nanoparticles solution of certain size;
2. the preparation of azelon:
Configuration concentration is that 0.5～2mg/ml, pH value are 1～3 insulin solutions, solution is placed on to cultivate in 65～90 ℃ insulating box in the centrifuge tube takes out after 20～30 hours, obtains nutrient solution; Getting the dropping of 4～6 microlitre nutrient solutions is on the mica sheet of 1cm * 1cm at the area of newly peeling off, and obtains depositing the mica sheet of azelon;
3. the palladium oxide nano wire is synthetic:
Getting that palladium oxide nanoparticles solution that 1. 20-30 microlitre step prepare drips at the area that deposits azelon in advance is on the mica sheet of 1cm * 1cm, cultivated 8～15 minutes, wash the residual solution on surface then gently with deionized water, then in air, dry up with nitrogen, obtain the palladium oxide nano wire;
4. the reduction of palladium oxide:
The borine dimethyl amine of getting 40-50 microlitre concentration and be 3～8mM drips to be had on the mica sheet of oxidation palladium nanometer wire in preparation, cultivates 20～40 minutes, with reduction of palladium oxide into palladium; With deionized water lavage specimens product surface, remove unnecessary borine dimethyl amine then, both can obtain the one-dimensional metal palladium nanometer wire of preliminary dimension after drying up with nitrogen.
2. the preparation method of the Metal Palladium nano wire of controllable size according to claim 1, the concentration that it is characterized in that described palladium chloride solution is 0.1～50mM.
3. the preparation method of the Metal Palladium nano wire of controllable size according to claim 2, the concentration that it is characterized in that described palladium chloride solution is 1～30mM.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668579A (en) * | 2015-02-11 | 2015-06-03 | 燕山大学 | Method for preparing palladium nano wires by use of heliothis armigera nuclear polyhedrin |
| CN105414559A (en) * | 2015-11-27 | 2016-03-23 | 燕山大学 | Manufacturing method of superfine single crystal palladium nanowire |
| CN105689725A (en) * | 2016-02-04 | 2016-06-22 | 中国科学院金属研究所 | Method for preparing metal palladium or palladium alloy nanowires |
| CN106041114A (en) * | 2016-05-20 | 2016-10-26 | 燕山大学 | Preparation method of Pt-based alloy nanowire |
| CN106975754A (en) * | 2016-12-30 | 2017-07-25 | 西安交通大学青岛研究院 | A kind of preparation method of palladium nanometer wire |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1911782A (en) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | Preparation method of palladium nanometer wire oldered array material |
| CN101850969A (en) * | 2010-02-11 | 2010-10-06 | 浙江工业大学 | Method for synthesizing boron carbide nano wires by using plant fibers |
-
2013
- 2013-04-27 CN CN2013101558769A patent/CN103252501A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911782A (en) * | 2006-07-21 | 2007-02-14 | 东莞理工学院 | Preparation method of palladium nanometer wire oldered array material |
| CN101850969A (en) * | 2010-02-11 | 2010-10-06 | 浙江工业大学 | Method for synthesizing boron carbide nano wires by using plant fibers |
Non-Patent Citations (3)
| Title |
|---|
| LONGGAI ZHANG ETAL: "Insulin amyloid fibrils : An excellent platform for controlled synthesis of ultrathin superlong platinum nanowires with high electrocatalytic activity", 《JOURNAL OF CHEMISTRY SOCIETY》 * |
| RALF JANSEN ET AL: "Amyloidgenic self-assembly of insulin aggregates probed by high resolution atomic force microscopy", 《BIOPHYSICAL JOURNAL》 * |
| XINGFEI ZHOU ET AL: "Biotemplated fabrication of size controlled palladium nanopaticle chains", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104668579A (en) * | 2015-02-11 | 2015-06-03 | 燕山大学 | Method for preparing palladium nano wires by use of heliothis armigera nuclear polyhedrin |
| CN105414559A (en) * | 2015-11-27 | 2016-03-23 | 燕山大学 | Manufacturing method of superfine single crystal palladium nanowire |
| CN105689725A (en) * | 2016-02-04 | 2016-06-22 | 中国科学院金属研究所 | Method for preparing metal palladium or palladium alloy nanowires |
| CN106041114A (en) * | 2016-05-20 | 2016-10-26 | 燕山大学 | Preparation method of Pt-based alloy nanowire |
| CN106975754A (en) * | 2016-12-30 | 2017-07-25 | 西安交通大学青岛研究院 | A kind of preparation method of palladium nanometer wire |
| CN106975754B (en) * | 2016-12-30 | 2019-08-30 | 杭州罗松贸易有限公司 | A kind of preparation method of palladium nanometer wire |
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Application publication date: 20130821 |