CN104532048B - A kind of single chemical takes off alloy and prepares Ag-Cu nanoporous nucleocapsid structure method - Google Patents
A kind of single chemical takes off alloy and prepares Ag-Cu nanoporous nucleocapsid structure method Download PDFInfo
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- CN104532048B CN104532048B CN201410814749.XA CN201410814749A CN104532048B CN 104532048 B CN104532048 B CN 104532048B CN 201410814749 A CN201410814749 A CN 201410814749A CN 104532048 B CN104532048 B CN 104532048B
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Abstract
The invention belongs to Materials Science and Engineering field, take off alloy particularly to a kind of single chemical and prepare Ag Cu nanoporous nucleocapsid structure method.The inventive method, on the basis of regulating and controlling foundry alloy composition and structure, uses simple single step room temperature chemistry to take off alloy, it is achieved that the preparation of the complicated metal micro-nano structure of Ag Cu nanoporous nucleocapsid structure.The novel single chemical that the present invention proposes takes off the complicated metal micro-nano structure method of alloy preparation, has the features such as equipment is simple, easy and simple to handle, with low cost, product favorable reproducibility, controllability strong, applicable production in enormous quantities.
Description
Technical field
The invention belongs to Materials Science and Engineering field, take off alloy particularly to a kind of single chemical and prepare Ag-Cu
Nanoporous nucleocapsid structure method.
Background technology
Metal nano material is because of its dimensional effect and skin effect, it is possible to show widely different with macroscopic view block materials
The most different characteristics, at multiple necks such as surface modification, sensing, optics, catalysis and energy conversion and storages
Territory has extensive application potential.Thus explore simple synthetic method for preparing the metal of various form
Micro nano structure is an important topic of micro-nano scientific domain, and result of study has important use value.
Have multiple technologies at present and can realize synthesis and the preparation of metal micro-nano structure, such as gas phase physics
Deposition, chemical vapor deposition, solution-gel method, arc discharge method, sputtering method, template etc..But
The all requirements to synthesis device of most of synthetic methods are higher, or synthesis step is complicated so that synthesis cost
Higher, and it is unfavorable for large-scale production.
The de-alloyage of chemistry is the novel metal micro nano structure preparation method recently developed, because of its operation letter
Just, equipment is simple, with low cost, controllability strong and is prone to industrialized production and is led by micro-nano science
The extensive concern in territory.But, conventional chemistry takes off alloyage and is simply possible to use in and prepares metal micro-nano loose structure,
It is difficult to the preparation of other complicated metal micro-nano structures, thus greatly limit answering of the de-alloyage of chemistry
With.
In order to solve the defect of the de-alloyage of chemistry, the present invention proposes to use and carries out foundry alloy composition and structure
Regulation and control, take off alloy approach in conjunction with simple single step room temperature chemistry, it is achieved the control to chemical reaction process, open up
Having opened up chemical de-alloyage range of application, the complicated metal having prepared Ag-Cu nanoporous nucleocapsid structure is micro-
Nanostructured.
Summary of the invention
It is an object of the invention to provide novel single chemical and take off the complicated micro nano structure method of alloy preparation,
On the basis of foundry alloy composition and structure are regulated and controled, simple single step room temperature chemistry is used to take off alloy legal system
Standby go out Ag-Cu nanoporous nucleocapsid structure complicated metal micro-nano structure, for the complicated metal micro-nano of preparation
Structure provides new technological approaches.
Not enough for prior art, the invention provides a kind of single chemical and take off alloy to prepare Ag-Cu nanometer many
Hole nucleocapsid structure method.
A kind of single chemical takes off alloy and prepares Ag-Cu nanoporous nucleocapsid structure method, comprises the steps:
Step 1: preparation Zr-Cu-Ag-Al-O alloy: by pure Zr, pure Cu, pure Ag and pure Al in proportion
Mix, in the mixed atmosphere of argon and air, repeated multiple times carry out melting, treat that sample constituents is uniform
Rear cooling obtains Zr-Cu-Ag-Al-O alloy pig；
Step 2: preparation Zr-Cu-Ag-Al-O band: by gained Zr-Cu-Ag-Al-O alloy pig system in step 1
Standby one-tenth Zr-Cu-Ag-Al-O alloy strip；
Step 3: de-alloy: gained Zr-Cu-Ag-Al-O alloy strip in step 2 is cut into suitable length, and
It is placed in hydrofluoric acid solution, at room temperature places and carry out the de-alloy of chemistry；
Step 4: cleaning-drying: the Zr-Cu-Ag-Al-O alloy strip after gained takes off alloy in step 3 is taken out,
Use deionized water and alcohol-pickled cleaning respectively, be dried the most in atmosphere, obtain Ag-Cu nanoporous
Nucleocapsid structure.
In described step 1, the atomic ratio of pure Zr, pure Cu, pure Ag and pure Al is Zr:Cu:Ag:Al=38:
41:8:7.
In described step 1, the total pressure of the gaseous mixture of argon and appropriate air is 0.05MPa, wherein air
Volume fraction is 0.01%～0.1%, can be adjusted according to smelting furnace inner chamber size.
In described step 1, fusion process uses the method such as electric arc melting or induction melting.
In described step 1, the oxygen content of gained Zr-Cu-Ag-Al-O alloy pig is 5%～10%.
Preparing Zr-Cu-Ag-Al-O band in described step 2 uses single roller to revolve the method quenched.
In described step 2, the thickness of gained Zr-Cu-Ag-Al-O alloy strip is 20 μm～100 μm, and width is big
In 2mm, a length of more than 2m.
Gained Zr-Cu-Ag-Al-O alloy strip in step 2 is blocked by described step 3 and carries out de-alloy, block
After a length of 20mm～60mm.
In described step 3, the concentration of hydrofluoric acid solution is 0.05mol/L.
In described step 3, the chemistry de-alloy time is 24 hours.
Described Ag-Cu nanoporous nucleocapsid structure is nanoporous shape, and aperture and ligament size are no more than 100
Nm, this body structure surface is Ag shell, and kernel is made up of Ni metal, Ag.
The invention have the benefit that
1. compared to other metal micro-nano structure preparation methoies, this method equipment needed thereby is simple, and technique is simple,
With low cost, it is easy to industrialization large-scale production；
2. without consuming the energy, energy consumption is low, production process environmentally safe；
3. controllability is strong, good repetitiveness.
Accompanying drawing explanation
Fig. 1 is gained Zr in the embodiment of the present invention 138Cu41Ag8Al7O7Alloy strip and chemistry obtain after taking off alloy
Ag-Cu nanoporous nucleocapsid structure XRD figure spectrum；
Fig. 2 is gained Ag-Cu nanoporous nucleocapsid structure scanning electron microscope in the embodiment of the present invention 1
(SEM) photo；
Fig. 3 is the energy spectrogram of gained Ag-Cu nanoporous nucleocapsid structure in the embodiment of the present invention 1；
Fig. 4 is (a) transmission electron microscope of gained Ag-Cu nanoporous nucleocapsid structure in the embodiment of the present invention 1
(TEM) photo and the SEAD style figure of (b) correspondence；
Fig. 5 is that (a) transmission electron microscope of gained Ag-Cu nanoporous nucleocapsid structure in the embodiment of the present invention 1 is high
Differentiating photo and (b) TEM dark field image photo, wherein illustration 1 and illustration 2 are respectively region 1 in (a)
With the result after the fast Fourier transform of region 2.
Detailed description of the invention
The invention provides a kind of single chemical to take off alloy and prepare Ag-Cu nanoporous nucleocapsid structure method, under
Face combines the drawings and specific embodiments, and the present invention will be further described.
Embodiment 1
Preparation Ag-Cu nanoporous nucleocapsid structure, comprises the following steps:
Step 1: preparation Zr-Cu-Ag-Al-O alloy: pure Zr, pure Cu, pure Ag and pure Al are mixed
Closing, in the 0.05MPa argon mixed atmosphere with air, (volume of air content is about 0.05%) electric arc melts
Refine and make for three times sample uniform, after cooling, obtain Zr38Cu41Ag8Al7O7Alloy pig；
Step 2: preparation Zr38Cu41Ag8Al7O7Alloy strip: by gained Zr in step 138Cu41Ag8Al7O7
Alloy uses single roller rotation system of quenching to be prepared into, and width is about 6mm, thickness is about the alloy strip of 70 μm.
Step 3: de-alloy: configuration concentration is the hydrofluoric acid solution of 0.05mol/L, by gained in step 2
Zr38Cu41Ag8Al7O7Alloy strip is cut into the segment that length is about 2cm, is placed in the concentration that volume is 1L and is
In the hydrofluoric acid solution of 0.05mol/L, at room temperature place and carry out the de-alloy of chemistry about 24 hours；
Step 4: cleaning-drying: by the Zr after gained takes off alloy in step 338Cu41Ag8Al7O7Alloy strip takes
Go out, use deionized water and alcohol-pickled cleaning respectively, be dried the most in atmosphere, now
Zr38Cu41Ag8Al7O7Alloy strip surface i.e. forms Ag-Cu nanoporous nucleocapsid structure.
Fig. 1 is the Zr described in the present embodiment38Cu41Ag8Al7O7Alloy strip and chemistry obtain after taking off alloy
The XRD figure spectrum of Ag-Cu nanoporous nucleocapsid structure.From the figure, it can be seen that before de-alloy
Zr38Cu41Ag8Al7O7Alloy strip is made up of amorphous phase and a small amount of Crystallization Phases, and after the de-alloy of chemistry, sample is by pure
Ag is constituted with pure Cu phase.
Fig. 2 is the SEM photograph of Ag-Cu nanoporous nucleocapsid structure described in the present embodiment.From figure permissible
Seeing, the hole of this structure has two kinds of typical sizes, a kind of 15nm that is about, and another kind is about 40nm,
Ligament diameter is about 60nm.
Fig. 3 is the energy spectrogram of Ag-Cu nanoporous nucleocapsid structure described in the present embodiment.See from figure,
This structure only comprises Cu and Ag element.Through measuring, this constituent is about Cu44Ag56。
Fig. 4 is (a) transmission electron microscope (TEM) of Ag-Cu nanoporous nucleocapsid structure described in the present embodiment
Photo and the SEAD style of (b) correspondence.It will be seen that the hole of this structure has from (a)
Having two kinds of typical sizes, a kind of 15nm that is about, another kind of about 40nm, ligament diameter is about 60nm.
Fig. 5 is (a) transmission electron microscope high-resolution photo of Ag-Cu nanoporous nucleocapsid structure described in embodiment
(b) the TEM dark field image photo that the diffraction spot of Ag obtains is chosen.Spacing of lattice in (a) is carried out
After demarcation, find that top layer is by Ag atomic building.To Ag-Cu nanoporous nucleocapsid structure surface element in (a)
Point and core carry out fast Fourier transform, illustration 1 and illustration 2 are fast Fourier transform result.
Demarcating it, find that top layer is made up of Ag, core is made up of Ag and Cu.B () is for choosing
The TEM dark field image photo that the diffraction spot of Ag obtains, it is found that the surface-boundary brightness of this structure is higher,
Thus illustrate that sample has the shell of one layer of Ag.In sum, this structure is to have the Ag-Cu of Ag shell
Nanoporous nucleocapsid structure.
Claims (10)
1. a single chemical takes off alloy and prepares Ag-Cu nanoporous nucleocapsid structure method, it is characterised in that
Comprise the steps:
Step 1: preparation Zr-Cu-Ag-Al-O alloy: by pure Zr, pure Cu, pure Ag and pure Al in proportion
Mix, in the mixed atmosphere of argon and air, repeated multiple times carry out melting, treat that sample constituents is uniform
Rear cooling obtains Zr-Cu-Ag-Al-O alloy pig；
Step 2: preparation Zr-Cu-Ag-Al-O band: by gained Zr-Cu-Ag-Al-O alloy pig system in step 1
Standby one-tenth Zr-Cu-Ag-Al-O alloy strip；
Step 3: de-alloy: gained Zr-Cu-Ag-Al-O alloy strip in step 2 is placed in hydrofluoric acid solution,
At room temperature place and carry out the de-alloy of chemistry；
Step 4: cleaning-drying: the Zr-Cu-Ag-Al-O alloy strip after gained takes off alloy in step 3 is taken out,
Use deionized water and alcohol-pickled cleaning respectively, be dried the most in atmosphere, obtain Ag-Cu nanoporous
Nucleocapsid structure；
In described step 1, the atomic ratio of pure Zr, pure Cu, pure Ag and pure Al is Zr:Cu:Ag:Al=38:
41:8:7.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 1, argon is 0.05MPa with the total pressure of the mixed atmosphere of air,
Wherein the volume fraction of air is 0.01%～0.1%.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 1, fusion process uses electric arc melting or induction melting side
Method.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 1, the oxygen content of gained Zr-Cu-Ag-Al-O alloy pig is
5%～10%.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that prepare Zr-Cu-Ag-Al-O band in described step 2 and use single roller to revolve the method quenched.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 2, the thickness of gained Zr-Cu-Ag-Al-O alloy strip is 20
μm～100 μm, width is more than 2mm, a length of more than 2m.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 3, gained Zr-Cu-Ag-Al-O alloy strip in step 2 is blocked
Carry out de-alloy, a length of 20mm～60mm after blocking.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 3, the concentration of hydrofluoric acid solution is 0.05mol/L.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid knot
Structure method, it is characterised in that in described step 3, the chemistry de-alloy time is 24 hours.
A kind of single chemical the most according to claim 1 takes off alloy and prepares Ag-Cu nanoporous nucleocapsid
Structural approach, it is characterised in that described Ag-Cu nanoporous nucleocapsid structure is nanoporous shape, aperture and
Ligament size is no more than 100nm, and this body structure surface is Ag shell, and kernel is made up of Ni metal, Ag.
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| CN108338161B (en) * | 2018-01-30 | 2019-07-26 | 河北工业大学 | A kind of supported porous silver oxide nanometer rod composite material of nano-porous silver and preparation method thereof |
| CN108265192B (en) * | 2018-01-30 | 2019-08-09 | 河北工业大学 | A kind of respirable laminar nano Porous Cu silver composite material and preparation method thereof |
| CN108557757B (en) * | 2018-01-30 | 2019-07-26 | 河北工业大学 | A kind of supported porous silver oxide nanosheet composite material of nano-porous silver and preparation method thereof |
| CN108330526B (en) * | 2018-01-30 | 2019-07-26 | 河北工业大学 | A kind of supported porous oxidation silver nanoparticle ball composite material and preparation method of nano-porous silver |
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| CN102943187A (en) * | 2012-11-19 | 2013-02-27 | 河北工业大学 | Preparation method of nano porous copper |
| CN103343253A (en) * | 2013-07-03 | 2013-10-09 | 河北工业大学 | Method for preparing nano-porous copper |
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| CN102943187A (en) * | 2012-11-19 | 2013-02-27 | 河北工业大学 | Preparation method of nano porous copper |
| CN103343253A (en) * | 2013-07-03 | 2013-10-09 | 河北工业大学 | Method for preparing nano-porous copper |
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