CN103882489B - Preparation method of magnetic alloy nanowire with diameter gradient - Google Patents
Preparation method of magnetic alloy nanowire with diameter gradient Download PDFInfo
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- CN103882489B CN103882489B CN201410052432.7A CN201410052432A CN103882489B CN 103882489 B CN103882489 B CN 103882489B CN 201410052432 A CN201410052432 A CN 201410052432A CN 103882489 B CN103882489 B CN 103882489B
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- 239000002070 nanowire Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910001004 magnetic alloy Inorganic materials 0.000 title claims abstract description 20
- 230000005291 magnetic effect Effects 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 37
- 230000003647 oxidation Effects 0.000 claims description 30
- 238000007254 oxidation reaction Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- 238000009415 formwork Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 10
- 238000004070 electrodeposition Methods 0.000 claims description 10
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008151 electrolyte solution Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 229910000838 Al alloy Inorganic materials 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006056 electrooxidation reaction Methods 0.000 abstract description 5
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 229910000990 Ni alloy Inorganic materials 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 244000025254 Cannabis sativa Species 0.000 description 3
- 229910000531 Co alloy Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The invention provides a preparation method of a magnetic alloy nanowire with diameter gradient, which comprises the following steps: preparing an aluminum oxide film with nano pores with diameter gradient by using an electrochemical corrosion principle; and on the basis of the anodic aluminum oxide template, carrying out direct current deposition by using a dual-electrode system to reduce and crystallize metal ions in the nano pores to finally generate the target product alloy nanowire. The preparation method can be used for preparing the magnetic alloy nanowire with uniform diameter variation, is a new attempt, and has far-reaching significance for promoting development of magnetic recording industry.
Description
(1) technical field
The present invention relates to a kind of preparation method of the magnetic alloy nano wire with diameter gradient.
(2) background technology
Nano wire refers to that diameter is in nanoscale scope (1～100nm) and has the one-dimensional linear material of very high length-diameter ratio
Material.Nano wire not only has the characteristic of nanoparticle, such as quantum size effect, small-size effect, skin effect and macroscopic quantum
Tunnel-effect etc., there are the new effect that nanostructured combination causes, such as quantum coupling and cooperative effect etc., thus showing again
The electronics of uniqueness, magnetics, optics and catalytic property.
For magnetic nanometer, because high length-diameter ratio can lead to it to have significant magnetic anisotropy, particularly work as magnetic
When material enters nanoscale, multidomain will become single domain, thus showing extremely strong superparamagnetic e ffect.If by every magnetic Nano
Line is as an information memory cell, then the memory density of Magnetic Nanowire Arrays can exceed 15gbit/cm2, much high
Memory density (0.6gbit/cm in now widely used hard disc of computer2).Thus, magnetic nanometer is remembered in high density magnetic
The association areas such as record have huge potential application foreground.
In the nano wire of synthesizing magnetic currently reported out, either alloy or ferrite, almost it is all homogeneous diameter
Nano wire, and mono-disperse magnetic alloy nano wire all has the characteristics that magnetic shape anisotropy, this allows for single magnetic Nano
Line is typically only capable of as an information memory cell under single domain state.If magnetic nanometer can present in the longitudinal direction
Microstructural space consecutive variations, that is, synthesize a kind of magnetic nanometer with one-dimensional gradient it would be possible to make one
Magnetic nanometer has multiple information memory cells, thus realize the vertical perpendicular and parallel two-way of gradient magnetic nano-wire array depositing
Storage, this will be significantly greatly increased the memory density of medium.
(3) content of the invention
It is an object of the invention to provide a kind of preparation method of the magnetic alloy nano wire with graded diameter, the method energy
Enough prepare the magnetic alloy nano wire of uniform diameter change.
The technical solution used in the present invention is:
A kind of preparation method of the magnetic alloy nano wire with diameter gradient, methods described includes:
(1) template is prepared and (is prepared the aluminum oxide film of the nano pore with diameter gradient using electrochemical corrosion principle
Film):
(1) aluminium flake pretreatment: aluminium flake prior to 500 DEG C at anneal 2～4 hours, then ultrasonic 10min in acetone, then
Mass concentration be 5% sodium hydroxide solution in soak 5min, finally ultrasonic 3min in acetone；Aluminium flake used selects high-quality high
The aluminium flake of pure (purity is 99.999%) is preferably；
(2) aoxidize for the first time: pretreated aluminium flake is corroded 4～6 hours under direct current 40～60v voltage, electrolyte
Oxalic acid solution for concentration 0.3m～0.4m；
(3) remove once oxidation film: at 65 DEG C, aluminium flake is placed in h3po4Mass concentration 6%, cro3Mass concentration 1.5%
Process 20min～45min in mixed liquor, remove once oxidation film；
(4) aoxidize for second: aluminium flake carries out second oxidation, and oxidation voltage is uniformly passed in 8～12 hours from 25～40v
Increase to 40～60v (be at the uniform velocity incremented to 40v from 25v preferably in 8～12 hours or be at the uniform velocity incremented to 60v from 40v), electrolyte is
The oxalic acid solution of concentration 0.3m～0.4m；
(5) reaming: at 35 DEG C, aluminium flake is placed in the h of mass concentration 5%3po4Reaming 20～45min in solution, obtains anode
Alumina formwork；
(2) (on the basis of the anodic oxidation aluminium formwork of preparation, using two electrode systems, unidirectional current sinks DC electrodeposition
Long-pending method makes metal ion reduce in nano pore, crystallizes, and ultimately produces target product alloy nano-wire):
Using the anodic oxidation aluminium formwork of preparation as anode, with graphite flake as negative electrode, in the electrolytic solution under magnetic agitation
Carry out DC electrodeposition and prepare nano wire, direct current power source voltage is 2v～4v, temperature is room temperature；Electrolyte composition is as follows:
coso4·7h2o、niso4·7h2o、feso4·7h2Any two kinds of each 80～100g/l, boric acid 30～45g/l in o, anti-bad
Hematic acid 15g/l, solvent is water, ph 3～4 (being adjusted with sulphuric acid)；
(3) discharge nano wire:
Post-depositional anodic oxidation aluminium formwork soaks in the naoh solution of mass concentration 5%, fully go oxide film dissolving and
Aluminum substrate, obtains final product described magnetic alloy nano wire.
The invention provides a kind of preparation method of the magnetic alloy nano wire with graded diameter, the method can be prepared
The magnetic alloy nano wire of uniform diameter change, is a kind of new trial, has far reaching significance to promoting magnetic recording industry development.
(4) brief description
Fig. 1 is the alumina formwork electromicroscopic photograph of the fe-ni magnetic alloy nano wire of embodiment 1 preparation；
Fig. 2 is the alumina formwork electromicroscopic photograph of the co-ni magnetic alloy nano wire of embodiment 2 preparation；
Fig. 3 is the alumina formwork electromicroscopic photograph of the fe-co magnetic alloy nano wire of embodiment 3 preparation.
(5) specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This:
Embodiment 1:
A kind of preparation method of the fe-ni magnetic alloy nano wire with graded diameter, comprises the steps:
(1) prepare template
(1-1) select the aluminium flake of high-quality high-purity (purity is 99.999%), anneal 2 hours at 500 DEG C, ultrasonic in acetone
10min, then concentration be 5% (wt) sodium hydroxide solution in soak 5min, finally ultrasonic 3min in acetone, complete aluminium flake
Pretreatment.
(1-2) there is the aluminum oxide film of the nano pore of diameter gradient using the preparation of electrochemical corrosion principle.This process
Using electrochemical erosion method twice, oxidation for the first time is corroded 5 hours under direct current 40v voltage, and electrolyte is the grass of concentration 0.3m
Acid solution.
(1-3) remove once oxidation film.Aluminium flake is placed in 6%h3po4And 1.5%cro (wt)3(wt) 65 in mixed liquor
Under the conditions of DEG C, 1.5h removes once oxidation film.
(1-4) aoxidize for second.Oxidation voltage at the uniform velocity boosted to 40v from 25v in 6 hours, and electrolyte is concentration 0.3m
Oxalic acid solution.
(1-5) reaming.Finally in 5% (wt) h3po435 DEG C of reaming 20min in solution.
The electromicroscopic photograph of prepared alumina formwork is shown in Fig. 1 it is seen that in nano pore, along on axis direction, duct
Diameter has continuous diameter change, obtains the nano pore that relative diameter is varied from it is ensured that obtaining becoming with gradient
The fe-ni alloy nano-wire changed.
(2) electro-deposition
With the anodic oxidation aluminium formwork of aforementioned preparation as anode, with graphite flake as negative electrode, make metal using electro-deposition method
Ion reduces in nano pore, crystallization, ultimately produces target product fe-ni alloy nano-wire.DC voltage 2v, 8 points of time
Clock, plus magnetic agitation, temperature conditionss are room temperature.Bath composition: niso4·7h2o 80g/l,feso4·7h2O 80g/l, boron
Sour 30g/l, ascorbic acid 15g/l, ph value is 3, and solvent is water.
(3) discharge nano wire
Post-depositional alumina formwork is placed in 5% (wt) naoh solution and soaks, and fully removes oxide film dissolving and aluminum substrate, obtains
To purer fe-ni alloy nano-wire.
Embodiment 2:
A kind of preparation method of the co-ni magnetic alloy nano wire with graded diameter, comprises the steps:
(1) prepare template
(1-1) select the aluminium flake of high-quality high-purity (purity is 99.999%), anneal 3 hours at 500 DEG C, ultrasonic in acetone
10min, then concentration be 5% (wt) sodium hydroxide solution in soak 5min, finally ultrasonic 3min in acetone, complete aluminium flake
Pretreatment.
(1-2) there is the aluminum oxide film of the nano pore of diameter gradient using the preparation of electrochemical corrosion principle.This process
Using electrochemical erosion method twice, oxidation for the first time is corroded 5 hours under direct current 60v voltage, and electrolyte is the grass of concentration 0.35m
Acid solution.
(1-3) remove once oxidation film.Aluminium flake is placed in 6%h3po4And 1.5%cro (wt)3(wt) 65 in mixed liquor
DEG C condition 2h that goes down removes once oxidation film.
(1-4) aoxidize for second.Oxidation voltage uniformly increased to 60v from 40v in 8 hours, and electrolyte is concentration 0.35m
Oxalic acid solution.
(1-5) reaming.Last 35 DEG C of reaming 45min in 5%h3po4 (wt) solution.
The electromicroscopic photograph of prepared alumina formwork is shown in Fig. 2 it is seen that in nano pore, along on axis direction, duct
Diameter has continuous diameter change, obtains the nano pore that relative diameter is varied from it is ensured that obtaining becoming with gradient
The co-ni alloy nano-wire changed.
(2) electro-deposition
With the anodic oxidation aluminium formwork of aforementioned preparation as anode, with graphite flake as negative electrode, make metal using electro-deposition method
Ion reduces in nano pore, crystallizes, and ultimately produces target product co-ni alloy nano-wire.DC voltage 3v, 10 points of time
Clock, plus magnetic agitation, temperature conditionss are room temperature.Bath composition: niso4·7h2o(90g/l),coso4·7h2O 90g/l,
Boric acid 40g/l, ascorbic acid 15g/l, ph value is 3.5, and solvent is water.
(3) discharge nano wire
Post-depositional anodic oxidation aluminium formwork soaks in 5% (wt) naoh solution, fully removes oxide film dissolving and aluminum substrate,
Obtain purer co-ni alloy nano-wire.
Embodiment 3:
A kind of preparation method of the fe-co magnetic alloy nano wire with graded diameter, comprises the steps:
(1) prepare template
(1-1) select the aluminium flake of high-quality high-purity (purity is 99.999%), anneal 4 hours at 500 DEG C, ultrasonic in acetone
10min, then concentration be 5% (wt) sodium hydroxide solution in soak 5min, finally ultrasonic 3min in acetone, complete aluminium flake
Pretreatment.
(1-2) there is the aluminum oxide film of the nano pore of diameter gradient using the preparation of electrochemical corrosion principle.This process
Using electrochemical erosion method twice the, once oxidation corrodes 5 hours under direct current 40v voltage, and electrolyte is the grass of concentration 0.4m
Acid solution.
(1-3) remove once oxidation film.Aluminium flake is placed in 6%h3po4And 1.5%cro (wt)3(wt) 65 in mixed liquor
Once oxidation film is removed under the conditions of DEG C.
(1-4) aoxidize for second.Oxidation voltage was all ramped up 40v from 25v in 7 hours, and electrolyte is concentration 0.4m
Oxalic acid solution.
(1-5) reaming.Finally in 5% (wt) h3po435 DEG C of reamings 30 minutes in solution.
The electromicroscopic photograph of prepared alumina formwork is shown in Fig. 3 it is seen that in nano pore, along on axis direction, duct
Diameter has continuous diameter change, obtains the nano pore that relative diameter is varied from it is ensured that obtaining becoming with gradient
The fe-co alloy nano-wire changed.
(2) electro-deposition
With the anodic oxidation aluminium formwork of aforementioned preparation as anode, with graphite flake as negative electrode, make metal using electro-deposition method
Ion reduces in nano pore, crystallizes, and ultimately produces target product fe-co alloy nano-wire.DC voltage 4v, 15 points of time
Clock, plus magnetic agitation, temperature conditionss are room temperature.Bath composition feso4·7h2O 110g/l, coso4·7h2O 110g/l,
Boric acid 45g/l, ascorbic acid 15g/l, ph value about 4.Temperature conditionss are room temperature.
(3) discharge nano wire
Post-depositional alumina formwork soaks in 5% (wt) naoh solution, fully removes oxide film dissolving and aluminum substrate, obtains
Purer fe-co alloy nano-wire.
Claims (1)
1. a kind of preparation method of the magnetic alloy nano wire with diameter gradient, methods described includes:
(1) template preparation:
(1) aluminium flake pretreatment: aluminium flake prior to 500 DEG C at anneal 2～4 hours, then ultrasonic 10min in acetone, then in quality
Concentration be 5% sodium hydroxide solution in soak 5min, finally ultrasonic 3min in acetone；
(2) aoxidize for the first time: pretreated aluminium flake is corroded 4～6 hours under direct current 40～60v voltage, electrolyte is dense
The oxalic acid solution of degree 0.3m～0.4m；
(3) remove once oxidation film: at 65 DEG C, aluminium flake is placed in h3po4Mass concentration 6%, cro3The mixing of mass concentration 1.5%
Process 20min～45min in liquid, remove once oxidation film；
(4) second aoxidize: aluminium flake carries out second oxidation, oxidation voltage from 25～40v in 8～12 hours uniform increments to
40～60v, electrolyte is the oxalic acid solution of concentration 0.3m～0.4m；
(5) reaming: at 35 DEG C, aluminium flake is placed in the h of mass concentration 5%3po4Reaming 20～45min in solution, obtains anodic oxidation
Aluminum alloy pattern plate；
(2) DC electrodeposition:
Using the anodic oxidation aluminium formwork of preparation as anode, with graphite flake as negative electrode, carry out under magnetic agitation in the electrolytic solution
DC electrodeposition prepares nano wire, and direct current power source voltage is 2v～4v, and temperature is room temperature；Electrolyte composition is as follows: coso4·
7h2o、niso4·7h2o、feso4·7h2Any two kinds of each 80～100g/l in o, boric acid 30～45g/l, ascorbic acid 15g/
L, solvent is water, ph 3～4；
(3) discharge nano wire:
Post-depositional anodic oxidation aluminium formwork soaks in the naoh solution of mass concentration 5%, fully goes oxide film dissolving and aluminium base
Body, obtains final product described magnetic alloy nano wire.
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| CN1529330A (en) * | 2003-09-29 | 2004-09-15 | �Ϻ���ͨ��ѧ | Iron-cobalt alloy nano linear array permanent-magnetic film material and its preparation |
| CN101016650A (en) * | 2006-12-30 | 2007-08-15 | 华东理工大学 | Method of preparing high square ratio magnetic one-dimensional nano line array |
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| CN1529330A (en) * | 2003-09-29 | 2004-09-15 | �Ϻ���ͨ��ѧ | Iron-cobalt alloy nano linear array permanent-magnetic film material and its preparation |
| CN101016650A (en) * | 2006-12-30 | 2007-08-15 | 华东理工大学 | Method of preparing high square ratio magnetic one-dimensional nano line array |
Non-Patent Citations (2)
| Title |
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| 具有梯度直径和多级枝状结构金属纳米线的制备与表征;张晓光;《中国优秀硕士学位论文全文数据库（硕士）工程科技I辑》;20070915;第B20-84页 * |
| 基于氧化铝模板法制备形状可控的金属纳米线;徐丽萍;《中国优秀硕士学位论文全文数据库（硕士）工程科技I辑》;20070915;第B20-80页 * |
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