CN107398554B - A kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu - Google Patents
A kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses the methods that a kind of de- alloy of chemistry prepares the micro-nano laminated structure of Cu, the following steps are included: (1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: after pure Cu, pure Ni and pure Fe powder are mixed in atomic ratio for 17~18:17~18:62~68 ratio, Cu-Ni-Fe metastable state eutectic structure is prepared using increasing material manufacturing system；(2) it takes off alloy: obtained Cu-Ni-Fe metastable state eutectic structure is placed in the nitric acid solution of 0.03~0.07mol/L, place 2~8 hours at room temperature, carry out the de- alloy of chemistry；(3) it is cleaned and dried: the Cu-Ni-Fe metastable state eutectic structure after obtained de- alloy is taken out, successively use deionized water and alcohol soaking and washing, obtain the micro-nano laminated structure of Cu after dry.The preparation method obtains Cu-Ni-Fe metastable state tissue by increasing material manufacturing system, prepares the micro-nano laminated structure of Cu using the de- alloy approach of simple chemistry, provides new technological approaches to prepare complicated metal micro-nano structure.
Description
Technical field
The present invention relates to Materials Science and Engineering fields, and in particular to a kind of de- alloy preparation micro-nano sheet knot of Cu of chemistry
The method of structure.
Background technique
Metal nano material can be shown far different with macroscopical block materials because of its dimensional effect and skin effect
Characteristic, on surface, modification, sensing, optics, catalysis and the multiple fields such as energy conversion and storage have widely applied latent
Power.The method for thus exploring the new metal micro-nano structure for being used to prepare various forms is a Xiang Chong of micro-nano scientific domain
Project is wanted, result of study has important use value.
Existing multiple technologies may be implemented the synthesis and preparation of metal micro-nano structure at present, such as gas phase physical deposition,
Chemical vapor deposition, solution-gel method, arc discharge method, sputtering method, template etc..But most methods set synthesis
Standby is more demanding, or haves the defects that complicated step, higher cost and be unfavorable for large-scale production.
The de- alloyage of chemistry is a kind of novel metal micro nano structure preparation method developed recently, has equipment letter
Feature single, easy to operate, low in cost, controllability is strong, great application value.But traditional chemistry takes off alloyage and is simply possible to use in
Prepare metal micro-nano porous structure, it is difficult to the preparation for realizing other complicated metal micro-nano structures, thus greatly limiting
Learn the application of de- alloyage.
Summary of the invention
The purpose of the invention is to provide a kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu, pass through increasing
Material manufacture system obtains Cu-Ni-Fe metastable state tissue, prepares the micro-nano sheet knot of Cu using the de- alloy approach of simple chemistry
Structure provides new technological approaches to prepare complicated metal micro-nano structure.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu, comprising the following steps:
(1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: by pure Cu, pure Ni and pure Fe powder by atomic ratio be 17~
After the ratio of 18:17~18:62~68 is mixed, Cu-Ni-Fe metastable state eutectic group is prepared using increasing material manufacturing system
It knits；
(2) it takes off alloy: obtained Cu-Ni-Fe metastable state eutectic structure is placed in the nitric acid solution of 0.03~0.07mol/L
In, it places 2~8 hours at room temperature, carries out the de- alloy of chemistry；
(3) be cleaned and dried: by after obtained de- alloy Cu-Ni-Fe metastable state eutectic structure take out, successively using go from
Sub- water and alcohol soaking and washing obtain the micro-nano laminated structure of Cu after dry.
Specifically, in the step (1) pure Cu, pure Ni and pure Fe atomic ratio 17.5:17.5:65.
Specifically, increasing material manufacturing system has energy source in the step (1), and the energy source is laser or electron beam
High-energy source.
More specifically, the step (1) and is lower than in water oxygen content in high-purity argon gas protection or vacuum protection
Cu-Ni-Fe metastable state eutectic structure is prepared using increasing material manufacturing system under the conditions of 10ppm.
Preferably, the increasing material manufacturing system be synchronous powder feeding system increasing material manufacturing system, and its material system be it is openable,
It can continuously be manufactured.
Further, the concentration of nitric acid solution is 0.05mol/L in the step (2).
Further, the chemistry de- alloy time is 4~6 hours in the step (2), until solution is in light yellow；
Further, in the step (3), first with deionized water to the Cu-Ni-Fe metastable state after obtained de- alloy
After eutectic structure soaking and washing 1~3 time, then with alcohol soaking and washing 2~4 times, finally it is dried.
Preferably, in the step (3), the drying is to spontaneously dry 15~24 hours at room temperature.
Specifically, the thickness of the micro-nano laminated structure of Cu obtained in the step (3) is not more than 1 micron, and length is
10~2000 microns.
Compared with prior art, the invention has the following advantages:
(1) Cu-Ni-Fe metastable state eutectic structure is prepared using increasing material manufacturing system in the present invention, due to increasing material manufacturing
The rapid cooling of technology acts on, and can get the metastable state eutectic structure that other preparation methods are difficult to obtain, which can directly lead to
The de- alloy of simple chemistry is crossed to prepare a micron Cu laminated structure, thus the Cu-Ni-Fe alloy for overcoming other methods to obtain without
Method directly obtains the defect of the similar micro-nano laminated structure of Cu by taking off alloy.Also, Cu- is prepared using increasing material manufacturing system
Ni-Fe metastable state eutectic structure is high-efficient, can greatly shorten the preparation time of metal alloy, and then shorten entire preparation process
Duration, be suitable for being mass produced.
(2) the Cu-Ni-Fe alloy that the present invention is prepared on substrate using increasing material manufacturing system is made by de- alloy
Cu-Ni-Fe alloy is changed into the micro-nano laminated structure of Cu also can be used in addition to the preparation that can be used for the micro-nano laminated structure of Cu
In the preparation of the micro-nano sheet coating of Cu, the coating and substrate have good metallurgical bonding, not easily to fall off.
(3) present invention is compared to other metal micro-nano structure preparation methods, and this method technique is more simple, and step is more
It is few, and manufacturing cost is cheap, and equipment needed for preparation process is also less, and operation is simpler, and operating condition is easy to control,
It is prepared that the micro-nano laminated structure stability of Cu is good, and preparation process is reproducible, is easy to industrialization large-scale production, can push away
Wide application.
(4) present invention is without consuming the energy, and low energy consumption, production process no pollution to the environment.
(2) present invention carries out the de- alloy of chemistry using nitric acid solution, and iron and nickel are more soluble in nitric acid for copper,
It can reach the purpose of removing, also, the chemistry de- alloy time of the invention is short, is conducive to the duration for shortening entire preparation process,
Accelerate preparation progress；In addition, nitric acid solution itself is nontoxic, it is more advantageous to the personal safety of safeguard work personnel.
Detailed description of the invention
Fig. 1 is preparation flow block diagram of the invention.
Fig. 2 is the XRD spectrum of gained Cu micro-nano laminated structure corrosion front and back in present example 1；
Fig. 3 is the SEM photograph of the gained micro-nano laminated structure of Cu in present example 1；
Fig. 4 is the EDS map of the gained micro-nano laminated structure of Cu in present example 1.
Specific embodiment
The invention will be further described with embodiment for explanation with reference to the accompanying drawing, and mode of the invention includes but not only limits
In following embodiment.
The purpose of the present embodiment is that new technological approaches is provided for complicated metal micro-nano structure, as shown in Figure 1, the technology
Scheme mainly includes preparation Cu-Ni-Fe metastable state eutectic structure, and → de- alloy → is cleaned and dried these three steps, wherein most main
The improvement wanted is that Cu-Ni-Fe metastable state eutectic structure is prepared using increasing material manufacturing system, which can directly pass through
The simple de- alloy of chemistry prepares a micron Cu laminated structure, and the Cu-Ni-Fe metastable state eutectic that benefit obtains with other methods
Tissue directly can not obtain similar structures by de- alloy.Also, wealth manufacture system preparation Cu-Ni-Fe is metastable using increasing
State eutectic structure is high-efficient, can greatly shorten the preparation time of metal alloy, and then shorten the duration of entire preparation process, fit
It is suitable for large-scale production.In the present embodiment, used increasing material manufacturing system is synchronous powder feeding system increasing material manufacturing system, specific next
Say, be the RenAM 500M system with SafeChange filter, and its material system be it is openable, can carry out continuous
Manufacturing time is saved in manufacture.
The specific preparation process of the present embodiment is illustrated by taking following instance as an example.
Example 1
Prepare the method for the micro-nano laminated structure of Cu the following steps are included:
(1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: it is by atomic ratio by pure Cu, pure Ni and pure Fe powder
After the ratio of 17.5:17.5:65 is mixed, in water oxygen content lower than under 10ppm, high-purity argon gas protective condition, synchronization is utilized
Cu-Ni-Fe metastable state eutectic structure is prepared in powder-feeding laser increasing material manufacturing system；
(2) take off alloy: first configuration concentration is the nitric acid solution of 0.05mol/L, the Cu-Ni-Fe for then obtaining step (1)
Metastable state eutectic structure is cut into 5mm × 5mm × 10mm fritter, is placed in the nitric acid solution, places 4 hours at room temperature,
Carry out the de- alloy of chemistry；
It is worth noting that, in the process, nitric acid solution should the amount of skipping over, then controlled by controlling the alloy time
Final product processed, the present embodiment are that de- alloy is carried out in excess nitric acid solution, and discovery liquid is in pale yellow after placing 4 hours
Color, i.e., de- alloy are completed.
(3) be cleaned and dried: the Cu-Ni-Fe metastable state eutectic structure after the de- alloy that step (2) is obtained is taken out, and first uses
After deionized water is to the Cu-Ni-Fe metastable state eutectic structure soaking and washing after obtained de- alloy, then with alcohol soaking and washing 2
It is secondary, it finally spontaneously dries 15 hours at room temperature, obtains the micro-nano laminated structure of Cu.
Its cleaning-drying is common cleaning-drying process, and it is more preferable to carry out its effect by above-mentioned steps, more efficient.
In above-mentioned preparation process, this example has taken XRD to the Cu-Ni-Fe metastable state eutectic structure before and after de- alloy
Map obtains the XRD spectrum of Cu as shown in Figure 2 micro-nano laminated structure corrosion front and back, as seen from the figure, before de- alloy in alloy
Mainly comprising Cu and (Fe, Ni) two-phase, laminated structure is mainly Cu after taking off alloy.
In addition, this example also has taken SEM photograph and EDS map to the micro-nano laminated structure of obtained Cu, obtain such as Fig. 3
Shown in the SEM photograph of the micro-nano laminated structure of Cu and the EDS map of the micro-nano laminated structure of Cu shown in Fig. 4；It can be with by Fig. 3
To find out, alloy surface forms continuous laminated structure after de- alloy, and laminated structure thickness is about 1 μm, and length is about 30 μm or more,
And total is evenly distributed, stablizes；As seen from Figure 4, which is mainly made of Cu, wherein there are also micro Fe and Ni are residual
It stays.
Example 2
This example prepare the method for the micro-nano laminated structure of Cu the following steps are included:
(1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: it is 17 that pure Cu, pure Ni and pure Fe powder, which are pressed atomic ratio:
After the ratio of 17:62 is mixed, in the case where water oxygen content is lower than 10ppm, vacuum condition, using using electron beam high-energy source as energy
Cu-Ni-Fe metastable state eutectic structure is prepared in the increasing material manufacturing system in amount source；
(2) it takes off alloy: obtained Cu-Ni-Fe metastable state eutectic structure is placed in the nitric acid solution of 0.03mol/L,
After placing 6 hours at room temperature, in light yellow, i.e. the de- alloy of chemistry finishes nitric acid solution；
(3) it is cleaned and dried: the Cu-Ni-Fe metastable state eutectic structure after obtained de- alloy being taken out, deionized water is first used
After Cu-Ni-Fe metastable state eutectic structure soaking and washing 3 times after obtained de- alloy, then with alcohol soaking and washing 4 times, most
It spontaneously dries 15 hours at room temperature afterwards, obtains the micro-nano laminated structure of Cu after dry, detected, obtained Cu is micro-nano
Laminated structure is stablized, and its thickness is not more than 1 micron, and length is longer than 20 microns.With reproducibility.
Example 3
This example prepare the method for the micro-nano laminated structure of Cu the following steps are included:
(1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: it is 18 that pure Cu, pure Ni and pure Fe powder, which are pressed atomic ratio:
After the ratio of 18:68 is mixed, in water oxygen content lower than under 10ppm, high-purity argon gas protective condition, utilize with electron beam high energy
Cu-Ni-Fe metastable state eutectic structure is prepared as the increasing material manufacturing system of energy source in source；
(2) it takes off alloy: obtained Cu-Ni-Fe metastable state eutectic structure is placed in the nitric acid solution of 0.07mol/L,
After placing 8 hours at room temperature, in light yellow, i.e. the de- alloy of chemistry finishes nitric acid solution；
(3) it is cleaned and dried: the Cu-Ni-Fe metastable state eutectic structure after obtained de- alloy being taken out, deionized water is first used
After Cu-Ni-Fe metastable state eutectic structure soaking and washing 1~3 time after obtained de- alloy, then with alcohol soaking and washing 2~4
It is secondary, it finally spontaneously dries 24 hours at room temperature, obtains the micro-nano laminated structure of Cu after dry, learn Cu micro-nano through measurement
The thickness of rice laminated structure is not more than 1 micron, and length is longer than 20 microns.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
It encloses, as long as that in body design thought of the invention and mentally makes has no the change of essential meaning or polishing, is solved
The technical issues of it is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (9)
1. a kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu, which comprises the following steps:
(1) increasing material manufacturing Cu-Ni-Fe metastable state eutectic structure: it is 17~18 that pure Cu, pure Ni and pure Fe powder, which are pressed atomic ratio:
After the ratio of 17~18:62~68 is mixed, Cu-Ni-Fe metastable state eutectic structure is prepared using increasing material manufacturing system；
(2) it takes off alloy: obtained Cu-Ni-Fe metastable state eutectic structure is placed in the nitric acid solution of 0.03~0.07mol/L,
It places 2~8 hours at room temperature, carries out the de- alloy of chemistry；
(3) it is cleaned and dried: the Cu-Ni-Fe metastable state eutectic structure after obtained de- alloy is taken out, successively use deionized water
With alcohol soaking and washing, the micro-nano laminated structure of Cu is obtained after dry.
2. the method that the de- alloy of a kind of chemistry according to claim 1 prepares the micro-nano laminated structure of Cu, which is characterized in that
The atomic ratio 17.5:17.5:65 of pure Cu, pure Ni and pure Fe in the step (1).
3. the method that the de- alloy of a kind of chemistry according to claim 2 prepares the micro-nano laminated structure of Cu, which is characterized in that
Increasing material manufacturing system has energy source in the step (1), and the energy source is laser or electron beam high-energy source.
4. the method that the de- alloy of a kind of chemistry according to claim 3 prepares the micro-nano laminated structure of Cu, which is characterized in that
The step (1) is to utilize increasing material system in high-purity argon gas protection or vacuum protection, and under the conditions of water oxygen content is lower than 10ppm
The system of making prepares Cu-Ni-Fe metastable state eutectic structure.
5. the method that the de- alloy of a kind of chemistry according to claim 4 prepares the micro-nano laminated structure of Cu, which is characterized in that
The increasing material manufacturing system be synchronous powder feeding system increasing material manufacturing system, and its material system be it is openable, can continuously be manufactured.
6. a kind of method that the de- alloy of chemistry prepares the micro-nano laminated structure of Cu described in any one according to claim 1~5,
It is characterized in that, the concentration of nitric acid solution is 0.05mol/L in the step (2).
7. the method that the de- alloy of a kind of chemistry according to claim 6 prepares the micro-nano laminated structure of Cu, which is characterized in that
The chemistry de- alloy time is 4~6 hours in the step (2), until solution is in light yellow.
8. the method that the de- alloy of a kind of chemistry according to claim 7 prepares the micro-nano laminated structure of Cu, which is characterized in that
In the step (3), the drying is to spontaneously dry 15~24 hours at room temperature.
9. the method that the de- alloy of a kind of chemistry according to claim 1 or claim 7 prepares the micro-nano laminated structure of Cu, feature exist
In the thickness of the micro-nano laminated structure of Cu obtained in the step (3) is not more than 1 micron, and length is 10~2000 microns.
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