CN104183630A - A substrate with magnetic nanowires being arranged on the surface and a preparation method of the substrate - Google Patents

A substrate with magnetic nanowires being arranged on the surface and a preparation method of the substrate Download PDF

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Publication number
CN104183630A
CN104183630A CN201410235930.5A CN201410235930A CN104183630A CN 104183630 A CN104183630 A CN 104183630A CN 201410235930 A CN201410235930 A CN 201410235930A CN 104183630 A CN104183630 A CN 104183630A
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substrate
magnetic nanometer
nano wire
magnetic
ethanolic solution
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相文峰
贺卓
董佳丽
岳义
赵昆
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Priority to CN201410235930.5A priority Critical patent/CN104183630A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
    • 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

Abstract

The invention relates to a substrate with magnetic nanowires being arranged on the surface and a preparation method of the substrate. The surface of the substrate is provided with the orderly-arranged magnetic nanowires. The preparation method of the substrate comprises the steps of dispersing the magnetic nanowires into a dispersing solution, and then, using a magnetic field to enable the magnetic nanowires to be orderly-arranged and deposited on the surface of the substrate. By utilizing the magnetic properties of the magnetic nanowire material itself and under the action of a magnetic field, directional arrangement can be realized, and large-area, multiple-angle, multiple-mode, multiple-layer controllable nano material arrangement can be realized; the operation is simple; and the large-area preparation and arrangement of the materials help to promote the development of large-scale and integrated production of semiconductor devices.

Description

A kind of surface alignment substrate of nano wire and preparation method thereof that is magnetic
Technical field
The present invention relates to a kind of surface alignment substrate of nano wire and preparation method thereof that is magnetic, belong to semi-conducting material preparing technical field.
Background technology
In prior art, the preparation method of nano material (the namely method of growth, arranging nano-wire) adopts chemical method mostly, mainly comprises sol-gel process, hydro-thermal and solvent heat synthetic method, chemical precipitation method, template etc.But the sol-gel process prices of raw and semifnished materials are expensive, and between gel particle, agglutinating property is poor, nano wire prepared by hydro-thermal and chemical precipitation method is dispersed in the middle of solution, can not form oldered array, the equipment that template adopts is simple, easy operating, normal temperature and pressure can carry out, production cost is low, be easy to realize suitability for industrialized production, especially use anodised aluminium (Anodic Aluminum Oxide, AAO) template, its aperture is controlled, and in the same size, cylinder hole is perpendicular to face, independent between Kong Yukong, hole is orderly columnar arrangement, its synthetic material is easy to collect, although template can realize perpendicular to the nano wire of face and arranging, but the nano wire of ordered arrangement can not independently exist, after template is washed off, the nano wire of prepared ordered arrangement will become and distribute in a jumble, this has limited the further application of template synthesis nano material.
And above-mentioned method can not realize arranging nano-wire in large area, can not realize the various ways of nano wire, the compound arrangement of many levels, be not suitable with the development need of semiconductor device scale, integrated production.
Summary of the invention
In view of the defect that above-mentioned prior art exists, the object of the invention is to propose a kind of surface alignment substrate of nano wire and preparation method thereof that is magnetic, the surface of this substrate has the magnetic nanometer of ordered arrangement in large area.
The present invention also aims to provide the preparation method of the substrate that above-mentioned surface alignment is magnetic nano wire.
For achieving the above object, the invention provides the be magnetic substrate of nano wire of a kind of surface alignment, wherein, the surface of this substrate has the magnetic nanometer of ordered arrangement.
According to specific embodiment of the invention scheme, preferably, the magnetic nanometer of above-mentioned substrate surface can have following several different arrangement mode:
The whole surface of substrate has one deck according to the magnetic nanometer of same direction ordered arrangement, can be called one dimension and arrange; Or,
The surface of substrate has two-layer above magnetic nanometer, and the magnetic nanometer of every one deck is according to same direction ordered arrangement, and the magnetic nanometer of different layers is arranged according to different directions, can be called multi-angle hierarchal arrangement; Or,
The surface of substrate has the magnetic nanometer of hypermatrix row ordered arrangement, can be called piecemeal arrayed, surface at this substrate, the magnetic nanometer of all same block same layers is same direction and arranges, same block can have the magnetic nanometer of one or more layers multi-angle, between different blocks, by white space, separate, the kind of the nano wire that the orientation of the magnetic nanometer of different blocks can be different, arrange also can be different.
According to specific embodiment of the invention scheme, preferably, described magnetic nanometer is Ni base nano-wire, and more preferably, described Ni base nano-wire comprises Ni nano wire, Ni/ (metal or metal oxide)/Ni composite nano-line or NiO nano wire; Wherein, described metal comprises one or both in the materials such as Ni, Au, Cu, and described metal oxide comprises NiO, ZnO, TiO 2deng one or both in material, described metal or metal oxide also comprise other similar material, and what be not limited to list is several.
Above-mentioned Ni/ (metal or metal oxide)/Ni composite nano-line is the nano wire of minutes three sections, interlude is metal or metal oxide, two ends are Ni nano wires, and the present invention utilizes the magnetic of two ends Ni cap (Ni nano wire) to carry out arranging nano-wire; Above-mentioned NiO nano wire is the NiO nano wire of whole, is the Ni nano wire oxidation having arranged is formed.
According to specific embodiment of the invention scheme, preferably, in every one deck, the distribution density of direction the above magnetic nanometer vertical with nano wire is 1-5 root/μ m.
According to specific embodiment of the invention scheme, the substrate adopting can be the conventional substrate in this area, such as silicon chip, polymethyl methacrylate sheet etc., and above-mentioned silicon chip can be to be also coated with SiO 2the single of film throws silicon chip, but is not limited to this.
The present invention also provides the preparation method of the substrate that above-mentioned surface alignment is magnetic nano wire, and it comprises magnetic nanometer is scattered in dispersion soln, then adopts magnetic field to make magnetic nanometer form ordered arrangement, and is deposited on the step of substrate surface.According to the difference of needed arrangement mode, can take different preparation processes.
According to specific embodiment of the invention scheme, preferably, said method comprises the following steps:
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtains whole surface and has one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement;
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtain whole surface and there is one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement, then this substrate is put into the ethanolic solution that is dispersed with magnetic nanometer again, then the uniform magnetic field that this ethanolic solution is placed in to different magnetic field direction repeats to heat standing or room temperature placement (so that the magnetic nanometer of the later layer depositing and the magnetic nanometer of front one deck have different directions), ethanolic solution volatilization, the step of clean substrate surfaces, until obtain the substrate that surface has two-layer above magnetic nanometer,
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtain whole surface and there is one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement, then on the surface of this substrate, coat photoresist, utilize mask technique, the photoresist of substrate surface partly exposed, make substrate surface photoresist piecemeal, expose the nano wire of part substrate surface; The nano wire ultrasonic cleaning exposing is clean; Clean the photoresist of removing substrate surface remainder, obtain the substrate that surface has the magnetic nanometer of hypermatrix row ordered arrangement;
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, in substrate surface integral body, coat photoresist, utilize mask technique that the photoresist of substrate surface is partly exposed, the subregion of exposure substrate, expose the nano wire in this region, ultrasonic processing cleans up the nano wire exposing;
Substrate after this cleaning is put into again to the ethanolic solution of the magnetic nanometer that is dispersed with identical or different kind, the uniform magnetic field that then this ethanolic solution is placed in to different magnetic field direction repeats to heat standing or room temperature placement;
After ethanolic solution volatilization is dry, take out substrate, clean substrate surfaces; This substrate is put into acetone soln and remove the residual photoresist of substrate surface unexposed portion, obtain surface and there is piecemeal array, the identical or substrate of the nano wire of identical type magnetic nanometer, different orientations not.
Above-mentioned surface has piecemeal array, substrate identical or the not nano wire of identical type magnetic nanometer, different orientations refers to: the nano wire blockette of substrate surface is arranged, the nano wire of different blocks can be the nano wire of commaterial, also can be the nano wire of different materials, the orientation of the nano wire in the different blocks direction that can be the same or different, can angledly arrange to each other.
According to specific embodiment of the invention scheme, preferably, above-mentioned preparation method is further comprising the steps of:
In template, apposition growth obtains magnetic nanometer;
The be magnetic template of nano wire of apposition growth is put into NaOH solution and soaked and dissolve, discharge and obtain magnetic nanometer, preferably, the concentration of NaOH solution is 1mol/L-5mol/L, and soaking the time of dissolving is 5min-20min;
Magnetic nanometer is held and cleaned with magnet.
In above-mentioned preparation method, preferred, the concentration of dissolving the NaOH solution that discharges magnetic nanometer is 3mol/L, and soaking the time of dissolving is 10min.
In above-mentioned preparation method, the magnetic nanometer adopting can be that conventional method prepares, and preferably adopts electrochemical deposition, sol-gel or the electrophoretic deposition magnetic nanometer that growth obtains in the anodic oxidation aluminium formwork of metal-plated membrane overleaf; More preferably, the aperture in the hole on the anodic oxidation aluminium formwork adopting is 200nm, and length is 50 μ m.Adopting the template in the hole of this aperture and the degree of depth can prepare diameter is that 200nm, length are the magnetic nanometer of 5 μ m-50 μ m.
The back side metal-coated membrane of above-mentioned anodic oxidation aluminium formwork is made electrode, and this metal film can be the metal film of gold-plated, silver-colored, copper etc.
According to specific embodiment of the invention scheme, preferably, when adopting electrochemical deposition to prepare magnetic nanometer, it can comprise the following steps:
To containing NiSO 46H 2o and H 3bO 3reaction solution in add dilute sulfuric acid, pH value is adjusted to 3, in described reaction solution, NiSO 46H 2o and H 3bO 3molar concentration be 0.1mol/L-1mol/L;
Template is placed in to reaction solution, with 4mA/cm 2-10mA/cm 2continuous current carry out the reaction of 2min, then current density is reduced by half, with 2mA/cm 2-5mA/cm 2continuous current carry out the reaction of 30min-3h, obtain magnetic nanometer (what obtain is Ni nano wire) herein.
According to specific embodiment of the invention scheme, more preferably, when adopting electrochemical deposition to prepare magnetic nanometer, it can comprise the following steps:
To containing NiSO 46H 2o and H 3bO 3reaction solution in add dilute sulfuric acid, pH value is adjusted to 3, in described reaction solution, NiSO 46H 2o and H 3bO 3solution is respectively 0.4mol/L and 0.6mol/L;
Template is placed in to reaction solution, with 6mA/cm 2continuous current carry out the reaction of 2min, then with 3mA/cm 2continuous current carry out the reaction of 30min-3h, obtain magnetic nanometer (what obtain is Ni nano wire) herein.
In above-mentioned electrochemical deposition method, as needed, prepare " Ni/ metal/Ni nano wire " or " Ni/ metal oxide/Ni nano wire ", need first electroplated Ni nano wire, after having electroplated Ni nano wire part, electrolyte is changed to corresponding metal ion solution, use again electrochemical deposition method plated metal ion nano wire, finally change again electrolyte electroplated Ni nano wire; Or after having electroplated Ni nano wire part, electrolyte is changed to the charged particle solution of corresponding metal oxide, then uses electrophoretic deposition depositing metal oxide nano wire, finally change again electrolyte electroplated Ni nano wire; Here with the Ni nano wire sealing cap at two ends, realize the control of externally-applied magnetic field.As need are prepared NiO nano wire,, after preparation Ni nano wire, by Ni nano wire high-temperature oxydation, be NiO nano wire.
According to specific embodiment of the invention scheme, preferably, in above-mentioned electrochemical deposition, can also be included in before the dissolving of NaOH solution, the be magnetic template of nano wire of apposition growth is soaked with chloroazotic acid, remove the step of metal film, the time of immersion is 5min-10min.
In above-mentioned preparation method, the step that magnetic nanometer is for example scattered in, in dispersion soln (ethanolic solution) can realize by ultrasonic dispersion, the time of ultrasonic dispersion is preferably 1 minute, can use deionized water and ethanol to clean respectively separately when magnetic nanometer is cleaned two to three times.
In above-mentioned preparation method, preferred, the temperature heating in magnetic field when standing is controlled as the boiling temperature lower than ethanol.
Technical scheme provided by the present invention is utilized self magnetic of nano-material, and under magnetic fields, realization aligns, and can realize the controlled nano material of large-area, multiple angles, various ways, multiple level and arrange, and simple to operate.On-chip magnetic Nano material provided by the present invention; mainly the one-dimensional magnetic nano material relevant to Ni; utilize the ferromagnetism of Ni material; can realize preparation and the arrangement of Ni associated materials; as Ni/ (metal or metal oxide)/Ni composite nano-line, NiO nano wire etc.; the realization of the ordered arrangement of the large area preparation of these materials and various ways, many levels, will greatly promote the development of semiconductor device scale, integrated production.
Accompanying drawing explanation
Fig. 1 is the SEM figure that on the Si substrate of embodiment 1, large area is arranged Ni base nano-wire;
Fig. 2 a is that on the Si substrate of embodiment 5, multi-angle multilayer is arranged Ni base nano-wire SEM figure;
Fig. 2 b is the partial enlarged drawing of Fig. 2 a;
Fig. 3 is the schematic diagram that on the Si substrate of embodiment 1,2,3,4, large area is arranged Ni base nano-wire;
Fig. 4 is the schematic diagram that on the Si substrate of embodiment 5, multi-angle multilayer is arranged Ni base nano-wire;
Fig. 5 is the schematic diagram that on the Si substrate of embodiment 6, piecemeal is arranged Ni base nano-wire;
Fig. 6 is the schematic diagram that on the Si substrate of embodiment 7, variety classes Ni and nano wire are arranged in left and right.
Embodiment
Below by specific embodiment, method of the present invention is described, so that technical solution of the present invention is easier to understand, grasp, but the present invention is not limited thereto.Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the surperficial Si substrate with the Ni nano wire of large-area ordered arrangement (is coated with SiO 2layer), this preparation method comprises the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2the H of O and 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 6mA/cm 2constant current carry out the reaction of 2min, then keep 3mA/cm 2the reaction of 3h is carried out in constant current, obtains the long nano wire of 50 μ m;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
The Ni nano wire cleaning up is immersed in ethanolic solution (analyze pure, absolute ethyl alcohol), and ultrasonic dispersion 1min, puts into Si substrate the ethanolic solution that is dispersed with Ni nano wire, and adds uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, take out substrate, by deionized water, ethanol clean surface, obtain the Si substrate that surface has the Ni nano wire of large-area ordered arrangement, its SEM figure as shown in Figure 1, arranges schematic diagram as shown in Figure 3, on the Si substrate of gained, Ni nano wire is single direction, individual layer, large-area ordered arranging.
Embodiment 2
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the surperficial Si substrate with the NiO nano wire of large-area ordered arrangement (is coated with SiO 2layer), this preparation method comprises the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2the H of O and 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 6mA/cm 2constant current carry out the reaction of 2min, keep 3mA/cm 2the reaction of 3h is carried out in constant current, obtains the long nano wire of 50 μ m;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
The Ni nano wire cleaning up is immersed in ethanolic solution, and ultrasonic dispersion 1min, puts into Si substrate the ethanolic solution that is dispersed with Ni nano wire, and adds uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, takes out substrate, by deionized water, ethanol clean surface, obtains the substrate that surface has the Ni nano wire that large area is arranged in parallel;
Ni nano wire high-temperature oxydation surface to the substrate of the Ni nano wire that large area is arranged in parallel is NiO nano wire, the optimal conditions of high-temperature oxydation Ni nano wire is: in tube furnace, keep oxygen atmosphere high-temperature oxydation, keep as required 400-800 ℃, oxidation 2-8h, obtain the Si substrate that surface has the NiO nano wire of large area arrangement, it arranges schematic diagram as shown in Figure 3, is single direction, large-area ordered arranging.
Embodiment 3
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the surperficial Si substrate with Ni/ metal/Ni composite nano-line of large-area ordered arrangement (is coated with SiO 2layer), this preparation method comprises the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2o and concentration are the H of 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 3mA/cm 2continuous current carry out the reaction of 1h, obtain the long Ni nano wire of 5 μ m;
Electrolyte is changed to Cu solion (CuSO 4dilution heat of sulfuric acid), with dilute sulfuric acid, regulate pH value to 3, electrochemical deposition method obtains Cu nano wire, again electrolyte is replaced by the electrolyte of preparation Ni nano wire, with electrochemical deposition method deposition Ni nano wire, forms tri-sections of nano wires of Ni/Cu/Ni of 50 μ m;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni/Cu/Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
The Ni/Cu/Ni nano wire cleaning up is immersed in ethanolic solution, and ultrasonic dispersion 1min, puts into Si substrate the ethanolic solution that is dispersed with Ni/Cu/Ni nano wire, and adds uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, take out substrate, by deionized water, ethanol clean surface, obtain the Si substrate that surface has Ni/ metal/Ni composite nano-line of large-area ordered arrangement, it arranges schematic diagram as shown in Figure 3, is single direction, large-area ordered arranging.
Embodiment 4
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the surperficial Si substrate with Ni/ metal oxide/Ni composite nano-line of large-area ordered arrangement (is coated with SiO 2layer), this preparation method comprises the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2o and concentration are the H of 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 6mA/cm 2continuous current carry out the reaction of 2min, then keep 3mA/cm 2the reaction of 1h is carried out in constant current, obtains the long nickel nano wire of 5 μ m;
Electrolyte is changed to TiO 2colloidal sol, electrophoretic deposition obtains TiO 2nano wire, is replaced by electrolyte the electrolyte of preparing Ni nano wire again, with electrochemical deposition method deposition Ni nano wire, forms the Ni/TiO of 50 μ m 2tri-sections of nano wires of/Ni;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni/TiO 2/ Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
By the Ni/TiO cleaning up 2/ Ni nano wire is immersed in ethanolic solution, and ultrasonic dispersion 1min, puts into Si substrate to be dispersed with Ni/TiO 2in the ethanolic solution of/Ni nano wire, and add uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, take out substrate, by deionized water, ethanol clean surface, obtain the Si substrate that surface has Ni/ metal oxide/Ni composite nano-line of large-area ordered arrangement, it arranges schematic diagram as shown in Figure 3, is single direction, large-area ordered arranging.
Embodiment 5
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the surperficial Si substrate with the Ni nano wire of multi-angle layering ordered arrangement (is coated with SiO 2layer), comprise the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2the H of O and 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 6mA/cm 2constant current carry out the reaction of 2min, then keep 3mA/cm 2the reaction of 3h is carried out in constant current, obtains the long nano wire of 50 μ m;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
The Ni nano wire cleaning up is immersed in ethanolic solution, and ultrasonic dispersion 1min, puts into Si substrate the ethanolic solution that is dispersed with Ni nano wire, and adds uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, takes out substrate, by deionized water, ethanol clean surface, obtains the substrate that surperficial parallel is shown large-area Ni nano wire;
The substrate that arranges nano wire is put into the ethanolic solution immersed with nano wire again, and add uniform magnetic field in the beaker both sides of containing solution, this adds magnetic field and adds for the first time magnetic field angled, and the present embodiment is got 90 °;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, take out substrate, by deionized water, ethanol clean surface, so operation, obtains the Si substrate that surface has the Ni nano wire of multi-angle layering ordered arrangement, and its SEM figure is as shown in Fig. 2 a, 2b, it arranges schematic diagram as shown in Figure 4, is bilayer, vertical direction, large-area ordered arranging.
Embodiment 6
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the Si substrate of surperficial piecemeal arrangement Ni nano wire (is coated with SiO 2layer), comprise the steps:
With electrochemical deposition method direct growth Ni nano wire in anodic oxidation aluminium formwork: before plating, first make electrode at the back side of template plating layer of gold film;
To the reactant liquor (NiSO that is 0.4mol/L containing concentration 46H 2the H of O and 0.6mol/L 3bO 3) in add dilution heat of sulfuric acid, pH value is adjusted to 3;
Template is placed in to reactant liquor, with 6mA/cm 2constant current carry out the reaction of 2min, then keep 3mA/cm 2the reaction of 3h is carried out in constant current, obtains the long nano wire of 50 μ m;
There is the template of nano-material to put into the chloroazotic acid of now joining apposition growth, soak 5-10min, dissolve the golden film at the template back side;
Go the template of golden film to put into the NaOH solution that concentration is 3mol/L dissolving, dissolve and discharge Ni nano wire, and clean nano wire with deionized water, ethanolic solution;
The Ni nano wire cleaning up is immersed in ethanolic solution, and ultrasonic dispersion 1min, puts into Si substrate the ethanolic solution that is dispersed with Ni nano wire, and adds uniform magnetic field in the beaker both sides of containing solution;
The standing collating unit that adds magnetic field, after ethanolic solution is evaporated completely, takes out substrate, by deionized water, ethanol clean surface, obtains being parallel to the large-area Ni nano wire of substrate surface;
Technology is divided into polylith by the large-area Ni nano wire of arranging on substrate with photoresist, forms the piecemeal arranged array of Ni nano wire, and concrete steps are: 1) in the substrate surface integral body that is arranged with large-area Ni nano wire, coat photoresist; 2) utilize photoresist and mask technique, the photoresist of substrate surface is partly exposed, make the photoresist piecemeal of substrate surface, thereby expose the nano wire of part substrate surface; 3) nano wire exposing is cleaned up by ultrasonic method; 4) use the photoresist of acetone soln clean substrate surfaces remainder;
By substrate put into deionized water, ethanolic solution cleans, and obtains the Si substrate that surperficial piecemeal is arranged Ni nano wire, it arranges schematic diagram as shown in Figure 5.
Embodiment 7
The present embodiment provides a kind of surface alignment to have substrate of nano wire and preparation method thereof, and this substrate is that the Si substrate of surperficial left and right two parts arrangement variety classes nano wire (is coated with SiO 2layer), as Ni nano wire is arranged on the left side, Ni/Cu/Ni nano wire is arranged on the right, and the nano wire orientation of two kinds of left and right is perpendicular.
The Ni nano wire preparing in embodiment 1 is dissolved in ethanolic solution, adds magnetic field alignment on substrate, after solution evaporation is dry, take out substrate, clean up;
In substrate surface integral body, coat photoresist, utilize mask plate that the photoresist of substrate surface is partly exposed, exposure substrate right half part, exposes the Ni nano wire of right half part, and ultrasonic processing cleans up the nano wire exposing;
The Ni/Cu/Ni composite nano-line preparing in embodiment 2 is dissolved in ethanolic solution, add the magnetic field vertical with arranging Ni nano wire direction, Ni/Cu/Ni composite nano-line is arranged in to above-mentioned left-half to be had on the substrate of photoresist covering, after solution evaporation is dry, take out substrate, clean up;
Substrate is put into acetone soln and remove the residual photoresist of substrate surface left-half, can obtain the left side is Ni nano wire, and the right is the substrate of Ni/Cu/Ni nano wire, and two kinds of left and right nano wire is arranged perpendicular, and it arranges schematic diagram as Fig. 6.

Claims (10)

1. the surface alignment substrate for nano wire that is magnetic, wherein, the surface of this substrate has the magnetic nanometer of ordered arrangement.
2. substrate according to claim 1, wherein, the whole surface of this substrate has one deck according to the magnetic nanometer of same direction ordered arrangement; Or,
The surface of this substrate has two-layer and above magnetic nanometer, and the magnetic nanometer of every one deck is according to same direction ordered arrangement, and the magnetic nanometer of different layers is arranged according to different directions; Or,
The surface of this substrate has the magnetic nanometer of hypermatrix row ordered arrangement.
3. substrate according to claim 1, wherein, described magnetic nanometer is Ni base nano-wire, preferred, described Ni base nano-wire comprises Ni nano wire, Ni/ (metal or metal oxide)/Ni composite nano-line or NiO nano wire; Wherein, described metal comprises one or both in Ni, Au, Cu, and described metal oxide comprises NiO, ZnO, TiO 2deng in one or both, be not limited to listed different materials.
4. substrate according to claim 2, wherein, in every one deck, the distribution density of direction the above magnetic nanometer vertical with nano wire is 1-5 root/μ m.
5. the preparation method of substrate of nano wire that is magnetic of the surface alignment described in a claim 1-4 any one, it comprises magnetic nanometer is scattered in dispersion soln, then adopt magnetic field to make magnetic nanometer form ordered arrangement, and be deposited on the step of substrate surface.
6. preparation method according to claim 5, wherein, the method comprises the following steps:
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtains whole surface and has one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement;
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtain whole surface and there is one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement, then this substrate is put into the ethanolic solution that is dispersed with magnetic nanometer again, then the uniform magnetic field that this ethanolic solution is placed in to different magnetic field direction repeats to heat standing or room temperature is placed, ethanolic solution volatilizees, the step of clean substrate surfaces, until obtain the substrate that surface has two-layer above magnetic nanometer;
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, obtain whole surface and there is one deck according to the substrate of the magnetic nanometer of same direction ordered arrangement, then on the surface of this substrate, coat photoresist, utilize mask technique, the photoresist of substrate surface partly exposed, make substrate surface photoresist piecemeal, expose the nano wire of part substrate surface; The nano wire ultrasonic cleaning exposing is clean; Clean the photoresist of removing substrate surface remainder, obtain the substrate that surface has the magnetic nanometer of hypermatrix row ordered arrangement;
Or,
Magnetic nanometer is scattered in ethanolic solution, substrate is put into the ethanolic solution that this is dispersed with magnetic nanometer, then this ethanolic solution is placed in to uniform magnetic field and heats standing or room temperature placement;
After ethanolic solution is evaporated completely, take out substrate, clean substrate surfaces, in substrate surface integral body, coat photoresist, utilize mask technique that the photoresist of substrate surface is partly exposed, the subregion of exposure substrate, expose the nano wire in this region, ultrasonic processing cleans up the nano wire exposing;
Substrate after this cleaning is put into again to the ethanolic solution of the magnetic nanometer that is dispersed with identical or different kind, the uniform magnetic field that then this ethanolic solution is placed in to different magnetic field direction repeats to heat standing or room temperature placement;
After ethanolic solution volatilization is dry, take out substrate, clean substrate surfaces; This substrate is put into acetone soln and remove the residual photoresist of substrate surface unexposed portion, obtain surface and there is piecemeal array, the identical or substrate of the nano wire of identical type magnetic nanometer, different orientations not.
7. according to the preparation method described in claim 5 or 6, wherein, this preparation method is further comprising the steps of:
In template, apposition growth obtains magnetic nanometer;
The be magnetic template of nano wire of apposition growth is put into NaOH solution and soaked and dissolve, discharge and obtain magnetic nanometer, preferably, the concentration of described NaOH solution is 1mol/L-5mol/L, and soaking the time of dissolving is 5min-20min;
Magnetic nanometer is held and cleaned with magnet.
8. according to the preparation method described in claim 5-7 any one, wherein, described magnetic nanometer is to adopt electrochemical deposition, sol-gel or the electrophoretic deposition magnetic nanometer that growth obtains in the anodic oxidation aluminium formwork of metal-plated membrane overleaf; Preferably, the aperture in the hole on described anodic oxidation aluminium formwork is 200nm, and length is 50 μ m.
9. preparation method according to claim 8, wherein, described electrochemical deposition comprises the following steps:
To containing NiSO 46H 2o and H 3bO 3reaction solution in add dilute sulfuric acid, pH value is adjusted to 3, in described reaction solution, NiSO 46H 2o and H 3bO 3molar concentration be 0.1mol/L-1mol/L;
Template is placed in to reaction solution, with 4mA/cm 2-10mA/cm 2continuous current carry out the reaction of 2min, then current density is reduced by half, with 2mA/cm 2-5mA/cm 2continuous current carry out the reaction of 30min-3h, obtain magnetic nanometer.
10. preparation method according to claim 7, wherein, before the method is also included in and dissolves with NaOH solution, soaks with chloroazotic acid the be magnetic template of nano wire of apposition growth, removes the step of metal film, and the time of immersion is 5min-10min.
CN201410235930.5A 2014-05-29 2014-05-29 A substrate with magnetic nanowires being arranged on the surface and a preparation method of the substrate Pending CN104183630A (en)

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