CN108405868B - A kind of method that selective corrosion prepares aluminium nickel nanofiber - Google Patents
A kind of method that selective corrosion prepares aluminium nickel nanofiber Download PDFInfo
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- CN108405868B CN108405868B CN201810339019.7A CN201810339019A CN108405868B CN 108405868 B CN108405868 B CN 108405868B CN 201810339019 A CN201810339019 A CN 201810339019A CN 108405868 B CN108405868 B CN 108405868B
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- B22F9/00—Making metallic powder or suspensions thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
- B22D11/003—Aluminium alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/026—Alloys based on aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
Abstract
The invention belongs to nanofiber preparation technical fields, a kind of method that selective corrosion prepares aluminium nickel nanofiber is provided, first choice uses quickly solidification or hypergravity solidification to prepare as cast condition alumel of the nickle atom content for 2~3at.%, including alpha -aluminum matrix and aluminium nickel fiber；It uses mass concentration to carry out selective corrosion processing to as cast condition alumel for 10~30% sodium hydroxide solution, obtains suspension；Then suspension is filtered, after obtaining suspended particulate, suspended particulate is dried, obtains aluminium nickel nanofiber.The present invention is using quickly solidification or hypergravity solidification preparation as cast condition alumel, it can obtain containing alpha -aluminum matrix and the aluminium nickel fiber being distributed on matrix, in conjunction with the selective corrosion processing for the sodium hydroxide that subsequent quality concentration is 10~30%, so that alpha -aluminum matrix dissolution is in solution, and aluminium nickel fiber completely retains and is suspended in sodium hydroxide solution, again by filtering and drying process, aluminium nickel nanofiber is obtained.
Description
Technical field
The invention belongs to nanofiber technology field, in particular to a kind of selective corrosion prepares the side of aluminium nickel nanofiber
Method.
Background technique
Nanofiber refers to that diameter is less than 100nm and the longer filamentary material of length, and usually diameter is less than in practice
The material of 1000nm is also referred to as nanofiber, and specific surface area will be upper 100 times higher than micron order fiber.Due to nanofiber diameter
It is smaller, there is biggish specific surface area, be redirected so that some special physicochemical properties such as dimensional effects, molecule can be generated
With dimensional contraction etc..Nanofiber is received significant attention with its excellent physicochemical properties.
Currently, the preparation method of common nanofiber has method of electrostatic spinning and template, there is technique in these methods
Complicated disadvantage.Selective corrosion mode is increasingly becoming the preferred manner of nanofiber preparation, choosing with its simple and easy advantage
The corrosion of selecting property refers to mutually erodes one of heterogeneous alloy completely, and a kind of another mutually incorrosive investigation of materials completely
Method.
For example, document (Achim Walt etc., Nanostructuresfrom directionally solidified
NiAl-W eutectic alloys, ElectrochimicaActa, 2006,52:1799-1804) it describes and a kind of prepares Re
Or the new process of W nano wire, i.e., NiAl- (Re, W) heterogeneous alloy is first prepared using directional solidification technique, then using HCl and
H2O2Mixed liquor combine voltage selective dissolution appropriate or corrosion NiAl matrix, obtain Re nano wire or W nano wire.But
It is the HCl and H of document report2O2Mixed liquor can only prepare the nano wires of these especially corrosion resistant metals of Re and W, it is uncomfortable
In the aluminium nickel nanofiber that preparation corrosion resistance is poor.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides a kind of method that the corrosion of selecting property prepares aluminium nickel nanofiber, this
It is simple to invent the method provided, aluminium nickel nanofiber can be prepared by selective corrosion mode.
In order to achieve the above object, the invention provides the following technical scheme:
The present invention provides a kind of methods that selective corrosion prepares aluminium nickel nanofiber, include the following steps:
(1) using quickly solidification or hypergravity solidification preparation as cast condition alumel；With atomic percentage, the as cast condition aluminium
Nickel alloy contains 2~3% nickel；As cast condition alumel includes that alpha -aluminum matrix and the aluminium nickel being distributed on the alpha -aluminum matrix are fine
Dimension；
(2) the alpha -aluminum base in the as cast condition alumel for using step (1) described in sodium hydroxide solution selective corrosion to obtain
Body obtains suspension；The mass concentration of the sodium hydroxide solution is 10~30%, contains aluminium nickel fiber in the suspension；
(3) suspension that the step (2) obtains is filtered, suspended particulate is obtained；
(4) suspended particulate that the dry step (3) obtains, obtains aluminium nickel nanofiber.
Preferably, the time that selective corrosion is handled in the step (2) is 1h~2h.
Preferably, in the step (1) in as cast condition alumel the mass ratio of alpha -aluminum matrix and aluminium nickel fiber be (7.3~
11.5): 1.
Preferably, the mode quickly solidified in the step (1) is melt_spun, specifically includes: aluminium Ni-B alloy liquid is poured
Infuse the cooling roller surface of rotation.
Preferably, the temperature of the aluminium Ni-B alloy liquid is 750~950 DEG C.
Preferably, the revolving speed of the chill roll is 500~1000rpm；The material of the chill roll is pure iron or mild steel.
Preferably, the aluminium Ni-B alloy liquid is obtained by fine aluminium and pure nickel melting；The mass ratio of the fine aluminium and pure nickel is (97
~98): (3~2).
Preferably, the gravitational field in the step (1) in hypergravity process of setting is 1000~4000G.
It preferably, further include that the as cast condition alumel is carried out to broken place before step (2) the selective corrosion processing
Reason, obtains fragmentation as cast condition alumel；Full-size≤10mm of the fragmentation as cast condition alumel.
Preferably, the drying temperature in the step (4) is 80~100 DEG C；The time of the drying is 3~5h.
The present invention provides a kind of method that selective corrosion prepares aluminium nickel nanofiber, include the following steps: that first choice is adopted
The as cast condition alumel that nickle atom content is 2~3at.% is prepared with quick solidification or hypergravity solidification；Use mass concentration for
Alpha -aluminum matrix in the obtained as cast condition alumel of 10~30% sodium hydroxide solution selective corrosion, obtains containing aluminium nickel
The suspension of fiber；Then the suspension obtained described in filtering, after obtaining suspended particulate, is dried suspended particulate, obtains
Aluminium nickel nanofiber.The present invention can be obtained using quickly solidification or hypergravity solidification preparation as cast condition alumel containing alpha -aluminum
Matrix and the aluminium nickel fiber being distributed on alpha -aluminum matrix, in conjunction with the selectivity for the sodium hydroxide that subsequent quality concentration is 10~30%
Corrosion treatment, so that alpha -aluminum matrix dissolution is in solution, and aluminium nickel fiber completely retains and is suspended in sodium hydroxide solution, then leads to
Filtering and drying process, obtain aluminium nickel nanofiber.Embodiment the result shows that, above scheme provided by the invention can obtain
Diameter is in 300nm hereinafter, the aluminium nickel nanofiber that length is 10~90 μm.
Detailed description of the invention
Fig. 1 is the SEM figure of as cast condition alumel tissue made from the embodiment of the present invention 1；
Fig. 2 is the SEM figure of aluminium nickel nanofiber made from the embodiment of the present invention 1；
Fig. 3 is the SEM figure of as cast condition alumel tissue made from the embodiment of the present invention 2；
Fig. 4 is the SEM figure of aluminium nickel nanofiber made from the embodiment of the present invention 2；
Fig. 5 is the SEM figure of as cast condition alumel tissue made from the embodiment of the present invention 3；
Fig. 6 is the SEM figure of aluminium nickel nanofiber made from the embodiment of the present invention 3；
Fig. 7 is the SEM figure of as cast condition alumel tissue made from the embodiment of the present invention 4；
Fig. 8 is the SEM figure of aluminium nickel nanofiber made from the embodiment of the present invention 4；
Fig. 9 is the SEM figure of as cast condition alumel tissue made from the embodiment of the present invention 5；
Figure 10 is the SEM figure of aluminium nickel nanofiber made from the embodiment of the present invention 5；
Figure 11 is the SEM figure of as cast condition alumel tissue under 1 selective corrosion of comparative example of the present invention.
Specific embodiment
The present invention provides a kind of methods that selective corrosion prepares aluminium nickel nanofiber, include the following steps:
(1) using quickly solidification or hypergravity solidification preparation as cast condition alumel；With atomic percentage, the as cast condition aluminium
Nickel alloy contains 2~3% nickel；The as cast condition alumel includes alpha -aluminum matrix and the aluminium nickel that is distributed on the alpha -aluminum matrix
Fiber；
(2) the alpha -aluminum base in the as cast condition alumel for using step (1) described in sodium hydroxide solution selective corrosion to obtain
Body obtains suspension；The mass concentration of the sodium hydroxide solution is 10~30%, contains aluminium nickel fiber in the suspension；
(3) suspension that the step (2) obtains is filtered, suspended particulate is obtained；
(4) suspended particulate that the dry step (3) obtains, obtains aluminium nickel nanofiber.
The present invention is using quickly solidification or hypergravity solidification preparation as cast condition alumel.The present invention uses the quick solidification
Or hypergravity solidifies the alloy structure for the as cast condition alumel being prepared and includes alpha -aluminum matrix and be distributed in the alpha -aluminum matrix
On aluminium nickel fiber.The mass ratio of alpha -aluminum matrix and aluminium nickel fiber is preferably (7.3 in the as cast condition alumel in the present invention
~11.5): 1, further preferably (7.9~10.4): 1.In the present invention, chemical composition is nickel in the as cast condition alumel
And aluminium；In terms of atomic percentage content, in the as cast condition alumel content of nickel be 2~3at.%, preferably 2.2~
2.8at.%；In an embodiment of the present invention, specially 2.4at.%, 2.5at.%, 2.6at.% or 2.7at.%.
In the present invention, when using quickly solidification preparation as cast condition alumel, the mode quickly solidified is preferably
Melt_spun specifically includes: aluminium Ni-B alloy liquid is poured into the cooling roller surface of rotation.In the present invention, the teeming rate
Preferably 5~10kg/min, further preferably 6~8kg/min.In the present invention, the temperature of the aluminium Ni-B alloy liquid is preferred
It is 750~950 DEG C, further preferably 780~940 DEG C, more preferably 800~920 DEG C；In an embodiment of the present invention, institute
The temperature for stating aluminium Ni-B alloy liquid is specially 760 DEG C, 770 DEG C, 790 DEG C, 710 DEG C, 720 DEG C, 730 DEG C, 770 DEG C, 790 DEG C, 810
DEG C, 830 DEG C, 850 DEG C, 870 DEG C or 900 DEG C.The present invention controls the temperature of aluminium Ni-B alloy liquid in rapid solidification, avoids temperature
Aluminium Ni-B alloy liquid poor fluidity caused by too low, caused by spray nozzle clogging, be also avoided that oxidation caused by temperature is excessively high, Ji Nengbao
Card aluminium Ni-B alloy liquid has preferable mobility, and does not allow oxidizable, realization quickly solidification, and then obtain having by alpha -aluminum and aluminium
Two kinds of the nickel nanofiber alumel thin slices mutually constituted.In the present invention, the atomic percent of nickel contains in the aluminium Ni-B alloy liquid
Amount is preferably 2~3at.%, further preferably 2.2~2.8at.%；In an embodiment of the present invention, specially
2.4at.%, 2.5at.%, 2.6at.% or 2.7at.%.In the present invention, as cast condition alumel aluminium Ni-B alloy liquid is prepared
Middle nickel is consistent with the content of nickel in the as cast condition alumel.
In the present invention, the aluminium Ni-B alloy liquid is preferably obtained by fine aluminium and pure nickel melting.The present invention to the fine aluminium and
The specific source of pure nickel does not have particular/special requirement, using well-known to those skilled in the art.In the present invention, the fine aluminium
The mass ratio of the material with pure nickel is preferably (97~98): (3~2), further preferably (97.2~97.8): (2.8~2.2)；
In an embodiment of the present invention, the mass ratio of the material of the fine aluminium and pure nickel be specially 97:3,97.8:2.2,97.6:2.4,
97.5:2.5,97.4:2.6,97.3:2.7 or 97.2:2.8.The present invention does not have special want to the specific embodiment of the melting
It asks, using Metal Melting mode well-known to those skilled in the art.In an embodiment of the present invention, the melting is specific
It is carried out in resistance furnace or induction heater.
The aluminium Ni-B alloy liquid is poured into the cooling roller surface of rotation by the present invention, is carried out melt_spun, is realized fast rapid hardening
Gu obtaining as cast condition alumel.In the present invention, the revolving speed of the chill roll is preferably 500~1000rpm, further preferably
For 550~950rpm, more preferably 600~900rpm, most preferably 700~800rpm；In an embodiment of the present invention, described
The revolving speed of chill roll be specially 520rpm, 570rpm, 590rpm, 610rpm, 630rpm, 670rpm, 710rpm, 740rpm,
770rpm, 810rpm, 860rpm, 920rpm, 940rpm, 970rpm or 990rpm.In the present invention, the material of the chill roll
Preferably pure iron or mild steel；The temperature of the chill roll is preferably room temperature.The present invention has two using the effect of the chill roll
A aspect: one is that by the quick solidification of alumel, obtain have mutually constituted for two kinds by alpha -aluminum with aluminium nickel nanofiber
Alumel thin slice；Help to obtain aluminium nickel nanofiber during subsequent selective corrosion；Second is that chill roll material
For pure iron or mild steel, it is different from single roller at present and gets rid of band field copper roller currently in use, its advantage is that iron roll surface will not be with aluminium
The reaction of Ni-B alloy liquid, and copper roller surface can be reacted with aluminium Ni-B alloy liquid.Specific embodiment of the present invention to the melt_spun
There is no particular/special requirement, using well-known to those skilled in the art.In an embodiment of the present invention, the melt_spun tool
Body gets rid of band machine by single roller and completes.
The present invention is solidified using the aluminium Ni-B alloy liquid, it is ensured that obtained alumel, there are two types of phase structures for tool, i.e.,
Alpha -aluminum+aluminium nickel fiber.
When the present invention is using the quick solidification mode preparation as cast condition alumel, cooling rate is big, and phase structure will become
Tiny, aluminium nickel fiber will become aluminium nickel nanofiber, it is ensured that the alumel after solidification has such as undertissue: alpha -aluminum matrix+aluminium
Nickel nanofiber, convenient for only corroding alpha -aluminum matrix in subsequent selective corrosion process, without corroding aluminium nickel nanofiber, because
And alpha -aluminum matrix is dissolved, and aluminium nickel nanofiber will be left behind, and eventually pass through the available aluminium nickel nanofiber of filter.
When using hypergravity solidification preparation as cast condition alumel, specific embodiment party that the present invention solidifies the hypergravity
Formula does not have particular/special requirement, using mode well-known to those skilled in the art；Aluminium Ni-B alloy liquid is made in super gravity field
Cooled and solidified is carried out under.In the present invention, the super gravity field in the hypergravity process of setting is preferably 1000~4000G,
Further preferably 1200~3800G, more preferably 1500~3500G, most preferably 2000~3000G.In the present invention, institute
It is consistent with the aluminium Ni-B alloy liquid in above-mentioned flash set technology scheme to state aluminium Ni-B alloy liquid, details are not described herein.
When the present invention is using hypergravity solidification mode preparation as cast condition alumel, when super gravity field is greater than 1000G,
Phase structure will become tiny, and aluminium nickel fiber becomes aluminium nickel nanofiber；Alumel after ensuring to solidify has such as undertissue: α-
Aluminum substrate+aluminium nickel nanofiber.In this way, only corroding alpha -aluminum matrix in subsequent selective corrosion process, received without corroding aluminium nickel
Rice fiber, thus alpha -aluminum matrix is dissolved, and aluminium nickel nanofiber will be left behind, and eventually pass through the available aluminium nickel Nanowire of filter
Dimension.
After obtaining as cast condition alumel, the present invention is using in as cast condition alumel described in sodium hydroxide solution selective corrosion
Alpha -aluminum matrix, obtain suspension；Selective corrosion mechanism of the present invention is that pure aluminum can be reacted with sodium hydroxide solution, is formed
Sodium aluminate solution；And the aluminium in aluminium nickel fiber phase has formd aluminium nickel intermetallic compound with nickel, key is covalent bond, knot
Structure is stablized, and sodium hydroxide solution cannot be reacted with aluminium nickel intermetallic compound.In the present invention, the matter of the sodium hydroxide solution
Measuring concentration is preferably 10~30%, and further preferably 12~28%, more preferably 15~25%, most preferably 18~20%.
In the present invention, the time of the selective corrosion processing is preferably 1h~2h, further preferably 1.2~1.5h.In this hair
In bright, the as cast condition alumel is preferably immersed in the sodium hydroxide solution by the mode of the selective corrosion processing
In；In the present invention, in the sodium hydroxide solution in sodium hydroxide and as cast condition alumel the mass ratio of aluminium be preferably (3~
8): 1, further preferably (4~5): 1.The present invention selects the as cast condition alumel using the sodium hydroxide solution
The corrosion treatment of selecting property, alpha -aluminum matrix, which is corroded, in the as cast condition alumel is dissolved into sodium hydroxide solution, and is distributed originally
Aluminium nickel fiber suspension on the alpha -aluminum matrix forms suspension in sodium hydroxide solution.In the present invention, the suspension
The aluminium nickel fiber of meta-aluminic acid radical ion and suspension containing dissolution in liquid.
Before the selective corrosion, the as cast condition alumel is preferably carried out break process by the present invention, obtains fragmentation casting
State alumel carries out selective corrosion to the fragmentation as cast condition alumel.The present invention is not special to the crumbling method
It is required that being become smaller i.e. using alloy breaks down mode well-known to those skilled in the art with being able to achieve the size of as cast condition alumel
It can.In the present invention, the fragmentation as cast condition alumel full-size preferably≤10mm, further preferably≤5mm.The present invention
The diminution of as cast condition alumel size is realized in such a way that the as cast condition alumel that will be obtained is broken, it is rotten convenient for subsequent selective
During erosion, with coming into full contact with for sodium hydroxide solution, corrosion efficiency is improved.
After obtaining suspension, the present invention is filtered the suspension, obtains suspended particulate.In the present invention, described
The mode of filtering preferably includes filter paper filtering or vacuum filtration.The present invention does not have particular/special requirement to the mode of the filtering, uses
Separation well-known to those skilled in the art to be able to achieve suspended particulate and solution.
After obtaining suspended particulate, the suspended particulate is dried the present invention, obtains aluminium nickel nanofiber.In the present invention
In, the temperature of the drying is preferably 80~100 DEG C；The time of the drying is preferably 3~5h, further preferably 4h.This
The drying process is passed through in invention, realizes the removal to moisture, weakens the oxidation of aluminium nickel nanofiber.
Before the drying, the present invention preferably washs the suspended particulate, obtains clean suspended particulate.In this hair
In bright, the washing is preferably distilled water with detergent；The number of the washing is preferably 3 times；The present invention uses the washing
Removal of the time to residual solution in suspended particulate improves the purity of aluminium nickel nanofiber.
The diameter of the aluminium nickel nanofiber that the present invention obtains preferably≤300nm, further preferred 150~280nm, more preferably
150~250nm, most preferably 150~200nm；The length of the aluminium nickel nanofiber is preferably 10~90 μm, further preferably
It is 10~60 μm, more preferably 15~50 μm.In the present invention, the aluminium nickel nanofiber macroscopic view is powder.In the present invention,
The aluminium nickel nanofiber has diameter small, and draw ratio is big, and specific surface area is high, the high excellent properties of activity.
Aluminium Ni-B alloy liquid within the scope of present component is after conventional coagulation, and aluminium nickel fiber is compared in obtained alumel
Coarseer, diameter is about 0.5~1 μm.When the present invention is using the quick solidification mode preparation as cast condition alumel, cooling speed
Rate is big, and phase structure will become tiny, and aluminium nickel fiber will become aluminium nickel nanofiber, and diameter refine to 150 by 0.5~1 μm~
200nm, specific surface area increase by 11~25 times.Preparation of the present invention also for aluminium nickel nanofiber is provided using sodium hydroxide solution
The new approaches of selective corrosion preparation.
In order to further illustrate the present invention, it with reference to the accompanying drawings and examples prepared by selective corrosion provided by the invention
The method of aluminium nickel nanofiber is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using aluminium block (purity 99.99wt.%), nickel sheet (purity 99.95wt.%) is raw material, according to Al
The atom ratio of 97.6at.% and Ni 2.4at% prepares the alloy raw material that gross mass is 100g, puts it into graphite crucible
In, then be put into togerther in the heating furnace that temperature is 800 DEG C together with crucible and carry out melting, it is kept the temperature after it is completely melt half small
When, so that the temperature of melt is maintained at 800 DEG C.
Band machine is got rid of using single roller above-mentioned melt is injected into pure iron roller surfaces and get rid of band, realizes that quickly solidification obtains
The sheet alumel of as cast condition, the temperature control of melt is 800 DEG C when getting rid of band, and teeming rate control is 10kg/min；Roller
Revolving speed be limited to 500rpm.
Microstructure observation is carried out to as cast condition alumel is obtained, as a result as shown in Figure 1, it is seen then that quickly obtain after solidification
The tissue of as cast condition alumel be aluminum substrate and the aluminium nickel fiber that is distributed on aluminum substrate, wherein the diameter of aluminium nickel fiber is about
250~300nm.
The alumel of above-mentioned as cast condition is carried out to be broken into the strip alumel that full-size is several millimeters；
10 grams of above-mentioned strip alumel is taken, being put into 400mL mass concentration is to be corroded in 10wt.%NaOH solution
Reaction, reaction time 1.5h, by the aluminum substrate corrosion dissolution in alumel, aluminium nickel fiber suspension is in sodium hydroxide solution
In, obtain suspension；
Above-mentioned suspension is filtered using filter paper and vacuum filtration machine, suspended particulate is obtained, using distilled water solution
Three times to suspended particulate washing, finally the suspended particulate after washing is put into the vacuum oven that temperature is 80 DEG C, drying 4 is small
When after take out, obtain alumel nanometer fibre powder.
The SEM pattern of gained alumel nanometer fibre powder is as shown in Fig. 2, the diameter of aluminium nickel nanometer fibre powder exists
Between 250~300nm, length is 20~80 μm.
Embodiment 2
Using aluminium block (purity 99.99wt.%), nickel sheet (purity 99.95wt.%) is raw material, according to Al
The atom ratio of 97.5at.% and Ni 2.5at% prepares the alloy raw material that gross mass is 100g, puts it into graphite crucible
In, then be put into togerther in the heating furnace that temperature is 850 DEG C together with crucible and carry out melting, it is kept the temperature after it is completely melt half small
When, so that the temperature of melt is maintained at 850 DEG C.
Band machine is got rid of using single roller above-mentioned melt is injected into mild steel roller surfaces and get rid of band, realization quickly solidifies
To the sheet alumel of as cast condition, the temperature of melt is 850 DEG C when getting rid of band；Teeming rate control is 8kg/min, and roller turns
Speed limit is set to 1000rpm.
Microstructure observation is carried out to obtained as cast condition alumel, as a result as shown in Figure 3, it is seen then that quickly after solidification
To the tissue of as cast condition alumel be aluminum substrate and the aluminium nickel fiber that is distributed on aluminum substrate.
The alumel of above-mentioned as cast condition is carried out to be broken into the strip alumel that full-size is several millimeters of sizes；
10 grams of above-mentioned strip alumel is taken, is put into the NaOH solution that 250mL mass concentration is 20% and is corroded
Reaction, by the aluminum substrate corrosion dissolution in alumel, aluminium nickel fiber suspension obtains suspension in sodium hydroxide solution；
Above-mentioned suspension is filtered using filter paper and vacuum filtration machine, suspended particulate is obtained, using distilled water solution
Three times to suspended particulate washing, finally the suspended particulate after washing is put into the vacuum oven that temperature is 80 DEG C, drying 4 is small
When after take out, obtain alumel nanometer fibre powder.
The SEM pattern of gained alumel nanometer fibre powder is as shown in figure 4, the diameter of aluminium nickel nanometer fibre powder exists
Between 200~250nm, length is 20~60 μm.
Embodiment 3
Using aluminium block (purity 99.99wt.%), nickel sheet (purity 99.95wt.%) is raw material, according to Al
The atom ratio of 97.4at.% and Ni 2.6at% prepares the alloy raw material that gross mass is 100g, puts it into graphite crucible
In, then be put into togerther in the heating furnace that temperature is 850 DEG C together with crucible and carry out melting, it is kept the temperature after it is completely melt half small
When, so that the temperature of melt is maintained at 850 DEG C.
Band machine is got rid of using single roller above-mentioned melt is injected into mild steel roller surfaces and get rid of band, realization quickly solidifies
To the sheet alumel of as cast condition, the temperature of melt is 850 DEG C when getting rid of band；Teeming rate control is 6kg/min, and roller turns
Speed limit is set to 600rpm.
Microstructure observation is carried out to obtained as cast condition alumel, as a result as shown in Figure 5, it is seen then that quickly after solidification
To the tissue of as cast condition alumel be aluminum substrate and the aluminium nickel fiber that is distributed on aluminum substrate.
The alumel of above-mentioned as cast condition is carried out to be broken into the strip alumel that full-size is several millimeters of sizes；It takes
10 grams of above-mentioned strip alumel is put into 200mL and is put into mass concentration to carry out corrosion reaction in 30% NaOH solution, obtains
To suspension；
Above-mentioned suspension is filtered using filter paper and vacuum filtration machine, suspended particulate is obtained, using distilled water solution
Three times to suspended particulate washing, finally the suspended particulate after washing is put into the vacuum oven that temperature is 80 DEG C, drying 4 is small
When after take out, obtain alumel nanometer fibre powder.
The SEM pattern of gained alumel nanometer fibre powder is as shown in fig. 6, the diameter of aluminium nickel nanometer fibre powder exists
Between 180~200nm, length is 15~50 μm.
Embodiment 4
Using aluminium block (purity 99.99wt.%), nickel sheet (purity 99.95wt.%) is raw material, according to Al
The atom ratio of 97.3at.% and Ni 2.7at% prepares the alloy raw material that gross mass is 100g, puts it into graphite crucible
In, then be put into togerther in the heating furnace that temperature is 900 DEG C together with crucible and carry out melting, it is kept the temperature after it is completely melt half small
When, so that the temperature of melt is maintained at 900 DEG C.
Above-mentioned melted melt is put into togerther hypergravity coagulating machine together with graphite crucible and carries out hypergravity solidification, is surpassed
Gravitational field size is set as 1000G；
Microstructure observation is carried out to obtained as cast condition alumel, as a result as shown in Figure 7, it is seen then that after hypergravity solidification
The tissue of obtained as cast condition alumel is aluminum substrate and the aluminium nickel fiber being distributed on aluminum substrate.
The alumel of above-mentioned as cast condition is carried out to be broken into the small blocky alumel that full-size is several millimeters of sizes；It takes
10 grams of above-mentioned strip alumel is put into the NaOH solution that 300mL mass concentration is 20% and carries out corrosion reaction, by aluminium nickel
Aluminum substrate corrosion dissolution in alloy, aluminium nickel fiber suspension obtain suspension in sodium hydroxide solution；
Above-mentioned suspension is filtered using filter paper and vacuum filtration machine, suspended particulate is obtained, using distilled water solution
Three times to suspended particulate washing, finally the suspended particulate after washing is put into the vacuum oven that temperature is 80 DEG C, drying 4 is small
When after take out, obtain alumel nanometer fibre powder.
The SEM pattern of gained alumel nanometer fibre powder is as shown in figure 8, the diameter of aluminium nickel nanometer fibre powder exists
Between 250~300nm, length is 10~40 μm.
Embodiment 5
Using aluminium block (purity 99.99wt.%), nickel sheet (purity 99.95wt.%) is raw material, according to Al
The atom ratio of 97at.% and Ni 3at% is prepared the alloy raw material that gross mass is 100g, is put it into graphite crucible, then
It is put into togerther in the heating furnace that temperature is 900 DEG C together with crucible and carries out melting, kept the temperature half an hour after it is completely melt, make to melt
The temperature for changing liquid is maintained at 900 DEG C.
Above-mentioned melted melt is put into togerther hypergravity coagulating machine together with graphite crucible and carries out hypergravity solidification, is surpassed
Gravitational field size is set as 5000G；
Microstructure observation is carried out to obtained as cast condition alumel, as a result as shown in Figure 9, it is seen then that after hypergravity solidification
The tissue of obtained as cast condition alumel is aluminum substrate and the aluminium nickel fiber being distributed on aluminum substrate.
The alumel of above-mentioned as cast condition is carried out to be broken into the small blocky alumel that full-size is several millimeters of sizes；It takes
10 grams of above-mentioned strip alumel is put into the NaOH solution that 300mL mass concentration is 20% and carries out corrosion reaction, by aluminium nickel
Aluminum substrate corrosion dissolution in alloy, aluminium nickel fiber suspension obtain suspension in sodium hydroxide solution；
Above-mentioned suspension is filtered using filter paper and vacuum filtration machine, suspended particulate is obtained, using distilled water solution
Three times to suspended particulate washing, finally the suspended particulate after washing is put into the vacuum oven that temperature is 80 DEG C, drying 4 is small
When after take out, obtain alumel nanometer fibre powder.
The SEM pattern of gained alumel nanometer fibre powder is as shown in Figure 10, and the diameter of aluminium nickel nanometer fibre powder exists
Between 180~200nm, length is 15~50 μm.
Specific surface area performance detection, knot are carried out to the aluminium nickel nanofiber that Examples 1 to 5 obtains using laser particle analyzer
Fruit is respectively 4.9m2/g、6.1m2/g、7.0m2/g、4.9m2/ g and 7.0m2/g。
Comparative example 1
Aluminium nickel nanofiber is prepared in the way of embodiment 1, difference is, uses mass concentration for 25%HNO3Instead of
Mass concentration is that 10%NaOH solution-selective corrodes alumel, and the microstructure of obtained alumel is as shown in figure 11,
As seen from the figure, alpha -aluminum matrix and aluminium nickel fiber are all corroded in corrosion process, and selective corrosion effect is not obvious, using this
Aluminium nickel nanofiber can not be made in kind corrosive agent.
As seen from the above embodiment, the present invention diameter can be prepared in 300nm hereinafter, and length at 10~90 μm
Aluminium nickel nanofiber.Method provided by the invention is simple, easily operated with preparation process, is easily achieved large-scale industrial production
The features such as；And metallic aluminium, metallic nickel and the NaOH used in preparation process of the present invention is the common raw material of industry, has valence
Lattice are cheap, are easy the characteristics of purchasing.
Although above-described embodiment is made that detailed description to the present invention, it is only a part of the embodiment of the present invention,
Rather than whole embodiments, people can also obtain other embodiments under the premise of without creativeness according to the present embodiment, these
Embodiment belongs to the scope of the present invention.
Claims (8)
1. a kind of method that selective corrosion prepares aluminium nickel nanofiber, includes the following steps:
(1) as cast condition alumel is prepared using quickly solidification；With atomic percentage, the as cast condition alumel contains 2~3%
Nickel；The as cast condition alumel includes alpha -aluminum matrix and the aluminium nickel nanofiber that is distributed on the alpha -aluminum matrix；
(2) the alpha -aluminum matrix in the as cast condition alumel for using step (1) described in sodium hydroxide solution selective corrosion to obtain, obtains
To suspension；The mass concentration of the sodium hydroxide solution is 20~30%, sodium hydroxide and casting in the sodium hydroxide solution
The mass ratio of aluminium is 3~8:1 in state alumel, contains aluminium nickel nanofiber in the suspension；
(3) suspension that the step (2) obtains is filtered, suspended particulate is obtained；
(4) suspended particulate that the dry step (3) obtains, obtains aluminium nickel nanofiber；
The mode quickly solidified in the step (1) is melt_spun, specifically includes: aluminium Ni-B alloy liquid is poured into the cold of rotation
But roller surface；
The diameter of the aluminium nickel nanofiber is 150~300nm；
The length of the aluminium nickel nanofiber is 10~90 μm.
2. preparation method according to claim 1, which is characterized in that in the step (2) selective corrosion handle when
Between be 1h~2h.
3. preparation method according to claim 1, which is characterized in that alpha -aluminum in as cast condition alumel in the step (1)
The mass ratio of matrix and aluminium nickel nanofiber is (7.3~11.5): 1.
4. preparation method according to claim 1, which is characterized in that the temperature of the aluminium Ni-B alloy liquid is 750~950
℃。
5. preparation method according to claim 1, which is characterized in that the aluminium Ni-B alloy liquid is obtained by fine aluminium and pure nickel melting
It arrives；The mass ratio of the fine aluminium and pure nickel is (97~98): (3~2).
6. preparation method according to claim 1, which is characterized in that the revolving speed of the chill roll is 500~1000rpm；
The material of the chill roll is pure iron or mild steel.
7. preparation method according to claim 1, which is characterized in that further include before step (2) selective corrosion by
The as cast condition alumel carries out break process, obtains fragmentation as cast condition alumel；The maximum of the fragmentation as cast condition alumel
Size≤10mm.
8. preparation method according to claim 1, which is characterized in that the drying temperature in the step (4) is 80~100
℃；The time of the drying is 3~5h.
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| WO2006084128A2 (en) * | 2005-02-04 | 2006-08-10 | Brown University | Apparatus, method and computer program product providing radial addressing of nanowires |
| CN103774149A (en) * | 2014-02-10 | 2014-05-07 | 天津工业大学 | Preparation method of high-strength nano-porous nickel film |
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| WO2006084128A2 (en) * | 2005-02-04 | 2006-08-10 | Brown University | Apparatus, method and computer program product providing radial addressing of nanowires |
| CN103774149A (en) * | 2014-02-10 | 2014-05-07 | 天津工业大学 | Preparation method of high-strength nano-porous nickel film |
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