CN102554252A - Synthesizing method of porous bimetal nanostructure - Google Patents
Synthesizing method of porous bimetal nanostructure Download PDFInfo
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- CN102554252A CN102554252A CN2010105946223A CN201010594622A CN102554252A CN 102554252 A CN102554252 A CN 102554252A CN 2010105946223 A CN2010105946223 A CN 2010105946223A CN 201010594622 A CN201010594622 A CN 201010594622A CN 102554252 A CN102554252 A CN 102554252A
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Abstract
The invention discloses a mild synthesizing method of a porous bimetal nanostructure, which comprises steps of dissolving mixed metal precursor resources in a glucosan water solution, and reacting for at least three hours in a closed pressure reactor under 70-100 DEG C. The invention establishes a method for synthesizing the porous bimetal nanostructure by a one-step reaction, the required temperature is low, preparation conditions are mild, and the operation is simple and convenient to implement; chemical components of a product are controllable; and with different chemical components, such compounds prepared by the method show different catalytic performance.
Description
Technical field:
The invention belongs to the solid mineral material preparing technical field, particularly the preparation method of porous bimetal nano structure.
Background technology:
Gold (Au), palladium noble metals such as (Pd) have specific electronic structure, and demonstrate very important chemical catalysis reactivity worth, simultaneously because it has very high selection catalytic reaction activity, therefore have purposes very widely.Although the selectivity of noble metal catalyst such as Au, Pd is high, catalytic applications is extensive since its cost an arm and a leg, shortage of resources, this in certain degree limit being widely used of these noble metals.Therefore utilize relatively cheap silver (Ag) and base metal to substitute or partly substitute various corresponding noble metals and have important use value.Simultaneously, because silver and base metal can form bimetallic or the alloy with ad hoc structure with noble metals such as Au, Pd respectively, it in theory also has the research meaning.Can at high temperature form the AuAg unlimited solid solution with gold like silver, then can form some steady structures that are situated between at low temperatures.The porous Raney's nickel also is used to replace metal Pd to be used as catalyst for another example, and shows tangible catalytic effect, but owing to Raney's nickel needs under 800 degrees celsius, prepare, and metallic nickel is comparatively vivaciously and not too stable easily, and this has also limited the use of metallic nickel.Behind metal Ni and Pd formation alloy,, thereby improved widely Ni stability and catalytic cycle cycle in the NiPd bimetallic alloy because its solid solution phase is comparatively stable on thermodynamics.The NiPd alloy of recent 30 nanometers (nm) can prepare (Rare Metals Materials and engineering, 2010,39 through the polyalcohol method of reducing; 153-156); Simultaneously, the NiPd ultrafine particle catalyst can also pass through arc discharge method (number of patent application CN94115078.X, notification number CN1105289; Number of patent application CN94218594.3, notification number CN2219170), and reducing process heating crystallization (number of patent application CN200710056636.8, notification number CN101007280) makes.In addition, NiPd nanometer film and NiPd nano wire also utilize pulse laser induced (Tianjin Science & Engineering Univ, 2002, bullets 0400410653) and AAO electrochemical deposition method to make (Yue Erhong, Hunan University's academic dissertation, 2007 respectively; Yuan Juan, Hunan University's academic dissertation, 2004).These reports are conceived to the preparation of this type of nano-grain or film, and said method is not all prepared porous NiPd nanostructured.And the preparation condition relative complex of above-mentioned synthetic method, as using means such as high temperature, electrochemical deposition, laser or arc discharge, preparation powder process exists energy consumption height, big, the unequal deficiency of size distribution of granularity.
Summary of the invention:
The objective of the invention is to propose a kind of bimetal nano preparation methods, have the deficiency that complicated synthetic technology energy consumption is big, flow process is complicated now, and realize the preparation of bimetallic porous nanometer structure to overcome.
Porous bimetal nano material of the present invention is characterized in that partly substituting noble metal with base metal, is mainly the nano material bimetallic of Co-Au, Cu-Au, Ni-Au and four kinds of loose structures of Ni-Pd.
Porous bimetal nano preparation methods among the present invention is characterized in that: utilize polymers dextran (dextran) to be dissolved in the 15-20mL pure water, and be stirred to dissolving fully.Then with a certain amount of gold chloride (HAuCl
4) or the PdCl of acidifying
2Drop to and be stirred to dissolving fully in the above-mentioned solution, base metal Co, Cu, the Ni metal chloride that will be several times as much as noble metal Au simultaneously are added drop-wise to and the above-mentioned 5-10 minute moon of solution for continuous stirring system are thoroughly mixed.Then above-mentioned clear solution is transferred in the teflon-lined agitated reactor, reaction is no less than 3h under 70-100 ℃ of condition, can obtain the product of the porous bimetal nano material of crystallization.
The porous bimetal nano material that the present invention proposes is under the condition of gentleness, to obtain, and utilizes glucan can effectively promote the formation of bimetallic product loose structure at temperate condition as molecular template reagent.The ratio of bimetallic product metering simultaneously, pattern, size and micro-structural can corresponding adjustment and controls by the variation of experiment condition.
Because the present invention has taked the auxiliary synthetic technical measures of glucan, has overcome the shortcoming that existing high temperature synthetic technology energy consumption is big, operating process is complicated, has preparation condition gentleness, simple advantage and the good effect of operating process.The reaction incipient stage can be adopted common beaker, heated and stirred on agitator.Treat after solution mixes it to be changed over to the teflon-lined agitated reactor; Heating is 70 ℃-100 ℃ in baking oven; Heating-up temperature is all than synthetic this type of bimetallic temperature low (>=200 ℃) of bibliographical information in the past, and do not need deposition means such as electrochemistry, laser, arc discharge.Adopt the chemical composition of bimetallic product of the inventive method preparation controlled: promptly when the proportioning of the amount of substance of change reactant, can obtain the different bimetal nano material of element ratio.Along with the difference of its chemical composition, corresponding catalytic property also can change to some extent.Therefore, through regulating the chemical composition of synthetic bimetal nano material, can regulate and control the catalytic performance of this material.
The specific embodiment:
Below be some embodiments of the present invention.
Synthesizing of embodiment 1.Co-Au bimetal nano structure
In the 50mL beaker, the 0.023g glucan is dissolved in the 20mL pure water, after being stirred to glucan and dissolving fully, drip 0.2mL 24mM gold chloride (HAuCl
4) solution, on constant temperature blender with magnetic force, stir down, till the liquid of solution clear in 20-55 ℃.And then in above-mentioned solution, add 0.048mmol six hydration Cobalt Chloride (0.015g) stirring and dissolving.Subsequently above-mentioned solution is transferred to and has in the teflon-lined agitated reactor; And with agitated reactor tighten place baking oven in 70-100 ℃ down heating be no less than 3 hours; The gained sample is put into baking oven with distilled water and absolute ethanol washing after repeatedly dries, and promptly gets target product.
Adopt the analyses of X-ray powder diffraction (XRD) and ESEM (SEM) to show that product is the nanocrystalline of crystalline state and has loose structure.Power spectrum (EDS) analysis shows that product is made up of Elements C o and Au.
Synthesizing of embodiment 2.Cu-Au bimetal nano structure
In the 50mL beaker, the 0.023g glucan is dissolved in the 20mL pure water, after being stirred to glucan and dissolving fully, drip 0.2mL 24mM gold chloride (HAuCl
4) solution, on constant temperature blender with magnetic force, stir down, till the liquid of solution clear in 20-55 ℃.And then in above-mentioned solution, add 0.048mmol cupric sulfate pentahydrate (0.013g) stirring and dissolving.Subsequently above-mentioned solution is transferred to and has in the teflon-lined agitated reactor; And agitated reactor tightened place baking oven in 70-100 ℃ of following heating 8-12h; The gained sample is put into baking oven with distilled water and absolute ethanol washing after repeatedly dries, and promptly gets target product.
Adopt the analyses of X-ray powder diffraction (XRD) and ESEM (SEM) to show that product is the nanocrystalline of crystalline state and has loose structure.Power spectrum (EDS) analysis shows that product is made up of element Cu and Au.
Synthesizing of embodiment 3.Ni-Au bimetal nano structure
In the 50mL beaker, the 0.023g glucan is dissolved in the 20mL pure water, after being stirred to glucan and dissolving fully, drip 0.2mL 24mM gold chloride (HAuCl
4) solution, on constant temperature blender with magnetic force, stir down, till the liquid of solution clear in 20-55 ℃.And then in above-mentioned solution, add 0.048mmol Nickel dichloride hexahydrate (0.015g) stirring and dissolving.Subsequently above-mentioned solution is transferred to and has in the teflon-lined agitated reactor; And agitated reactor tightened place baking oven in 70-100 ℃ of following heating 8-12h; The gained sample is put into baking oven with distilled water and absolute ethanol washing after repeatedly dries, and promptly gets target product.
Adopt the analyses of X-ray powder diffraction (XRD) and ESEM (SEM) to show that product is the nanocrystalline of crystalline state and has loose structure.Power spectrum (EDS) analysis shows that product is made up of element Ni and Au.
Synthesizing of embodiment 4.Ni-Pd bimetal nano structure
In the 50mL beaker, the 0.023g glucan is dissolved in the 20mL pure water, after being stirred to glucan and dissolving fully, drip the palladium bichloride (PdCl of 0.1mL 48mM acidifying
2) solution, on constant temperature blender with magnetic force, stir down, till the liquid of solution clear in 20-55 ℃.And then in above-mentioned solution, add 0.048mmol Nickel dichloride hexahydrate (0.015g) stirring and dissolving.Subsequently above-mentioned solution is transferred to and has in the teflon-lined agitated reactor; And agitated reactor tightened place baking oven in 70-100 ℃ of following heating 8-12h; The gained sample is put into baking oven with distilled water and absolute ethanol washing after repeatedly dries, and promptly gets target product.
Adopt the analyses of X-ray powder diffraction (XRD) and ESEM (SEM) to show that product is the nanocrystalline of crystalline state and has loose structure.Power spectrum (EDS) analysis shows that product is made up of element Ni and Pd.
Claims (2)
1. porous bimetal nano material of the present invention is characterized in that partly substituting noble metal with base metal, is mainly the nano material bimetallic of Co-Au, Cu-Au, Ni-Au and four kinds of loose structures of Ni-Pd.
2. the porous bimetal nano preparation methods among the present invention is characterized in that: utilize polymers dextran (dextran) to be dissolved in the 15-20mL pure water, and be stirred to dissolving fully.Then with a certain amount of gold chloride (HAuCl
4) or the PdCl of acidifying
2Drop to and be stirred to dissolving fully in the above-mentioned solution, base metal Co, Cu, the Ni metal chloride that will be several times as much as noble metal Au simultaneously are added drop-wise to and the above-mentioned 5-10 minute moon of solution for continuous stirring system are thoroughly mixed.Then above-mentioned clear solution is transferred in the teflon-lined agitated reactor, reaction is no less than 3h under 70-100 ℃ of condition, can obtain the product of the porous bimetal nano material of crystallization.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102896328A (en) * | 2012-10-30 | 2013-01-30 | 西安交通大学 | Method for continuously preparing colloid PdM (M=Pt, Au) alloy nano particles |
| CN104177665A (en) * | 2014-08-25 | 2014-12-03 | 武汉大学 | Gold nanoparticle/beta-glucan compound, and preparation method and application thereof |
| CN105618784A (en) * | 2016-01-08 | 2016-06-01 | 浙江大学 | Preparation method for dendritic copper-palladium nanocrystalline alloy and product of preparation method |
| CN106180754A (en) * | 2016-08-10 | 2016-12-07 | 陕西师范大学 | A kind of method of simple preparation network structure Au Ag bimetal nano particles thin film |
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| US20020177143A1 (en) * | 2001-05-25 | 2002-11-28 | Mirkin Chad A. | Non-alloying core shell nanoparticles |
| CN1686649A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Preparation method of nuclear shell structured nano-gold copper powder |
| CN101157043A (en) * | 2007-09-26 | 2008-04-09 | 山东大学 | A nucleocapsid type nanometer stephanoporate metal catalyst as well as its preparing method |
| CN101683693A (en) * | 2008-09-25 | 2010-03-31 | 三星电机株式会社 | Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed |
| US20100251856A1 (en) * | 2009-04-03 | 2010-10-07 | Venugopal Santhanam | Methods for preparing metal and metal oxide nanoparticles |
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2010
- 2010-12-17 CN CN2010105946223A patent/CN102554252A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020177143A1 (en) * | 2001-05-25 | 2002-11-28 | Mirkin Chad A. | Non-alloying core shell nanoparticles |
| CN1686649A (en) * | 2005-04-26 | 2005-10-26 | 黄德欢 | Preparation method of nuclear shell structured nano-gold copper powder |
| CN101157043A (en) * | 2007-09-26 | 2008-04-09 | 山东大学 | A nucleocapsid type nanometer stephanoporate metal catalyst as well as its preparing method |
| CN101683693A (en) * | 2008-09-25 | 2010-03-31 | 三星电机株式会社 | Method for preparing metal nanoparticles using matal seed and metal nanoparticles comprising metal seed |
| US20100251856A1 (en) * | 2009-04-03 | 2010-10-07 | Venugopal Santhanam | Methods for preparing metal and metal oxide nanoparticles |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102896328A (en) * | 2012-10-30 | 2013-01-30 | 西安交通大学 | Method for continuously preparing colloid PdM (M=Pt, Au) alloy nano particles |
| CN104177665A (en) * | 2014-08-25 | 2014-12-03 | 武汉大学 | Gold nanoparticle/beta-glucan compound, and preparation method and application thereof |
| CN105618784A (en) * | 2016-01-08 | 2016-06-01 | 浙江大学 | Preparation method for dendritic copper-palladium nanocrystalline alloy and product of preparation method |
| CN106180754A (en) * | 2016-08-10 | 2016-12-07 | 陕西师范大学 | A kind of method of simple preparation network structure Au Ag bimetal nano particles thin film |
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Application publication date: 20120711 |