CN107755682B - A kind of method and application converting metal hybrid nano wire to nanosphere - Google Patents
A kind of method and application converting metal hybrid nano wire to nanosphere Download PDFInfo
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- CN107755682B CN107755682B CN201710851596.XA CN201710851596A CN107755682B CN 107755682 B CN107755682 B CN 107755682B CN 201710851596 A CN201710851596 A CN 201710851596A CN 107755682 B CN107755682 B CN 107755682B
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Abstract
A method of nanosphere is converted by metal nanometer line, comprising: electro-deposition prepares metal hybrid nano wire；Precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, reacts 2h under conditions of 60 DEG C to get monometallic nanosphere is arrived.The present invention synthesizes the nanosphere of different geometrical morphologies and chemical component by regulation reducing agent type and precursor solution.It is expected to construct other nano materials that can convert the nano wire of electro-deposition to nanosphere with this general method, applied to following high performance electrocatalysis material and other nanosecond science and technology.The nanosphere of this method preparation has many advantages, such as 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 following fuel-cell catalyst and other energy storage materials by metal nanoparticle synthesized by this efficient preparation process.
Description
Technical field
The invention belongs to electrochemical deposition preparation nano material and applied field technical fields.More particularly to aoxidizing
A kind of hybridized nanowire of electrochemical method electro-deposition is used in aluminum dipping form plate hole, the conjunction that then will have been synthesized by a stage reduction method again
The method that nanowires of gold is converted into globular nanostructures.
Background technique
Spherical nanostructure have important scientific research value, can be widely applied to catalysis, optics, microelectronics,
The fields 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 there are preparation processes it is complicated, manufacturing cycle is longer the disadvantages of, have aoxidized using electrochemical deposition method at present
Deposit alloy nano wire in aluminum alloy pattern plate, but the nano wire prepared is used as basic unit to be changed by a stage reduction method
Spherical nanostructure does not have been reported that also.
Summary of the invention
Object of the present invention is to solve preparation process present in Conventional nano particulate production is complicated, manufacturing cycle compared with
Long, the problems such as product morphology is uneven, and provide in conjunction with 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 component by regulation reducing agent type and precursor solution
Rice ball.It is expected to construct other nano materials that can convert the nano wire of electro-deposition to nanosphere with this general method,
Applied to the following high performance electrocatalysis material and other nanosecond science and technology.By carrying out electrification to the 5nm Pt nanoparticle of preparation
Test is learned, we, which obtain, has, stability higher than business platinum carbon catalyst activity more with Pt nanoparticle prepared by reduction method
Good performance is expected to be applied to next-generation fuel-cell catalyst.
To achieve the above object, the invention discloses the following technical solutions:
A method of nanosphere is converted by metal nanometer line, it is characterised in that is carried out by following step:
(1) electro-deposition prepares metal hybrid nano wire；The hybridized nanowire refers to platinum bismuth hybridized nanowire or palladium
Bismuth nano-wire；
(2) precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, is reacted under conditions of 60 DEG C
2h to get arrive monometallic nanosphere；
The precursor solution refers to H2PtCl6·6H2O or PdCl2Solution；
The reducing agent refers to ascorbic acid or NaBH4；
The ingredient of the monometallic nanosphere is by the ingredient of previously prepared hybridized nanowire and the kind of precursor solution
Class determines；The partial size of the monometallic nanosphere is regulated and controled by the type of reducing agent.
When the ascorbic acid using week reduction is as reducing agent, the partial size of the monometallic nanosphere of preparation is 160nm,
And " whisker " like structure is presented in surface；As the NaBH using strong reducing property4When as reducing agent, prepared monometallic nanosphere
Partial size is 5nm, and rough surface.
The precursor solution described in step (2) is H2PtCl6·6H2O, it is acquired when the described reducing agent ascorbic acid
Monometallic nanosphere be partial size 160nm platinum nanosphere, and surface present " whisker " like structure；When using strong reducing property
NaBH4When as reducing agent, the partial size 5nm of prepared platinum nanosphere, and rough surface.
Specific preparation process is as follows for monometallic platinum nanosphere of the present invention:
(1) acquisition of alumina formwork
First time anodic oxidation: high-purity aluminium flake is small with 50 V DC voltage anodic oxidations 6 in the oxalic acid solution of 0.3 M
When, it is then impregnated 6 hours in 60 DEG C of 6 wt% phosphoric acid and the mixed solution of 1.8 wt% chromic acid, to remove surface imperfection
Pellumina；
Second of anodic oxidation: then used with 50 V DC voltages at 0.3 M oxalic acid solution Anodic Oxidation 12 hours
The SnCl of saturation4Solution removes the unoxidized aluminium in the back side, then erodes the aluminium oxide positioned at hole bottom with the phosphoric acid solution of 5 wt%
Barrier 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 makes
The one end in alumina formwork hole is completely covered in golden film, to guarantee that nano wire can be obtained by the method for electrochemical deposition；
(3) platinum bismuth nano-wire is synthesized using optimization electro-deposition techniques
With reference to Chang Rong, the synthesis technology of et al. platinum electrodeposition palladium copper ternary nano line (Rong Chang,
Lijun Zheng, Chengwen Wang, Dachi Yang, Gaixia Zhang and Shuhui Sun, Appl.
Catal. B-Environ., 2017,211,205-211.), we have synthesized platinum bismuth hybridized nanometer using similar technique
Line.
(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 anti-bad
Hematic acid is restored, and mixed solution is placed in air dry oven after reacting 2h under conditions of 60 DEG C, repeatedly with deionized water
Cleaning obtains 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 preparation nanosphere with
Application in terms of fuel-cell catalyst, experimental result are shown: this method simple, controllable nanostructure with preparation process
Particle size, it is reproducible the advantages that；Had using the nano particle of above method preparation more 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 to convert zero dimension for the nano wire of one-dimentional structure 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 it solves the problems, such as to be experiment card
The feasibility of anticipation is illustrated, binary metal nano wire can be changed into unitary nano particle.
The committed step that the present invention is different from the 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 partial size of nano particle is controllable.
Disclosed by the invention convert metal nanometer line to possessed by the method for nanosphere has the active effect that
The method of the present invention has extensive universality, and can be generalized to other similar prepared by electro-deposition method
Metal material.The metal nano spherical structure prepared in this way is in following lithium ion battery electrode material, fuel cell
Have wide practical use in electrode catalyst and other nano-devices.
The nanosphere of this method preparation is with uniform particle sizes and controllable, method is simply and with universality, manufacturing cycle
The advantages that short and yield is high.It is urged by metal nanoparticle synthesized by this efficient preparation process in following fuel cell
Have wide practical use and potential learning value in terms of agent and other energy storage materials.
Detailed description of the invention
Fig. 1 platinum nanosphere synthetic schemes: (a) being deposited golden film, and (b) platinum electrodeposition bismuth nano-wire (c) goes alumina
Template (d) restores platinum bismuth nano-wire and obtains platinum nanosphere；
The scanning electron microscope image of Fig. 2 (a) platinum bismuth nano-wire array, (b) the corresponding energy spectrum analysis of dotted line frame；
Fig. 3 (a) and the platinum nanosphere scanning electron microscope image after (b) reduction, (c) transmission image of platinum nanosphere are (d) empty
The corresponding energy spectrum analysis of wire frame；
The scanning electron microscope image of Fig. 4 (a) palladium bismuth nano-wire, (b) by the corresponding energy spectrum analysis of dotted line frame in (a), (c) also
Palladium nanosphere scanning electron microscope image after original, (d) by the corresponding energy spectrum analysis of dotted line frame in (c)；
Fig. 5 (a) and (b) use NaBH4Platinum nanosphere scanning electron microscope image after reduction；(c) the corresponding power spectrum point of dotted line frame
Analysis.
Specific 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
Range, 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
Under the premise of invention spirit and scope, to the various changes or change of material component and dosage progress in these embodiments
It belongs to the scope of protection of the present invention.The raw materials used in the present invention and reagent are commercially available.
The present invention describes preparation process so that platinum bismuth nano-wire prepares platinum nanosphere as an example.
Alumina formwork is prepared using secondary oxidation method first, is then made by using electrochemical deposition technique in advance
Platinum bismuth bimetal nano line is deposited in standby alumina formwork, and platinum bismuth nano-wire is finally converted into glomerate platinum nanostructure.
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 pass through adjust electrochemical deposition parameter controlled；The geometrical morphology and chemical component of globular nanostructures can lead to
Reducing agent and precursor solution are crossed to regulate and control.The present invention is based on alumina formwork confinement electro-deposition techniques to synthesize nano wire, then
Globular nanostructures are converted to by a stage reduction method, obtained globular nanostructures are uniform and disperse.In following nanometer device
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, is then restored by a step
The platinum bismuth nano-wire of preparation is converted to monometallic platinum nanosphere by method.Specific preparation process is as described below.
(a) one end in hole is covered all in any one side one thickness golden film of vapor deposition of anodic oxidation aluminium formwork.(b)
It adjusts suitable electro-deposition parameter and prepares 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, ascorbic acid is added and restores to obtain platinum nanosphere.It is specific to close
It is illustrated in fig. 1 shown below at process.
Acquisition process are as follows: with the two-step electrochemical anodizing method of rafifinal, synthesize the alumina formwork with even duct
(40~50 volts of anodic oxidation voltage, oxidization time 10~16 hours).One side with plasma evaporation coating method in template is deposited
Golden film greater than 200nm thickness makees electrode.The ingredient 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.It, will be with oxidation after electro-deposition
The platinum bismuth nano-wire of aluminum alloy pattern plate is dissolved in 4M NaOH solution, 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 that 0.5M is then added is restored, and is mixed solution and is placed in air blast
After reacting 2h under conditions of 60 DEG C in drying box, is cleaned repeatedly with deionized water and obtain platinum nanosphere.
Microstructure and ingredient characterization result:
See according to scanning electron microscope (SEM) image and power spectrum test result of the platinum bismuth bimetal nano line of above-mentioned technique synthesis
Shown in Fig. 2.From the scanning electron microscope image of Fig. 2 (a) as can be seen that preparation platinum bismuth nano-wire be uniformly dispersed, marshalling and
Surface is smooth, and the diameter of nano wire is about 55nm, and the length of nano wire is determined by electrochemical parameter.Fig. 2 (b) is Fig. 2 (a) dotted line
The corresponding energy spectrum analysis in frame place, the results showed that the chemical component 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 restored according to above-mentioned technique, it is corresponding to sweep
Retouching sem image, images of transmissive electron microscope and power spectrum, test results are shown in figure 3.It can be observed from the scanning electron microscope image of Fig. 3 (a)
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 portion
Big image can more clearly observe that nanosphere is evenly dispersed, and rough surface.Fig. 3 (c) is the transmission of single platinum nanosphere
Image, it can be seen that the partial size of the platinum nanosphere of synthesis is about 160nm, and there are many " whisker " like structures on surface, these are unique
Geometry bigger specific surface area and more active sites can be provided, can be used for following 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 catalytic activity with higher and good stability.Fig. 3 (d) is the energy spectrum analysis of Fig. 3 (a) dotted line frame region, as a result
The prepared nanosphere of display is pure platinum grain.
Embodiment 2
The preparation of Pd nanosphere
Using similar technology of preparing, we are also successfully prepared for Pd nanosphere.Details are provided below: adopting first
PdBi nano wire is synthesized with electro-deposition techniques, precursor solution is then changed to 0.005M PdCl2Solution, using ascorbic acid
Reduction synthesis by palladium bismuth nano-wire is converted into pure palladium nanosphere.Fig. 4 (a) is the palladium bismuth nano-wire array that electro-deposition obtains, table
Face is smooth and marshalling.The ingredient that can be seen that nano wire from the energy spectrum analysis of Fig. 4 (b) is palladium and bismuth.Fig. 4 (c) is by palladium
Bismuth nano-wire restores obtained palladium nanosphere, and surface roughness.It can be seen that receiving for synthesis from the energy spectrum analysis of Fig. 4 (d)
The ingredient of rice ball is pure palladium.
Embodiment 3
The regulation 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 also
The weaker ascorbic acid of originality is adjusted to the NaBH with strong reducing property4Afterwards, platinum bismuth nano-wire can be converted into partial size is about
The platinum nanosphere of 5nm, test results are shown in figure 5 for corresponding scanning electron microscope image and power spectrum.From the scanning electron microscope (SEM) photograph of Fig. 5 (a)
As can be seen that the platinum nanosphere of synthesis is reunited together similar to spongy, and pattern is uniform.Fig. 5 (b) is Fig. 5 (a) dotted line frame
Partial enlarged drawing clearer can find out that the nanosphere of synthesis is evenly dispersed, and the partial size of ball is obviously reduced.Fig. 5 (c) is
The energy spectrum analysis of Fig. 5 (a) dotted line frame region, the nanosphere prepared as the result is shown are pure platinum grains.
Claims (6)
1. a kind of method for converting nanosphere for metal hybrid nano wire, it is characterised in that carried out by following step:
(1) electro-deposition prepares metal hybrid nano wire；The hybridized nanowire refers to that platinum bismuth hybridized nanowire or palladium bismuth are miscellaneous
Change nano wire；
(2) precursor solution and reducing agent are added in the metal hybrid nano wire of preparation, reacts 2h under conditions of 60 DEG C, i.e.,
Obtain monometallic nanosphere；
The precursor solution refers to H2PtCl6·6H2O or PdCl2Solution；
The reducing agent refers to ascorbic acid or NaBH4；
The ingredient of the monometallic nanosphere by previously prepared hybridized nanowire ingredient and precursor solution type Lai
It determines；The partial size of the monometallic nanosphere is regulated and controled by the type of reducing agent.
2. the method described in claim 1 for converting nanosphere for metal hybrid nano wire, it is characterised in that gone back when using weak
When the ascorbic acid of originality is as reducing agent, the monometallic nanosphere partial size of preparation is 160nm, and " whisker " like knot is presented in surface
Structure；As the NaBH using strong reducing property4When as reducing agent, prepared monometallic nanosphere partial size is 5nm, and surface is thick
It is rough.
3. the method described in claim 1 for converting nanosphere for metal hybrid nano wire, it is characterised in that when step (2) institute
The precursor solution stated is H2PtCl6·6H2O, when the reducing agent is ascorbic acid, obtained monometallic nanosphere is
The platinum nanosphere of partial size 160nm, and " whisker " like structure is presented in surface；As the NaBH using strong reducing property4When as reducing agent, institute
The partial size of the platinum nanosphere of preparation is 5nm, and rough surface.
4. the method described in claim 1 for converting nanosphere for metal hybrid nano wire, it is characterised in that the Dan Jin
Belonging to nanosphere, specific preparation process is as follows:
(1) acquisition of alumina formwork
First time anodic oxidation: by high-purity aluminium flake with 50 V DC voltage anodic oxidation 6 hours in the oxalic acid solution of 0.3 M,
Then it is impregnated 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 at 0.3 M oxalic acid solution Anodic Oxidation 12 hours, then with supersaturation
SnCl4Solution removes the unoxidized aluminium in the back side, then erodes the aluminium oxide obstacle positioned at hole bottom with the phosphoric acid solution of 5 wt%
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 makes golden film
The one end in alumina formwork hole is completely covered, to guarantee to obtain hybridized nanowire by the method for electrochemical deposition；
(3) platinum bismuth hybridized nanowire is synthesized using electro-deposition techniques
(4) one stage reduction methods prepare platinum nanosphere
0.005M H will be added in the pre-synthesis platinum bismuth hybridized nanowire of step (3)2PtCl6·6H2O solution adds anti-bad
Hematic acid is restored, and mixed solution is placed in air dry oven after reacting 2h under conditions of 60 DEG C, repeatedly with deionized water
Clean to platinum nanosphere.
5. the method described in claim 1 for converting nanosphere for metal hybrid nano wire, it is characterised in that when electro-deposition
When hybridized nanowire is palladium bismuth hybridized nanowire, presoma PdCl will be added in palladium bismuth hybridized nanowire2Solution and reducing agent are anti-
Bad hematic acid, after reacting 2h under conditions of 60 DEG C, what is obtained is shaggy monometallic palladium nanosphere.
6. using application of the nanosphere of claim 1 the method preparation in fuel-cell catalyst field.
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