CN100410166C - Magnetic field inducing method for growing magnetic one dimension nano line array - Google Patents
Magnetic field inducing method for growing magnetic one dimension nano line array Download PDFInfo
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- CN100410166C CN100410166C CNB2004100580855A CN200410058085A CN100410166C CN 100410166 C CN100410166 C CN 100410166C CN B2004100580855 A CNB2004100580855 A CN B2004100580855A CN 200410058085 A CN200410058085 A CN 200410058085A CN 100410166 C CN100410166 C CN 100410166C
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Abstract
The present invention relates to a magnetic field inducing process of growing a one-dimensional nanometer magnetic linear array, which belongs to the technical field of preparing one-dimensional nanometer magnetic linear arrays. The present invention comprises a process of preparing a template uniformly distributed with via holes and a direct current electrodepositing process, wherein the electrodepositing process comprises that a uniform magnetic field is arranged outside an electroplating bath; a metal electrode layer is sputtered on one side of the template; the template with an electrode is used as a cathode, and metal, or graphite or platinum to be plated is used as an anode; the cathode and the anode are arranged in the electroplating bath; salt solution of metal to be plated, which is contained in the electroplating bath, is used as electroplating solution. An external magnetic field ascends to a set value; after the external magnetic field is stabilized, the stabilization of the external magnetic field is kept after regulated to the set direction and the set angle. The set voltage is added between the cathode and the anode; a current in a control circuit is electrodeposited at one constant valuw; the electrodeposition time is set according to the length of a required nanometer line for obtaining nanometer linear arrays grown in template holes. The method can greatly increase the remanence ratio and the coercivity of the nanometer line arrays along a line shaft direction; simultaneously, the present invention can also manage the controllability of a material growing process.
Description
Technical field
The invention belongs to the preparing technical field of magnetic one-dimensional nano line array, feature relates to the improvement to template.
Technical background
The magnetic Nano linear array has potential application in discrete medium perpendicular magnetic recording, magnetic Nano device, magnetic-optic devices and microwave equipment.The method for preparing magnetic one-dimensional nano line array has a variety of, such as [P.Aranda et al, J.Magn.Magn.Mater.249,214-219] such as photoetching process, self assembly, template.Template can be divided into alumina formwork, crystal step, polymer template, biomolecule template etc. again according to the difference of template.Photoetching process can obtain the array of rule, but photoetching process speed is slow, price is high, and the array density that carves is low, and that nano wire can not be done in the array is oversize.Self-assembly method can be realized very high density, but the systematicness of array, stability, uniformity are relatively poor.Template particularly alumina formwork electrochemical deposition method but can realize the high density of nano-wire array, high even, high stability, can large-scale production.The alumina formwork electrodeposition process can be divided into direct current and alternate electrodepostion process again according to the difference of deposition current.Be two kinds of general introductions that deposition process prepares the nano-wire array process below:
1. alumina formwork direct current deposition method [H.Masuda et al, Science 1995,268,1466], [A.P.Li et al, adv.Mater.1999,11,483] may further comprise the steps:
(1) high-purity aluminium flake is deoiled, polishes after, as anode, the torpescence metal is made negative electrode, at acidic electrolysis bath, under the condition that exists as phosphoric acid, chromic acid, oxalic acid, sulfuric acid etc., keeps certain temperature, aluminium flake is carried out anodic oxidation, lasting 10 hours for the first time;
(2) aluminium flake that will have oxide layer soaks with chromic acid and phosphoric acid mixed solution, removes oxide layer; Clean, carry out anodic oxidation second time again, condition is with for the first time identical for the second time, but the time be 2 hours, after oxidation for the second time, the aluminium flake surface just forms even distribution alumina pore channel array, bottom the duct and the barrier layer that has one deck to approach, aluminium base junction.Aluminium flake after the oxidation is cleaned;
(3) remove remaining aluminium lamination after the anodic oxidation with the acid chlorization copper solution; Remove the barrier layer with phosphoric acid again, clean, dry, just obtain having the alumina formwork of equally distributed through hole;
(4) make electrode at this template one side sputter last layer metal, as negative electrode, plating metal or graphite or platinum are made anode with electroded template, and the plating metal salting liquid is that electroplate liquid carries out electro-deposition, can deposit in the hole of template and obtain nano wire, the nano wire in each hole is formed array; Control the electro-deposition parameter, just can obtain the nano-wire array of different length.
Above-mentioned steps (1)-(3) are the template preparation process, and step (4) is an electrodeposition process.
2. alumina formwork alternate electrodepostion process
Template alternating current deposition is close with template dc electrodeposition method, does not just remove aluminium lamination and barrier layer, utilizes alternating current directly to carry out electro-deposition.
From result [the D.H.Qin et.al.Appl.Phys.A 74 that has published at present, 761-765], the nano-wire array direction of principal axis along the line that exchanges prepared by electrodeposition has higher remanence ratio (0.8) and coercivity, and the array direction of principal axis remanence ratio along the line and the coercivity of the preparation of dc electrodeposition method are not high.Axial high remanence ratio and high-coercive force along the line has material impact to the nano-wire array performance.Though the alternating current deposition can obtain high remanence ratio, the alternating current deposition is because the process characteristic of self is difficult to guarantee that nanowire length is even, and controllability is relatively poor during growth.And in the electro-deposition method that now microelectronic industry need be used, dc electrodeposition is the technology of extensive use, and it is very important therefore to solve the problem that coercivity and remanence ratio are low in the dc electrodeposition process.
Summary of the invention
The objective of the invention is to prepare in the nano-wire array process in order to solve present template dc electrodeposition, magnetic such as coercivity, remanence ratio parameter is low excessively, can not satisfy the problem of practical application needs, propose the preparation method of induced by magnetic field growing high-performance magnetic one-dimensional nano line array.This method can significantly improve remanence ratio and coercivity, can take into account the controllability of material growth course simultaneously.
The preparation method of a kind of induced by magnetic field growth magnetic one-dimensional nano line array of the present invention comprises that preparation has template and two processes of dc electrodeposition of equally distributed through hole, is characterized in that described electrodeposition process may further comprise the steps:
1) in electroplating bath outer setting uniform magnetic field;
2) make electrode at template one side sputter last layer metal, as negative electrode, plating metal or graphite or platinum are made anode with electroded template, put into described coating bath, contain the plating metal salting liquid in this coating bath as electroplate liquid;
3) externally-applied magnetic field is risen to setting value, stable after, and keep stable after being adjusted to the direction, angle of setting;
4) add the voltage of setting between described yin, yang electrode, electric current carries out dc electrodeposition at a steady state value in the control circuit, sets time of deposition according to required nano wire length, obtains being grown in the nano-wire array in the pattern hole.
Described template can adopt the existing various templates that are used to prepare nano-wire array.
Described dc electrodeposition process except that add uniform magnetic field the 1st), 3) step, the 2nd), 4) identical with existing dc electrodeposition technology.
Operation principle of the present invention: up to the present the key factor that influences nano-wire array magnetic tends to think that the shape of nano wire and integrality are decisive factors.Experiment is found, compares with the nano-wire array that does not have field orientation, and field orientation does not obviously change grain orientation in the line.Therefore, what magnetic field changed in the nano wire growth course is the shape and the integrality of line, and then changes the magnetic of line.The inventor also obtains through experiment, no matter the power (even adding very little magnetic field (for example 100 oersteds)) in magnetic field, the difference of direction and position leaves standstill still rotation, growth produces big influence to nano wire in the capital, can improve nano-wire array axial coercivity along the line or remanence ratio.
Advantage of the present invention and good effect:
The present invention improves original electrochemical deposition to form, and has simple characteristics.For current production devices, can be easy to reequip.The nano-wire array that makes by this method not only length can arbitrarily be controlled, and nano wire length is even, and all has significantly to coercivity, remanence ratio than the bobbin of the nano-wire array for preparing under the no external magnetic field condition and improve.Also higher than the alternating current deposition with the coercivity and the remanence ratio of the nano-wire array of yardstick.Diminish perpendicular to nano wire direction remanence ratio simultaneously, show good direction of principal axis easy magnetization performance along the line.
Because dc electrodeposition is a lot of years of extensive use, have carried out a large amount of research work, therefore in this deposition technique, can directly utilize to be fruitful.
The universality of this method is fine.
Description of drawings
Fig. 1 is the pattern photo of the nickel nano wire of employing embodiments of the invention method preparation.
The hysteresis curve of the nickel nano-wire array that Fig. 2 records for vibrating specimen magnetometer.
The specific embodiment
The preparation method of the induced by magnetic field growth magnetic one-dimensional nano line array that the present invention proposes is described in detail as follows by embodiment:
Present embodiment prepares the method for magnetic one-dimensional nickel nano-wire array for adopting the alumina formwork dc electrodeposition, specifically may further comprise the steps:
1. be the preparation process of alumina formwork:
(1) alumina formwork adopts anodizing twice.Deoil aluminium flake after the polishing as anode, and copper be to electrode, electrolyte employing sulfuric acid, and temperature remains on 0 ℃.Inter-electrode voltage is 28V, anodic oxidation 12 hours;
(2) remove the alumina layer of generation with chromic acid and phosphoric acid mixed solution, clean, carry out the anodic oxidation second time.Condition together once;
(3) remove remaining aluminium lamination with the acid chlorization copper solution,, clean with the molten barrier layer of going of 5% phosphoric acid, oven dry, skim silver is done electrode in the one side sputter;
(4) can regulate direction, size, position, and the uniform magnetic field that can rotate in the electroplating bath outer setting, realize control the nano-wire array performance;
(5) alumina formwork of band silver electrode is a negative electrode, and the plating metal salting liquid is an electroplate liquid, and plating bath contains the 250g/L nickelous sulfate, 20g/L boric acid.The pure nickel sheet is an anode;
(6) pole orientation is gone to and the direction parallel to electrode, add magnetic field to 3000 oersted, after stablizing, the holding circuit current constant is at 30mA, and the control sedimentation time is 5 minutes, promptly obtains being grown in the nickel nano-wire array in the alumina formwork hole.
Fig. 1 is the pattern photo of two nickel nano wires, and the nanowire length that as seen makes is even, is 550nm, and diameter is about 20nm.The hysteresis curve of the nickel nano-wire array that Fig. 2 records for vibrating specimen magnetometer.By loop line as seen, the squareness ratio of array is 0.89, and coercivity is 690 oersteds.The performance parameter that exceeds alternating current deposition under the equal conditions.
The foregoing description only for illustrating method of the present invention, can not limit technical scheme of the present invention with this actual conditions.Variation, the replacement of every actual conditions to present embodiment all should be within protection scope of the present invention.
Claims (1)
1. the preparation method of an induced by magnetic field growth magnetic one-dimensional nano line array comprises preparing to have template and two processes of dc electrodeposition of even distribution through hole, it is characterized in that described electrodeposition process may further comprise the steps:
1) in electroplating bath outer setting uniform magnetic field;
2) make electrode at template one side sputter last layer metal, as negative electrode, plating metal or graphite or platinum are made anode with electroded template, put into described coating bath, contain the plating metal salting liquid in this coating bath as electroplate liquid;
3) externally-applied magnetic field is risen to setting value, stablize, and be adjusted to direction, the angle of setting;
4) add the voltage of setting between described yin, yang electrode, electric current carries out electro-deposition at a steady state value in the control circuit, sets time of deposition according to required nano wire length, obtains being grown in the nano-wire array in the pattern hole.
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| CN1896337B (en) * | 2006-06-16 | 2010-05-12 | 南京航空航天大学 | Full-automatic fluid system microreactor for electrodeposition coded nano-line |
| US7736753B2 (en) * | 2007-01-05 | 2010-06-15 | International Business Machines Corporation | Formation of nanostructures comprising compositionally modulated ferromagnetic layers by pulsed ECD |
| CN101126165B (en) * | 2007-06-15 | 2010-11-03 | 武汉理工大学 | Method for preparing one-dimensional nano material |
| CN101549406B (en) * | 2009-04-03 | 2011-01-26 | 北京航空航天大学 | A method for controllable growth of uniform nano nickel chain array induced by magnetic field |
| CN103031593B (en) * | 2012-05-31 | 2016-02-03 | 上海理工大学 | There is the preparation method of the one-dimensional magnetic nano-wire array of the axial remanence ratic of superelevation |
| CN107265414A (en) * | 2017-05-26 | 2017-10-20 | 安徽大学 | A kind of preparation method for heterogeneous nano chain of destroying first and then establish |
| CN111224091B (en) * | 2018-11-27 | 2021-08-31 | 中国科学院大连化学物理研究所 | Metal lithium wire and preparation method thereof |
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