CN107755682A - A kind of method and application that metal nanometer line is converted into nanosphere - Google Patents
A kind of method and application that metal nanometer line is converted into nanosphere Download PDFInfo
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- CN107755682A CN107755682A CN201710851596.XA CN201710851596A CN107755682A CN 107755682 A CN107755682 A CN 107755682A CN 201710851596 A CN201710851596 A CN 201710851596A CN 107755682 A CN107755682 A CN 107755682A
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Abstract
A kind of method that metal nanometer line is converted into nanosphere, including：Electro-deposition prepares metal hybrid nano wire；Precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, 2h is reacted under conditions of 60 DEG C, that is, obtains monometallic nanosphere.The present invention synthesizes the nanosphere of different geometrical morphologies and chemical composition by regulating and controlling reducing agent species and precursor solution.It is expected to construct other nano materials that the nano wire of electro-deposition can be converted into nanosphere with this general method, high performance electrocatalysis material and other nanosecond science and technology applied to future.Nanosphere prepared by this method has the advantages that uniform particle sizes and controllable, method is simply and high with universality, short preparation period and yield.Have wide practical use and potential learning value in terms of the fuel-cell catalyst and other energy storage materials in future by the metal nanoparticle synthesized by this efficient preparation technology.
Description
Technical field
The invention belongs to electrochemical deposition to prepare nano material and applied field technical field.More particularly to aoxidizing
A kind of hybridized nanowire of electrochemical method electro-deposition, the conjunction that then will have been synthesized by a stage reduction method again are used in aluminum dipping form plate hole
The method that nanowires of gold is converted into globular nanostructures.
Background technology
Spherical nanostructured has important scientific research value, can be widely applied to catalysis, optics, microelectronics,
The field such as magnetics and biomarker.
Traditional method for preparing nano particle generally includes chemical reduction method, hydro-thermal method, gas evaporation method and solvent heat
Method etc., but the shortcomings of preparation technology is complicated, manufacturing cycle is longer be present, aoxidized at present using electrochemical deposition method
Deposit alloy nano wire in aluminum alloy pattern plate, but be changed into by the use of the nano wire prepared as elementary cell by a stage reduction method
Spherical nanostructured does not have been reported that also.
The content of the invention
The present invention seeks to solve present in Conventional nano particulate production preparation technology is complicated, manufacturing cycle compared with
Long, the problems such as product morphology is uneven, and provide with reference to traditional nano wire technology of preparing a kind of general by metal nano
The method that line is converted to nanosphere.
The present invention synthesizes receiving for different geometrical morphologies and chemical composition by regulating and controlling reducing agent species and precursor solution
Rice ball.It is expected to construct other nano materials that the nano wire of electro-deposition can be converted into nanosphere with this general method,
Applied to following high performance electrocatalysis material and other nanosecond science and technology.By carrying out electrification to the 5nm Pt nanoparticles of preparation
Test is learned, we show that the Pt nanoparticle prepared with reducing process has, stability higher than business platinum carbon catalyst activity more
Good performance, is expected to be applied to fuel-cell catalyst of future generation.
To achieve the above object, the invention discloses following technical scheme：
A kind of method that metal nanometer line is converted into nanosphere, it is characterised in that carried out by the steps：
（1）Electro-deposition prepares metal hybrid nano wire；Described hybridized nanowire refers to that platinum bismuth hybridized nanowire or palladium bismuth are received
Rice noodles；
（2）Precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, 2h is reacted under conditions of 60 DEG C, i.e.,
Obtain monometallic nanosphere；
Described precursor solution refers to H2PtCl6·6H2O or PdCl2Solution；
Described reducing agent refers to ascorbic acid or NaBH4；
The composition of described monometallic nanosphere by the composition of previously prepared hybridized nanowire and the species of precursor solution Lai
Determine；The particle diameter of described monometallic nanosphere is regulated and controled by the species of reducing agent.
When the ascorbic acid using week reduction is as reducing agent, the particle diameter of the monometallic nanosphere of preparation is 160nm,
And " whisker " like structure is presented in surface；As the NaBH using strong reducing property4During as reducing agent, prepared monometallic nanosphere
Particle diameter is 5nm, and rough surface.
Work as step（2）Described precursor solution is H2PtCl6·6H2O, it is resulting during described reducing agent ascorbic acid
Monometallic nanosphere be particle diameter 160nm platinum nanosphere, and surface present " whisker " like structure；When using strong reducing property
NaBH4During as reducing agent, the particle diameter 5nm of prepared platinum nanosphere, and rough surface.
The specific preparation process of monometallic platinum nanosphere of the present invention is as follows：
(1) acquisition of alumina formwork
First time anodic oxidation：By high-purity aluminium flake in 0.3 M oxalic acid solution with 50 V DC voltages anodic oxidation 6 hours,
Then soaked 6 hours in 60 DEG C of 6 wt% phosphoric acid and the mixed solution of 1.8 wt% chromic acid, to remove the oxygen of surface imperfection
Change aluminium film；
Second of anodic oxidation：With 50 V DC voltages in 0.3 M oxalic acid solutions Anodic Oxidation 12 hours, then with supersaturation
SnCl4Solution removes the unoxidized aluminium in the back side, then erodes the aluminum oxide obstacle positioned at bottom hole portion with 5 wt% phosphoric acid solution
Layer, obtains the alumina formwork of two sides through hole；
(2) gold is steamed on the surface of alumina formwork
By adjusting the parameter of ion sputtering instrument, the golden film for being 200 nm in a face evaporation thickness of alumina formwork, make golden film
The one end in alumina formwork hole is completely covered, to ensure that nano wire can be obtained by the method for electrochemical deposition；
(3) using optimization electro-deposition techniques synthesis platinum bismuth nano-wire
With reference to Chang Rong, synthesis technique (the Rong Chang, Lijun of et al. platinum electrodeposition palladium copper ternary nano lines
Zheng, Chengwen Wang, Dachi Yang, Gaixia Zhang and Shuhui Sun, Appl. Catal.
B-Environ., 2017,211,205-211.), we have synthesized platinum bismuth hybridized nanowire using similar technique.
(4) one stage reduction methods prepare platinum nanosphere
0.005M H will be added in the pre-synthesis platinum bismuth nano-wire of step (3)2PtCl6·6H2O solution, adds ascorbic acid
Reduced, mixed solution is placed in air dry oven after reacting 2h under conditions of 60 DEG C, cleaned repeatedly with deionized water
Obtain platinum nanosphere.
When the hybridized nanowire of electro-deposition is palladium bismuth nano-wire, presoma 0.005M will be added in palladium bismuth nano-wire
PdCl2Solution and reducing agent ascorbic acid, after reacting 2h under conditions of 60 DEG C, what is obtained is shaggy monometallic palladium
Nanosphere.
The present invention further discloses using by metal nanometer line be converted into nanosphere method prepare nanosphere with
Application in terms of fuel-cell catalyst, experimental result are shown：This method has that preparation technology is simple, controllable nanostructured
Particle size, it is reproducible the advantages that；The nano particle prepared using the above method has more excellent than business platinum carbon catalyst
Electrocatalysis characteristic.
The present invention in contrived experiment problem is encountered that by metal nanometer line be converted into nano particle feasibility and
Formation mechenism, the content mainly investigated are that the nano wire of one-dimentional structure is converted into zero dimension by the method for reducing metal presoma
Nano particle, and realize the controllable adjustment of Nanoparticulate composition and particle size, it now is possible to solve the problems, such as it is experiment card
Understand the feasibility of anticipation, binary metal nano wire can be changed into unitary nano particle.
The committed step that the present invention is different from prior art is to optimize reduction technique, using suitable reducing agent by binary
Alloy nano-wire is converted into the nano particle of one-component, and the particle diameter of nano particle is controllable.
It is disclosed by the invention metal nanometer line is converted into good effect possessed by the method for nanosphere to be：
The inventive method has extensive universality, and can be generalized to similar other metals prepared by electro-deposition method
Material.The metal nano spherical structure prepared in this way is in the lithium ion battery electrode material in future, fuel cell electrode
Have wide practical use in catalyst and other nano-devices.
Nanosphere prepared by this method is with uniform particle sizes and controllable, method is simply and with universality, manufacturing cycle
The advantages that short and yield is high.Urged by fuel cell of the metal nanoparticle synthesized by this efficient preparation technology in future
Have wide practical use and potential learning value in terms of agent and other energy storage materials.
Brief description of the drawings
Fig. 1 platinum nanosphere synthetic schemes:(a) golden film is deposited, (b) platinum electrodeposition bismuth nano-wire, (c) goes alumina
Template, (d) reduction platinum bismuth nano-wire obtain platinum nanosphere；
The scanning electron microscope image of Fig. 2 (a) platinum bismuth nano-wire arrays, energy spectrum analysis corresponding to (b) dotted line frame；
Fig. 3 (a) and the platinum nanosphere scanning electron microscope image after (b) reduction, the transmission image of (c) platinum nanosphere, (d) dotted line frame
Corresponding energy spectrum analysis；
The scanning electron microscope image of Fig. 4 (a) palladium bismuth nano-wires, (b) energy spectrum analysis as corresponding to dotted line frame in (a), after (c) reduction
Palladium nanosphere scanning electron microscope image, (d) energy spectrum analysis as corresponding to dotted line frame in (c)；
Fig. 5 (a) and (b) use NaBH4Platinum nanosphere scanning electron microscope image after reduction；(c) energy spectrum analysis corresponding to dotted line frame.
Embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
The various changes carried out on the premise of invention spirit and scope to the material component in these embodiments and dosage or change
Belong to protection scope of the present invention.Raw materials used and reagent of the invention is commercially available.
The present invention describes preparation technology so that platinum bismuth nano-wire prepares platinum nanosphere as an example.
Alumina formwork is prepared using secondary oxidation method first, then made by using electrochemical deposition technique in advance
Deposition platinum bismuth bimetal nano line in standby alumina formwork, finally changes glomerate platinum nanostructured by platinum bismuth nano-wire.
Specifically include：The diameter of the platinum bismuth nano-wire of synthesis can be regulated and controled by the pore size of template of alumina formwork；Platinum bismuth nano-wire
Length then controlled by adjusting electrochemical deposition parameter；The geometrical morphology and chemical composition of globular nanostructures can lead to
Reducing agent and precursor solution are crossed to regulate and control.The present invention synthesizes nano wire based on alumina formwork confinement electro-deposition techniques, then
Globular nanostructures are converted to by a stage reduction method, obtained globular nanostructures are uniform and scattered.In the nanometer device in future
There is potential application value in part and nanosecond science and technology.
Embodiment 1
The preparation of platinum nanosphere
Noble metal hybridized nanowire is prepared using alumina formwork confinement codeposition technique first, then will by a stage reduction method
The platinum bismuth nano-wire of preparation is converted to monometallic platinum nanosphere.Specific preparation technology is as described below.
(a) a thickness golden film is deposited to cover all the one end in hole in any one side of anodic oxidation aluminium formwork.(b)
Adjust suitable electro-deposition parameter and prepare platinum bismuth alloy nano wire.(c) alumina formwork is removed with sodium hydroxide solution.(d)
Platinum bismuth nano-wire is placed in precursor solution H2PtCl6·6H2In O, add ascorbic acid and reduce to obtain platinum nanosphere.It is specific to close
It is illustrated in fig. 1 shown below into process.
Acquisition process is：With the two-step electrochemical anodizing method of rafifinal, alumina formwork of the synthesis with even duct
(40~50 volts of anodic oxidation voltage, oxidization time 10~16 hours).It is deposited with one side of the plasma evaporation coating method in template
The golden film thick more than 200nm makees electrode.The composition of electrolyte is 0.005M H2PtCl6·6H2O、0.005M Bi(NO3)2·
5H2O、0.0439M C3H5(OH)3、 0.0108M C4H6O6With 0.037M KOH, HNO is used3Adjust PH=0.9 of solution.Electrification
Learning deposition parameter includes：Constant current (1.2mA/cm2) deposition, sedimentation time 120min.After electro-deposition terminates, oxidation will be carried
The platinum bismuth nano-wire of aluminum alloy pattern plate is dissolved in 4M NaOH solutions, and deoxygenation is gone under conditions of 2h at 60 DEG C in air dry oven
Change aluminum alloy pattern plate, obtained platinum bismuth nano-wire array is cleaned repeatedly with deionized water.The platinum bismuth nano-wire of drying is added to
0.005M H2PtCl6·6H2In O solution, the ascorbic acid for then adding 0.5M is reduced, and is mixed solution and is placed in air blast
After reacting 2h under conditions of 60 DEG C in drying box, cleaned to obtain platinum nanosphere repeatedly with deionized water.
Microstructure and composition characterization result:
See Fig. 2 according to ESEM (SEM) image and power spectrum test result of the platinum bismuth bimetal nano line of above-mentioned technique synthesis
It is shown.From Fig. 2 (a) scanning electron microscope image as can be seen that the platinum bismuth nano-wire prepared be uniformly dispersed, marshalling and surface
Smooth, the diameter of nano wire is about 55nm, and the length of nano wire is determined by electrochemical parameter.Fig. 2 (b) is at Fig. 2 (a) dotted line frames
Corresponding energy spectrum analysis, the results showed that the chemical composition of synthesized nano wire is platinum and bismuth element.
The platinum nanosphere of pure phase is obtained after the platinum bismuth nano-wire of synthesis is further reduced according to above-mentioned technique, it is corresponding to sweep
It is as shown in Figure 3 to retouch sem image, images of transmissive electron microscope and power spectrum test result.It can be observed from Fig. 3 (a) scanning electron microscope image
Synthesized platinum nanosphere geometrical morphology is uniform, and can be with the preparation of large area.Fig. 3 (b) is putting for Fig. 3 (a) dotted box portions
Big image, it can more clearly observe that nanosphere is dispersed, and rough surface.Fig. 3 (c) is the transmission of single platinum nanosphere
Image, it can be seen that the particle diameter of the platinum nanosphere of synthesis is about 160nm, and surface has many " whisker " like structures, and these are unique
Geometry bigger specific surface area and more avtive spots can be provided, available for future fuel-cell catalyst.
By carrying out electro-chemical test to the nanoparticle catalyst of preparation, experimental result is shown：The nanometer prepared using the above method
Particle has higher catalytic activity and good stability.Fig. 3 (d) is the energy spectrum analysis in Fig. 3 (a) dotted line frames region, as a result
The prepared nanosphere of display is pure platinum grain.
Embodiment 2
It is prepared by Pd nanospheres
Using similar technology of preparing, we are also successfully prepared for Pd nanospheres.Details are provided below：First using electricity
Deposition technique synthesizes PdBi nano wires, and precursor solution then is changed into 0.005M PdCl2Solution, reduced using ascorbic acid
Synthesize and pure palladium nanosphere is converted into by palladium bismuth nano-wire.Fig. 4 (a) is the palladium bismuth nano-wire array that electro-deposition obtains, surface light
Sliding and marshalling.It can be seen that the composition of nano wire is palladium and bismuth from Fig. 4 (b) energy spectrum analysis.Fig. 4 (c) is to receive palladium bismuth
Palladium nanosphere obtained by rice noodles reduction, and surface roughness.The nanosphere of synthesis is can be seen that from Fig. 4 (d) energy spectrum analysis
Composition be pure palladium.
Embodiment 3
The regulation and control of nanosphere particle size
By changing the type of reducing agent, we can also regulate and control the particle size of nanosphere.For example, by reducing agent by reproducibility
Weaker ascorbic acid is adjusted to the NaBH with strong reducing property4Afterwards, it is about 5nm's that platinum bismuth nano-wire can be converted into particle diameter
Platinum nanosphere, corresponding scanning electron microscope image and power spectrum test result are as shown in Figure 5.Can be with from Fig. 5 (a) scanning electron microscope image
Find out that the platinum nanosphere of synthesis is reunited together similar to spongy, and pattern is uniform.Fig. 5 (b) is Fig. 5 (a) dotted box portions
Enlarged drawing, can be dispersed with the apparent nanosphere for finding out synthesis, and the particle diameter of ball is obviously reduced.Fig. 5 (c) is Fig. 5 (a)
The energy spectrum analysis in dotted line frame region, the nanosphere for as a result showing preparation are pure platinum grains.
Claims (6)
- A kind of 1. method that metal nanometer line is converted into nanosphere, it is characterised in that carried out by the steps：（1）Electro-deposition prepares metal hybrid nano wire；Described hybridized nanowire refers to that platinum bismuth hybridized nanowire or palladium bismuth are received Rice noodles；（2）Precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, 2h is reacted under conditions of 60 DEG C, i.e., Obtain monometallic nanosphere；Described precursor solution refers to H2PtCl6·6H2O or PdCl2Solution；Described reducing agent refers to ascorbic acid or NaBH4；The composition of described monometallic nanosphere by the composition of previously prepared hybridized nanowire and the species of precursor solution Lai Determine；The particle diameter of described monometallic nanosphere is regulated and controled by the species of reducing agent.
- 2. the method that metal nanometer line is converted into nanosphere described in claim 1, it is characterised in that when using week reduction Ascorbic acid as reducing agent when, the particle diameter of the monometallic nanosphere of preparation is 160nm, and " whisker " like structure is presented in surface； As the NaBH using strong reducing property4During as reducing agent, the particle diameter of prepared monometallic nanosphere is 5nm, and rough surface.
- 3. the method that metal nanometer line is converted into nanosphere described in claim 1, it is characterised in that work as step（2）Described Precursor solution is H2PtCl6·6H2O, when described reducing agent is ascorbic acid, resulting monometallic nanosphere is particle diameter 160nm platinum nanosphere, and " whisker " like structure is presented in surface；As the NaBH using strong reducing property4It is prepared during as reducing agent The particle diameter of platinum nanosphere be 5nm, and rough surface.
- 4. the method that metal nanometer line is converted into nanosphere described in claim 1, it is characterised in that described monometallic platinum The specific preparation process of nanosphere is as follows：(1) acquisition of alumina formworkFirst time anodic oxidation：By high-purity aluminium flake in 0.3 M oxalic acid solution with 50 V DC voltages anodic oxidation 6 hours, Then soaked 6 hours in 60 DEG C of 6 wt% phosphoric acid and the mixed solution of 1.8 wt% chromic acid, to remove the oxygen of surface imperfection Change aluminium film；Second of anodic oxidation：With 50 V DC voltages in 0.3 M oxalic acid solutions Anodic Oxidation 12 hours, then with supersaturation SnCl4Solution removes the unoxidized aluminium in the back side, then erodes the aluminum oxide obstacle positioned at bottom hole portion with 5 wt% phosphoric acid solution Layer, obtains the alumina formwork of two sides through hole；(2) gold is steamed on the surface of alumina formworkBy adjusting the parameter of ion sputtering instrument, the golden film for being 200 nm in a face evaporation thickness of alumina formwork, make golden film The one end in alumina formwork hole is completely covered, to ensure that nano wire can be obtained by the method for electrochemical deposition；(3) using optimization electro-deposition techniques synthesis platinum bismuth nano-wire(4) one stage reduction methods prepare platinum nanosphere0.005M H will be added in the pre-synthesis platinum bismuth nano-wire of step (3)2PtCl6·6H2O solution, adds ascorbic acid Reduced, mixed solution is placed in air dry oven after reacting 2h under conditions of 60 DEG C, cleaned repeatedly with deionized water To platinum nanosphere.
- 5. the method that metal nanometer line is converted into nanosphere described in claim 1, it is characterised in that when the hydridization of electro-deposition When nano wire is palladium bismuth nano-wire, presoma PdCl will be added in palladium bismuth nano-wire2Solution and reducing agent ascorbic acid, at 60 DEG C Under conditions of react 2h after, obtain be shaggy monometallic palladium nanosphere.
- 6. the nanosphere prepared using claim 1 methods described has potential application in fuel-cell catalyst field.
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| US20040157414A1 (en) * | 2000-03-29 | 2004-08-12 | Gole James L. | Silicon based nanospheres and nanowires |
| US20050056118A1 (en) * | 2002-12-09 | 2005-03-17 | Younan Xia | Methods of nanostructure formation and shape selection |
| CN102050423A (en) * | 2009-11-06 | 2011-05-11 | 国家纳米科学中心 | Nickel-bismuth hybridized nanowire and preparation method thereof |
| CN103752845A (en) * | 2014-01-15 | 2014-04-30 | 上海交通大学 | Nickel or nickel alloy perforated nanosphere and method for manufacturing same |
| CN106207155A (en) * | 2016-07-14 | 2016-12-07 | 东北师范大学 | One class integrates nano-hybrid material of positive/negative cyclical effect and preparation method thereof |
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- 2017-09-20 CN CN201710851596.XA patent/CN107755682B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040157414A1 (en) * | 2000-03-29 | 2004-08-12 | Gole James L. | Silicon based nanospheres and nanowires |
| CN1395324A (en) * | 2002-07-30 | 2003-02-05 | 天津大学 | liquid-phase electric deposition N-type and P-type one-dimensional nano line array temp. difference electric material, its equipment and preparation method |
| US20050056118A1 (en) * | 2002-12-09 | 2005-03-17 | Younan Xia | Methods of nanostructure formation and shape selection |
| CN102050423A (en) * | 2009-11-06 | 2011-05-11 | 国家纳米科学中心 | Nickel-bismuth hybridized nanowire and preparation method thereof |
| CN103752845A (en) * | 2014-01-15 | 2014-04-30 | 上海交通大学 | Nickel or nickel alloy perforated nanosphere and method for manufacturing same |
| CN106207155A (en) * | 2016-07-14 | 2016-12-07 | 东北师范大学 | One class integrates nano-hybrid material of positive/negative cyclical effect and preparation method thereof |
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