CN101871122B - Preparation method of Pt-endpoint FeNi nano rod - Google Patents
Preparation method of Pt-endpoint FeNi nano rod Download PDFInfo
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- CN101871122B CN101871122B CN2010101978973A CN201010197897A CN101871122B CN 101871122 B CN101871122 B CN 101871122B CN 2010101978973 A CN2010101978973 A CN 2010101978973A CN 201010197897 A CN201010197897 A CN 201010197897A CN 101871122 B CN101871122 B CN 101871122B
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Abstract
The invention belongs to the technical field of nano materials, in particular to a preparation method of a Pt-endpoint FeNi nano rod. In the invention, a template is formed by taking hydrothermal synthesis as a reaction system through adding surfactant oleic acid, and sodium oleate is used as a reaction medium and is reduced and induced under the action of polyalcohol to obtain a one-dimensional superstructure with noble metal Pt as an endpoint. The invention has simple preparation method, high yield, no environmental pollution and low cost and is easy to realize for future industrial production.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of Pt endpoint FeNi nano rod.
Background technology
One dimension ferrous metals nano material not only has the various special effectses of common nanoparticle; And have unique shape anisotropy and a magneticanisotropy; Be the important constituent element of constructing the function solenoid material, have important use in fields such as high density magnetic recording, sensitive components, absorption of electromagnetic wave, catalyzer, medical science and Biofunctional materials.Wherein the functional material that synthesizes a new generation of Fe base Nanoalloy material has been opened up new approach.
Fe, Co, the Ni transition element is considered to element the most outstanding in above field, because its unidimensional material nanotube for example; Nano wire has many excellent properties, learns physics and chemical process after deliberation and be applied on these materials of preparation ball milled for example; Electrochemical deposition, laser ablation, chemical vapour deposition; Sputtering method, spray method, chemical reduction method or the like.At present one-dimensional material synthetic aspect; The main electrodip process that adopts, but because electrodip process too is limited by template, and method is single; Complex process; Therefore, how obtaining unidimensional FeNi alloy nano-material with a kind of simple controlled method, is a significant research topic.
Summary of the invention
The object of the present invention is to provide a kind of, non-environmental-pollution, with low cost, method simply has the preparation method of the Pt endpoint FeNi nano rod of special construction.
The Pt endpoint FeNi nano rod that the present invention proposes; Utilize hydro-thermal synthetic as reaction system; Form template through adding tensio-active agent oleic acid, as reaction medium, reduction is induced and is obtained having the one dimension superstructure that precious metals pt is an end points under the effect of polyvalent alcohol with sodium oleate.
The preparation method of the Pt endpoint FeNi nano rod that the present invention proposes, concrete steps are following:
(1) with nickeliferous inorganic salt or contain nickel complex, iron content inorganic salt or contain iron complex and platiniferous inorganic salt or contain platinum complex and be dissolved in the ethanol, add sodium oleate, stirring, add the mixing solutions of oleic acid and terepthaloyl moietie again, be stirred to solid and dissolve fully; Wherein: nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mole ratio that contains the total mole number and the platiniferous inorganic salt of iron complex or contain platinum complex are 95: 5～99: 1; Sodium oleate and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of iron complex are 2: 1～5: 1; Oleic acid and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of substance of iron complex are 1: 15～1: 50; Ethanol and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of substance of iron complex are 30: 1～80: 1;
(2) terepthaloyl moietie is joined in step (1) products therefrom, whole mixed system is moved into autoclave, be heated to 200 ℃ with certain temperature rise rate; Insulation is 10-15 minute under this temperature; Reaction is cooled to room temperature after finishing, washing; Spinning obtains final product black alloy nanometer rod; Wherein the mol ratio of terepthaloyl moietie and molysite and the total amount of nickel salt is 15: 1～40: 1.
Among the present invention, said iron content inorganic salt or contain iron complex and nickeliferous inorganic salt or contain the checking and writing off than being 5 of nickel complex: 1-1: 5.
Among the present invention, said iron content inorganic salt be in iron protochloride, iron(ic)chloride or the iron nitrate etc. any, contain iron complex and be in ironic oxalate, Ferrox, acetyl acetone iron (II) or the acetyl acetone iron (III) etc. any; Said nickeliferous inorganic salt be in chlorine nickelous chloride or the nickelous nitrate etc. any, contain nickel complex be in ironic oxalate or the nickel acetate etc. any; The platiniferous inorganic salt be in Platinic chloride, platinum dichloride or the Tetrachloroplatinum etc. any, contain platinum complex and be dichloride dicyan phenylbenzene and close in platinum (II) or the acetyl acetone platinum (II) etc. any.
Among the present invention, stir described in the step (1) in ultrasonic concussion or the magnetic agitation etc. any.
Among the present invention, temperature rise rate is 1 ℃/minute～5 ℃/minute described in the step (2), is not higher than 5 ℃/minute.
Among the present invention, the alternately washing of deionized water, absolute ethyl alcohol and chloroform is used in washing described in the step (2).
Among the present invention, the spinning rotating speed is 1500-6000 rev/min described in the step (2), and the time is 15-20 minute.
Structure, pattern, composition to the inventive method products therefrom characterize, and can select for use transmission electron microscope (TEM), energy chromatographic instrument (EDS) etc. to characterize respectively, and TEM characterizes the microtexture of nanometer rod, and EDS shows the moity of product.
Utilize the inventive method to prepare the size homogeneous, have the FeNi nanometer rod of the Pt end of special construction, have good magnetic, character such as catalysis.
The inventive method is easy to operate, easy to control.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the product of embodiment 1.
Fig. 2 is the transmission electron microscope picture of the product of embodiment 2.
Fig. 3 is the transmission electron microscope picture of the product of embodiment 3
Fig. 4 is a products therefrom energy chromatogram (EDS) among the embodiment 1.
Embodiment
Further specify the present invention through embodiment below.
Embodiment 1:
The first step is with 0.3mmol Fe
2(C
2O
4)
35H
2O, 0.3mmol NiCl
26H
2O and 6 * 10
-7MmolH
2PtCl
66H
2O is dissolved in the 2ml absolute ethyl alcohol fully, adds the 0.02g sodium oleate then, ultrasonic concussion 10-20 minute.
Second goes on foot, and adds terepthaloyl moietie and the oleic mixing solutions of 2ml of 4ml again, then whole mixed system is transferred in the autoclave; Rise to 200 ℃ with 2 ℃/minute temperature rise rates from room temperature; And in muffle furnace, under 200 ℃ condition, being incubated 15 minutes, reaction is cooled to room temperature after finishing.
The 3rd step washed out reaction product with the 10ml ethanolic soln, the black powder deposition in the product mixed solution, occurs.The supersound process mixed solution disperses it as far as possible in ethanolic soln, and under 5000 rev/mins speed centrifugal 10 minutes then, discard supernatant liquid, the deionized water that uses the same method, absolute ethyl alcohol, chloroform alternately wash, centrifugal 5-10 time.Final sample is scattered in the absolute ethyl alcohol, and sample is analyzed.
Can find out that by transmission electron microscope (accompanying drawing 1) product has tangible Pt end points, and be the one-dimensional rod-like structure that a gained group bunch shape nanometer rod diameter is about 30nm, proves that product is a nano level.Can find out that by energy chromatogram (EDS, accompanying drawing 4) product consists of Fe, the copper mesh substrate that Ni, Pt, and each product presents different peak heights because of the content difference, the Cu among the figure use during for test causes.
Embodiment 2:
With 0.4mmol Fe
2(C
2O
4)
35H
2O, 0.2mmol NiCl
26H
2O and 6 * 10
-7Mmol H
2PtCl
66H
2O is dissolved in the 2ml absolute ethyl alcohol fully, adds the 0.02g sodium oleate then, ultrasonic concussion 10-20 minute; Add the oleic mixing solutions of 4ml terepthaloyl moietie and 2ml again, then whole mixed system is transferred in the autoclave, rise to 200 ℃ from room temperature with 5 ℃/minute temperature rise rates; And in muffle furnace, under 200 ℃ condition, be incubated 10 minutes; Reaction is cooled to room temperature after finishing, and all the other steps are operated by embodiment 1.
Can find out that by transmission electron microscope (accompanying drawing 2) product has tangible Pt end points, and be the one-dimensional rod-like structure, gained nanometer rod diameter is about 60nm, proves that product is a nano level.
Embodiment 3:
With 0.1mmol Fe
2(C
2O
4)
35H
2O, 0.5mmol NiCl
26H
2O and 6 * 10
-7Mmol H
2PtCl
66H
2O is dissolved in the 2ml absolute ethyl alcohol fully, adds the 0.02g sodium oleate then, ultrasonic concussion 10-20 minute; Add the oleic mixing solutions of 4ml terepthaloyl moietie and 2ml again, then whole mixed system is transferred in the autoclave, rise to 200 ℃ from room temperature with 2 ℃/minute temperature rise rates; And in muffle furnace, under 200 ℃ condition, be incubated 15 minutes; Reaction is cooled to room temperature after finishing, and all the other steps are operated by embodiment 1.
Can find out that by transmission electron microscope (accompanying drawing 3) product has tangible Pt end points, and be the one-dimensional rod-like structure, the group of a gained bunch shape nanometer rod diameter is about 60nm, proves that product is a nano level.
Claims (4)
1. the preparation method of a Pt endpoint FeNi nano rod is characterized in that concrete steps are following:
(1) with nickeliferous inorganic salt or contain nickel complex, iron content inorganic salt or contain iron complex and platiniferous inorganic salt or contain platinum complex and be dissolved in the ethanol, add sodium oleate, stirring, add the mixing solutions of oleic acid and terepthaloyl moietie again, be stirred to solid and dissolve fully; Wherein: nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mole ratio that contains the total mole number and the platiniferous inorganic salt of iron complex or contain platinum complex are 95: 5～99: 1; Sodium oleate and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of iron complex are 2: 1～5: 1; Oleic acid and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of substance of iron complex are 1: 15～1: 50; Ethanol and nickeliferous inorganic salt or contain nickel complex and iron content inorganic salt or the mol ratio that contains total amount of substance of iron complex are 30: 1～80: 1;
(2) terepthaloyl moietie is joined in step (1) products therefrom, whole mixed system is moved into autoclave, be heated to 200 ℃ with certain temperature rise rate; Insulation is 10-15 minute under this temperature; Reaction is cooled to room temperature after finishing, washing; Spinning obtains final product black alloy nanometer rod; Wherein the mol ratio of terepthaloyl moietie and molysite and the total amount of nickel salt is 15: 1～40: 1; Said temperature rise rate is 1 ℃/minute～5 ℃/minute, is not higher than 5 ℃/minute; The spinning rotating speed is 1500-6000 rev/min, and the time is 15-20 minute.
2. the preparation method of Pt endpoint FeNi nano rod according to claim 1; It is characterized in that said iron content inorganic salt be in iron protochloride, iron(ic)chloride or the iron nitrate any, contain iron complex and be in ironic oxalate, Ferrox, acetyl acetone iron (II) or the acetyl acetone iron (III) any; Said nickeliferous inorganic salt be in nickelous chloride or the nickelous nitrate any, contain nickel complex and be in ironic oxalate or the nickel acetate any; The platiniferous inorganic salt be in Platinic chloride, platinum dichloride or the Tetrachloroplatinum any, contain platinum complex and be dichloride dicyan phenylbenzene and close in platinum (II) or the acetyl acetone platinum (II) any.
3. the preparation method of Pt endpoint FeNi nano rod according to claim 1, it is characterized in that stirring described in the step (1) is ultrasonic concussion or magnetic agitation.
4. the preparation method of Pt endpoint FeNi nano rod according to claim 1 is characterized in that the use of washing described in the step (2) deionized water, absolute ethyl alcohol and alternately washing of chloroform.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101954489B (en) * | 2010-11-01 | 2012-12-05 | 同济大学 | Method for preparing heterostructure FeCo-Pt alloy nanorod |
| CN102166518B (en) * | 2011-03-21 | 2013-01-16 | 天津大学 | Method for preparing electrocatalytic noble metal nanomaterial with three-dimensional network structure |
| CN102389983B (en) * | 2011-11-09 | 2014-04-23 | 西北大学 | Synthesis method of noble metal nano particles |
| CN103128305B (en) * | 2011-11-28 | 2015-03-04 | 同济大学 | Method for preparing Ag/Co magnetic nano composites |
| CN105710384B (en) * | 2015-11-04 | 2017-12-29 | 中国科学院上海高等研究院 | 1-dimention nano bimetallic alloy with hexagon head of a nail structure and preparation method thereof |
| CN105833862B (en) * | 2016-03-31 | 2018-09-28 | 湖南省吉安特技术有限公司 | A kind of preparation method and application of nano oxidized platinum catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903427A (en) * | 2005-07-28 | 2007-01-31 | 中国科学院大连化学物理研究所 | Method for preparing metal ruthenium nano-wire |
| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
| CN101342598A (en) * | 2008-08-28 | 2009-01-14 | 上海交通大学 | Method for preparing metallic nickel nano-wire |
| CN101451270A (en) * | 2008-12-11 | 2009-06-10 | 常振宇 | Large scale preparation of noble metal nano wire |
| CN101530923A (en) * | 2009-02-25 | 2009-09-16 | 同济大学 | Method for preparing Fe-Ni-Pt alloy nanorod |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903427A (en) * | 2005-07-28 | 2007-01-31 | 中国科学院大连化学物理研究所 | Method for preparing metal ruthenium nano-wire |
| CN101289228A (en) * | 2008-06-03 | 2008-10-22 | 浙江理工大学 | Method for preparing porous zinc ferrite nano-rods |
| CN101342598A (en) * | 2008-08-28 | 2009-01-14 | 上海交通大学 | Method for preparing metallic nickel nano-wire |
| CN101451270A (en) * | 2008-12-11 | 2009-06-10 | 常振宇 | Large scale preparation of noble metal nano wire |
| CN101530923A (en) * | 2009-02-25 | 2009-09-16 | 同济大学 | Method for preparing Fe-Ni-Pt alloy nanorod |
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