CN103985502A - Method for preparing nanometer spin valve array - Google Patents

Method for preparing nanometer spin valve array Download PDF

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CN103985502A
CN103985502A CN201410238579.5A CN201410238579A CN103985502A CN 103985502 A CN103985502 A CN 103985502A CN 201410238579 A CN201410238579 A CN 201410238579A CN 103985502 A CN103985502 A CN 103985502A
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electrochemical deposition
layer
groove
spin valve
thickness
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CN103985502B (en
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王会新
李明
王允建
刘振深
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Henan University of Technology
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Henan University of Technology
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Abstract

The invention relates to a method for preparing a nanometer spin valve array. The problems that the temperature in the etching process is high, the use range is narrow, equipment is expensive, the limitation is large, the etching speed is low, cost is high, and scale production can not be achieved are effectively solved. The method comprises the following steps that a porous anodized aluminum template is selected, the porous anodized aluminum template is preprocessed, different plating baths are selected for use, and each layer of nanometer spin valves are formed through electrochemical deposition. According to the tiny spin valves with the multilayer structure, the lateral dimension of each tiny spin valve is only tens of nanometers, the tiny spin valves are densely arranged in sequence according to a regular hexagon, the areal density is as high as 10<11>/cm<2>, and therefore the spin valve array with the lateral dimension at the nanometer order is formed; the process is conducted at the normal temperature, interlayer metal diffusion caused by high temperature is avoided, the performance of the spin valves can not be affected, the requirements for equipment and the work environment are simple, operation is simple, the speed is high, cost is low and industrial popularization can be achieved easily.

Description

A kind of preparation method of nanometer Spin Valve array
Technical field
The present invention relates to a kind of preparation method of nanometer Spin Valve array.
Background technology
Giant magnetoresistance (GMR) effect is subject to extensive and long-term attention in the world, and the important application prospect of this and it is undivided.Although the magnetoresistive ratio of Spin Valve is smaller, it is still with advantages such as the consistent rotations of low saturation field, highfield sensitivity and magnetic moment, and rate has been introduced into practical stage.In short several years, just develop a series of highly sensitive GMR devices.Hard disc of computer magnetic reading head is manufactured in the most noticeable application of GMR effect exactly, and it has realized higher than 30GB/in commercialization hard disc of computer 2packing density, exceed magnetooptic recording, be the important breakthrough of computer electronics industry, this technology progressively becomes the main flow of microminiaturization, super-high density magnetic recording high-quality magnetic head development.Adopt the transducer of spin valve structure have highly sensitive under downfield, temperature coefficient is little, good stability feature.Obtain a wide range of applications at aspects such as detecting electric current, position, displacement, the anglec of rotation.Use the Magnetic Sensor of Spin Valve GMR element, detection sensitivity is than being used the device high of magneto-resistor (MR) element to several magnitudes, and more easily integrated, package dimension is less, and reliability is higher.It not only can replace former MR transducer, can also make sensor array, realizes intellectuality, is used for explaining traffick, and the feature of hidden defects in aircraft wing, construction safety device or pipe-line system is followed the tracks of the anomaly in earth magnetic field etc.Somebody proposes can be used as the sensing element of antibody and biological sample inspection, and range of application significantly expands than MR transducer.The sensor array of Spin Valve GMR element can also be applied even more extensively in household electrical appliances, auto industry and automatic control technology, as being applied to, automobile is unmanned, in charge, distinguishing device for counterfeit paper money and global position system.Along with the develop rapidly of electronics, microminiaturization and the high-density integrated degree of electronic component are more and more higher.The size of each construction unit is more and more less.
In recent years, some researcher applying electronic bundles or ion beam etching technology have been prepared the Spin Valve array of lateral dimension in sub-micrometer scale.There is following shortcoming in this preparation method: 1 can produce very high temperature in etching process, cause the diffusion of different metal between each layer of Spin Valve, the each layer thickness of Spin Valve is very thin, generally several between tens nanometers, this diffusion couple brings very large infringement to the performance of Spin Valve.Etching size is less, and temperature can be higher, and this infringement is larger, even makes it lose the performance of Spin Valve.And this method can not prepare littlely, lateral dimension is at the Spin Valve array of nanometer scale.2 device therefor costlinesses, requirement condition harshness, limitation is large, high vacuum, super clean, etching speed is slow, and cost is high, is not suitable for large-scale production.
Summary of the invention
For above-mentioned situation, for overcoming prior art defect, the present invention's object is just to provide a kind of preparation method of nanometer Spin Valve array, can effectively solve in etching temperature high, the scope of application is narrow, apparatus expensive, limitation is large, and etching speed is slow, high and the problem that can not large-scale production of cost.
The technical scheme that the present invention solves is to comprise the steps:
One, choose porous anodic aluminium oxide (AAM or AAO) template, hole two ends communicate, aperture 30-100nm, pitch of holes 90～120nm, surface density 10 11/ cm 2, (existing product, the AAM template or the AAO template that provide as Hefei Pu Yuan nanosecond science and technology Co., Ltd), easily, price is also cheaper in this template preparation;
Two, the preliminary treatment of porous anodic alumina template:
(1) at a surface of porous anodic alumina template (being one end of hole) sputter Au(gold) and Ta(tantalum) film, work electrode (negative electrode) during as electrochemical deposition (electrochemical deposition claims again electro-deposition), method is, porous anodic alumina template is placed in to magnetron sputtering, the Au film that is 400～800nm at surface sputtering last layer thickness of porous anodic alumina template, then the thick Ta film of sputter 10～20 nm again on Au film, work electrode (negative electrode) during as electrochemical deposition, and the Seed Layer of follow-up electro-deposition inverse ferric magnetosphere (being antiferromagnetic pinning layer) and ferromagnetic layer (being ferromagnetic nailed layer and ferromagnetic free layer), to make antiferromagnet FeMn(ferrimanganic) alloy is at face-centered cubic (111) crystal face preferential growth, thereby make the pinning effect of antiferromagnet stronger,
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed on to each immersion 10 minutes in acetone, absolute ethyl alcohol, deionized water, Ultrasonic Cleaning 5 minutes, is to clean and discharge the bubble in duct; Described acetone is pure for analyzing;
Three, adopt different electroplating bath each layer of electrochemical deposition nanometer Spin Valve respectively, overcome the shortcoming that uses the various metal codepositions that bring of single groove electrochemical deposition layers of material, method is, get groove 1, groove 2, groove 3 and groove 4, totally four electroplating baths, each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2(ruthenium titanium) electrode; (3) work electrode (negative electrode): the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 30-100nm, and five layers are successively, (1), antiferromagnetic pinning layer (AFL), formed thickness 8～15nm by FeMn alloy, wherein, in alloy, Mn accounts for 47%～53%; (2), ferromagnetic nailed layer (PFL), by NiFe(ferronickel) alloy or Co(cobalt) form, thickness 5～10nm, wherein, in alloy, Ni accounts for 75%～85%; (3), nonmagnetic metal separator, by Cu(copper) form, thickness 2～4nm; (4), ferromagnetic free layer (FFL), formed by NiFe alloy or Co, thickness 3～8nm, wherein, in alloy, Ni accounts for 75%～85%; (5), protective layer, formed thickness 10～15nm by Cu;
In described groove 1, have by FeSO 47H 2o(ferrous sulfate heptahydrate), 0.3～0.4 mol, MnSO 4(manganese sulfate) 0.4～0.5mol, (NH 4) 2sO 4(ammonium sulfate) 0.2～0.3 mol, C 6h 5na 3o 72H 2o (natrium citricum) 0.07～0.15 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution (claiming again deposit fluid);
Described groove 2 is interior by FeSO 47H 2o 0.02～0.1 mol, H 3bO 3(boric acid) 0.4～0.8 mol, NiSO 46H 2o(nickelous sulfate or six hydration nickel sulfate) 0.5～1mol, C 6h 5na 3o 72H 2o (natrium citricum) 0.1～0.2 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
In described groove 3, have by CoSO 47H 2o(cobalt sulfate) 0.42mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
In described groove 4, have by CuSO 45H 2o (cupric sulfate pentahydrate) 0.01～0.02mol and H 3bO 30.4～0.6 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; In the time that ferromagnetic nailed layer is made up of NiFe alloy, carry out electrochemical deposition with groove 2; In the time that ferromagnetic free layer is made up of NiFe alloy, use groove 2 to carry out electrochemical deposition; In the time that ferromagnetic nailed layer is made up of Co, carry out electrochemical deposition with groove 3; In the time that ferromagnetic free layer is made up of Co, use groove 3 to carry out electrochemical deposition; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, add the even external magnetic field of 500 Oe-1000 Oe, the uniaxial anisotropy of ferromagnetic nailed layer, ferromagnetic free layer and the pinning direction of arranging antiferromagnetic pinning layer are used for inducting;
(2) be there is to card in LAI200-PC104 random waveform and insert computer PCI slot, use the LAI200-PC104 random waveform on computer that the control software control pulse electrical signal generator blocking occurs, according to the different layers of electrochemical deposition nanometer Spin Valve, export different current potentials, method is, the antiferromagnetic pinning layer of electrochemical deposition, current potential is elected-1.0～-1.3V as; The ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer, current potential is elected-1.0～-1.2V as; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential～-0.4V; The LAI200_PC104:1Ch50Msps14Bits random waveform that described LAI200-PC104 random waveform occurs to block for Chengdu Jia Yi development in science and technology Co., Ltd is blocked;
(3) according to the speed of the electrochemical deposition of every layer of different materials of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of every layer of different materials electrochemical deposition, controls the thickness that is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture;
(4) temperature of electrochemical deposition is 18-25 DEG C;
(6) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, for preventing deposit fluid cross pollution, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(7) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer, and electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array;
The rate calculations method of every layer of different materials electrochemical deposition of described nanometer Spin Valve is: by (6) condition of above-mentioned steps one to four, the different materials of the every one deck to nanometer Spin Valve carries out electrochemical deposition successively respectively, in the time that electric current sharply increases suddenly, indicate that the hole on pretreated porous anodic alumina template is filled, record now this layer material electrochemical deposition time used, the speed of the electrochemical deposition of thickness (not comprising the thickness of Au film and Ta film) this layer material electrochemical deposition of ÷ of the alumina formwork of pretreated porous anodic alumina template time=this layer material used under above-mentioned electrochemical deposition condition itself,
The rate calculations method of every layer of different materials electrochemical deposition of described nanometer Spin Valve, the ferromagnetic free layer being made up of NiFe alloy taking electrochemical deposition is example: the Au film in surface sputtering a layer thickness of the thick porous anodic alumina template of 10 μ m as 500nm, then sputter 10 nm Ta films again on Au film, be successively placed in acetone, absolute ethyl alcohol, deionized water and soak 10 minutes, Ultrasonic Cleaning 5 minutes, be placed in groove 2 interior as work electrode (negative electrode), reference electrode be housed: saturated calomel electrode and auxiliary electrode: Ru0 in groove 2 2/ Ti0 2electrode, in groove 2, have by FeSO 47H 2o 0.07 mol, H 3bO 30.52 mol, NiSO 46H 2o 0.68mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter, and to make PH value be 3.5 electroplating solution, add the even external magnetic field of 700 Oe perpendicular to this template, there is the control software control pulse electrical signal generator of card by the LAI200-PC104 random waveform on computer, elect as-1.2V of current potential, temperature is 20 DEG C, in the time that electric current sharply increases suddenly, the hole that records this template is deposited time 9765s completely used, the electrochemical deposition speed that draws the NiFe alloy of ferromagnetic free layer under this condition is 10 μ m ÷ 9765s ≈ 1.024nm/s, analogize with the method, calculate the speed of the different materials electrochemical deposition of every one deck of nanometer Spin Valve,
Described FeSO 47H 2o, MnSO 4, (NH 4) 2sO 4, NiSO 46H 2o, CoSO 47H 2o, CuSO 45H 2o and C 6h 5na 3o 72H 2it is pure that O is analysis; Described H 3bO 3content be 99.999%.
The present invention adopts porous anodic alumina template, in its nano aperture, by the method for above-mentioned electrochemical deposition, preparation has the small Spin Valve of sandwich construction, only tens nanometer of each little Spin Valve lateral dimension, arranges by regular Hexagonal Close-packed order, and surface density is up to 10 11/ cm 2the Spin Valve array of lateral dimension in nanometer scale, be that current prior art can not be prepared, and carry out at normal temperatures, avoided Yin Gaowen and the diffusion of the interlayer metal that causes, can not affect Spin Valve performance, equipment and operational environment are required simply, and easy to operate, speed is fast, with low cost, easily realize industrialization promotion.
Brief description of the drawings
Fig. 1 is the flat scanning electron microscope picture of nanometer Spin Valve array of the present invention.
Fig. 2 is the side scanning electron microscope diagram sheet of nanometer Spin Valve array of the present invention.
Fig. 3 is the X ray diffracting spectrum of nanometer Spin Valve array of the present invention.
Fig. 4 is the magnetic hysteresis loop figure under nanometer Spin Valve array room temperature of the present invention.
Fig. 5 is the magnetic resistance loop line figure under nanometer Spin Valve array room temperature of the present invention.
Embodiment
Below in conjunction with actual conditions, the specific embodiment of the present invention is elaborated.
Embodiment 1
One, choose porous anodic alumina template, aperture 40nm, pitch of holes 100nm, surface density 10 11/ cm 2;
Two, the preliminary treatment of porous anodic alumina template:
(1) porous anodic alumina template is placed in magnetron sputtering, the Au film that is 500nm at surface sputtering last layer thickness of porous anodic alumina template, the then thick Ta film of sputter 15 nm again on Au film;
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed in acetone, absolute ethyl alcohol, deionized water and is soaked 10 minutes, Ultrasonic Cleaning 5 minutes;
Three, with groove 1, groove 2 and 4 three electroplating bath electrochemical deposition nanometer Spin Valves of groove, method is that each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2electrode; (3) work electrode (negative electrode): the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 40nm, and successively, (1), antiferromagnetic pinning layer, be made up of FeMn alloy five layers, thickness 10nm, and wherein, in alloy, Mn accounts for 51%; (2), ferromagnetic nailed layer, formed by NiFe alloy, thickness 8nm, wherein, in alloy, Ni accounts for 82%; (3), nonmagnetic metal separator, formed thickness 3nm by Cu; (4), ferromagnetic free layer, formed by NiFe alloy, thickness 5nm, wherein, in alloy, Ni accounts for 82%; (5), protective layer, formed thickness 15nm by Cu;
In groove 1, have by FeSO 47H 2o 0.36 mol, MnSO 40.47mol, (NH 4) 2sO 40.22 mol and C 6h 5na 3o 72H 2o 0.09 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In groove 2, have by FeSO 47H 2o 0.07mol, H 3bO 30.52mol, NiSO 46H 2o 0.68mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter of electroplating solution of making PH value 3.5;
In groove 4, have by CuSO 45H 2o 0.07mol and H 3bO 30.47 mol adds water to 1 liter of electroplating solution of making PH value 3.5;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; Groove 2: be used for respectively the ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, adds the even external magnetic field of 700 Oe;
(2) use the LAI200-PC104 random waveform on computer that the control software control pulse electrical signal generator blocking, the antiferromagnetic pinning layer of electrochemical deposition, elect as-1.3V of current potential occur; The ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer, all elect as-1.2V of current potential; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential;
(3) according to the speed of the every layer material electrochemical deposition of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of electro-deposition, control the thickness that every layer material is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture, antiferromagnetic pinning layer electrodepositing speed 1.472nm/s, sedimentation time 6.78s, deposit thickness 10nm; Ferromagnetic nailed layer, deposition rate is 1.024nm/s, sedimentation time 7.81s, deposit thickness 8nm; Nonmagnetic metal separator, deposition rate 0.957nm/s, sedimentation time 3.13s, deposit thickness 3nm; Ferromagnetic free layer, deposition rate 1.024nm/s, sedimentation time 4.88s, deposit thickness 5nm; Protective layer Cu deposition rate 0.957nm/s, sedimentation time 15.67s, deposit thickness 15nm;
(4) temperature of electrochemical deposition is 20 DEG C;
(5) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(6) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer, electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array.
Embodiment 2
One, select porous anodic alumina template, aperture 80nm, pitch of holes 95nm, surface density is 10 11/ cm 2;
Two, the preliminary treatment of porous anodic alumina template:
(1) porous anodic alumina template is placed in magnetron sputtering, the Au film that is 800nm at surface sputtering last layer thickness of porous anodic alumina template, the then thick Ta film of sputter 20 nm again on Au film;
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed in acetone, absolute ethyl alcohol, deionized water and is soaked 10 minutes, Ultrasonic Cleaning 5 minutes;
Three, with groove 1, groove 2, groove 3 and groove 4 totally four electroplating bath electrochemical deposition nanometer Spin Valves, method is that each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2electrode; (3) work electrode (negative electrode): the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 80nm, and successively, (1), antiferromagnetic pinning layer, be made up of FeMn alloy five layers, thickness 11nm, and wherein, in alloy, Mn accounts for 49%; (2), ferromagnetic nailed layer, formed by NiFe alloy, thickness 7nm, wherein, in alloy, Ni accounts for 78%; (3), nonmagnetic metal separator, formed thickness 3nm by Cu; (4), ferromagnetic free layer, formed thickness 4nm by Co; (5), protective layer, formed thickness 15nm by Cu;
In described groove 1, there is FeSO 47H 2o 0.38 mol, MnSO 40.42mol, (NH 4) 2sO 40.22 mol and C 6h 5na 3o 72H 2o 0.09 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
Described groove 2 is interior by FeSO 47H 2o 0.08 mol, H 3bO 30.52 mol, NiSO 46H 2o 0.63mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In described groove 3, have by CoSO 47H 2o 0.42mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In described groove 4, have by CuSO 45H 2o 0.07mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; Groove 2: be used for the ferromagnetic nailed layer of electrochemical deposition; Groove 3: be used for electrochemical deposition ferromagnetic free layer; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, adds the even external magnetic field of 1000 Oe;
(2) there is the control software control pulse electrical signal generator blocking, the antiferromagnetic pinning layer of electrochemical deposition, elect as-1.3V of current potential by the LAI200-PC104 random waveform on computer; The ferromagnetic nailed layer of electrochemical deposition, elect as-1.2V of current potential; Electrochemical deposition ferromagnetic free layer, elect as-1.2V of current potential; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential;
(3) according to the speed of the every layer material electrochemical deposition of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of electro-deposition, control the thickness that every layer material is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture, antiferromagnetic pinning layer electrodepositing speed 1.473nm/s, sedimentation time 7.47s, deposit thickness 11nm; Ferromagnetic nailed layer deposition rate is 1.025nm/s, sedimentation time 6.84s, deposit thickness 7nm; Nonmagnetic metal separator deposition rate 0.957nm/s, sedimentation time 3.13s, deposit thickness 3nm; Ferromagnetic free layer deposition rate 1.124nm/s, sedimentation time 3.56s, deposit thickness 4nm; Protective layer Cu deposition rate 0.957nm/s, sedimentation time 15.67s, deposit thickness 15nm;
(4) temperature of electrochemical deposition is 25 DEG C;
(5) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(6) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array.
First the present invention has proposed to prepare the method for nanometer Spin Valve array with porous alumina formwork (claiming again porous anodic alumina template) combined with electrochemical deposition technique, utilize Woelm Alumina for template, in its nano aperture, under normal temperature, normal pressure, by the method for electrochemical deposition, preparation nanometer Spin Valve array, solve an existing difficult problem of preparing inevitable generation high temperature damage Spin Valve performance in Spin Valve array process by electron beam or ion beam etching technology, the each interlayer of Spin Valve that utilizes the present invention to prepare does not have the diffusion of metal, and Spin Valve performance is better.Under room temperature, the coercive force of free layer (being ferromagnetic free layer) is 9～30 Oe, giant magnetoresistance effect, and GMR value reaches 4.2%～6.5%, and Spin Valve lateral dimension is less, only has tens nanometers, and surface density reaches 10 11/ cm 2and arrangement high-sequential, this method also has equipment and operational environment requirement simple, easy to operate, speed is fast, with low cost, easily realizes the advantages such as industrialization promotion, these performances and parameter all meet the requirement such as sensor array of preparation high density magnetic storage, Spin Valve GMR element above, for the preparation of related device is laid a good foundation.
The nanometer Spin Valve array that the present invention prepares show that through experiment pattern, magnetic and Giant Magnetoresistance are specific as follows: dissolve away after the porous anodic alumina template of nanometer Spin Valve outside the flat scanning electron microscope picture (as shown in Figure 1) of the nanometer Spin Valve array obtaining and the side scanning electron microscope diagram sheet (as shown in Figure 2) of nanometer Spin Valve array with 5%NaOH solution; From Fig. 1 and Fig. 2, can see nanometer Spin Valve arrayed high-sequential, form the Hexagonal Close-packed pattern of a width rule; Fig. 3 nanometer Spin Valve array X radiographic diffracting spectrum, NiFe and FeMn grow by face-centered cubic (111) crystal face as can be seen from Figure 3; Fig. 4 and Fig. 5 are respectively magnetic hysteresis loop figure and the giant magnetoresistance curve chart under nanometer Spin Valve array room temperature, as can be seen from Figure 3, the loop line center of free layer, near null field place, illustrates that the coupling between nailed layer (being ferromagnetic nailed layer) and free layer is very little.The magnetic hysteresis loop center of nailed layer is obviously offset towards the direction of checkout area.Exchange bias field is about 340 Oe.Exchange bias field is greater than coercive force, has very wide step in the positive direction in magnetic field, and the magnetic hysteresis loop of nailed layer and free layer separately.Under condition at checkout area by the positive field sweep of negative sense, in the time that the magnetic moment of free layer just overturns completely, the magnetic moment of nailed layer does not almost overturn, and the complete antiparallel degree that two-layer magnetic moment can reach is higher.In Fig. 4, can find out, its rectangular degree is fine, and the sensitivity in magnetic field is very large.In giant magnetoresistance loop line of the present invention, GMR value reaches 4.2%～6.5%, the coercive force of its free layer is 9～30 Oe, shows the weak ferromagnetic coupling that is coupled as between pinning layer and free layer, and these all meet the requirement of the device such as sensor array of preparing Spin Valve GMR element.
The present invention is through repeatedly experiment repeatedly, all show that GMR value is 4.2%～6.5%, the coercive force of free layer is 9～30 Oe, between pinning layer and free layer, be coupled as weak ferromagnetic coupling, stable performance, all meet the requirement of the device such as sensor array of preparing Spin Valve GMR element, have huge economic and social benefit.

Claims (3)

1. a preparation method for nanometer Spin Valve array, is characterized in that, concrete steps are:
One, choose porous anodic alumina template, hole two ends communicate, aperture 30-100nm, pitch of holes 90～120nm, surface density 10 11/ cm 2, easily, price is also cheaper in this template preparation;
Two, the preliminary treatment of porous anodic alumina template:
(1) at surface sputtering Au and the Ta film of porous anodic alumina template, work electrode during as electrochemical deposition, method is, porous anodic alumina template is placed in to magnetron sputtering, the Au film that is 400～800nm at surface sputtering last layer thickness of porous anodic alumina template, then the thick Ta film of sputter 10～20 nm again on Au film, work electrode during as electrochemical deposition, and the Seed Layer of follow-up electro-deposition inverse ferric magnetosphere and ferromagnetic layer, to make antiferromagnet FeMn alloy at face-centered cubic crystal face preferential growth, thereby make the pinning effect of antiferromagnet stronger,
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed on to each immersion 10 minutes in acetone, absolute ethyl alcohol, deionized water, Ultrasonic Cleaning 5 minutes, is to clean and discharge the bubble in duct; Described acetone is pure for analyzing;
Three, adopt different electroplating bath each layer of electrochemical deposition nanometer Spin Valve respectively, overcome the shortcoming that uses the various metal codepositions that bring of single groove electrochemical deposition layers of material, method is, get groove 1, groove 2, groove 3 and groove 4, totally four electroplating baths, each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2electrode; (3) work electrode: the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 30-100nm, and successively, (1), antiferromagnetic pinning layer, be made up of FeMn alloy five layers, thickness 8～15nm, and wherein, in alloy, Mn accounts for 47%～53%; (2), ferromagnetic nailed layer (PFL), formed by NiFe alloy or Co, thickness 5～10nm, wherein, in alloy, Ni accounts for 75%～85%; (3), nonmagnetic metal separator, formed thickness 2～4nm by Cu; (4), ferromagnetic free layer, formed by NiFe alloy or Co, thickness 3～8nm, wherein, in alloy, Ni accounts for 75%～85%; (5), protective layer, formed thickness 10～15nm by Cu;
In described groove 1, have by FeSO 47H 2o, 0.3～0.4 mol, MnSO 40.4～0.5mol, (NH 4) 2sO 40.2～0.3 mol, C 6h 5na 3o 72H 2o 0.07～0.15 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
Described groove 2 is interior by FeSO 47H 2o 0.02～0.1 mol, H 3bO 30.4～0.8 mol, NiSO 46H 2o 0.5～1mol, C 6h 5na 3o 72H 2o 0.1～0.2 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
In described groove 3, have by CoSO 47H 2o 0.42mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
In described groove 4, have by CuSO 45H 2o 0.01～0.02mol and H 3bO 30.4～0.6 mol adds water to 1 liter, and to make pH value be 3.0～4.0 electroplating solution;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; In the time that ferromagnetic nailed layer is made up of NiFe alloy, carry out electrochemical deposition with groove 2; In the time that ferromagnetic free layer is made up of NiFe alloy, use groove 2 to carry out electrochemical deposition; In the time that ferromagnetic nailed layer is made up of Co, carry out electrochemical deposition with groove 3; In the time that ferromagnetic free layer is made up of Co, use groove 3 to carry out electrochemical deposition; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, add the even external magnetic field of 500 Oe-1000 Oe, the uniaxial anisotropy of ferromagnetic nailed layer, ferromagnetic free layer and the pinning direction of arranging antiferromagnetic pinning layer are used for inducting;
(2) be there is to card in LAI200-PC104 random waveform and insert computer PCI slot, use the LAI200-PC104 random waveform on computer that the control software control pulse electrical signal generator blocking occurs, according to the different layers of electrochemical deposition nanometer Spin Valve, export different current potentials, method is, the antiferromagnetic pinning layer of electrochemical deposition, current potential is elected-1.0～-1.3V as; The ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer, current potential is elected-1.0～-1.2V as; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential～-0.4V; The LAI200_PC104:1Ch50Msps14Bits random waveform that described LAI200-PC104 random waveform occurs to block for Chengdu Jia Yi development in science and technology Co., Ltd is blocked;
(3) according to the speed of the electrochemical deposition of every layer of different materials of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of every layer of different materials electrochemical deposition, controls the thickness that is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture;
(4) temperature of electrochemical deposition is 18-25 DEG C;
(6) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, for preventing deposit fluid cross pollution, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(7) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer, and electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array;
The rate calculations method of every layer of different materials electrochemical deposition of described nanometer Spin Valve is: by (6) condition of above-mentioned steps one to four, the different materials of the every one deck to nanometer Spin Valve carries out electrochemical deposition successively respectively, in the time that electric current sharply increases suddenly, indicate that the hole on pretreated porous anodic alumina template is filled, record now this layer material electrochemical deposition time used, the speed of the electrochemical deposition of this layer material electrochemical deposition of the thickness ÷ of the alumina formwork of pretreated porous anodic alumina template time=this layer material used under above-mentioned electrochemical deposition condition itself,
The rate calculations method of every layer of different materials electrochemical deposition of described nanometer Spin Valve, the ferromagnetic free layer being made up of NiFe alloy taking electrochemical deposition is example: the Au film in surface sputtering a layer thickness of the thick porous anodic alumina template of 10 μ m as 500nm, then sputter 10 nm Ta films again on Au film, be successively placed in acetone, absolute ethyl alcohol, deionized water and soak 10 minutes, Ultrasonic Cleaning 5 minutes, be placed in groove 2 interior as work electrode, reference electrode is housed in groove 2: saturated calomel electrode and auxiliary electrode: Ru0 2/ Ti0 2electrode, in groove 2, have by FeSO 47H 2o 0.07 mol, H 3bO 30.52 mol, NiSO 46H 2o 0.68mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter, and to make PH value be 3.5 electroplating solution, add the even external magnetic field of 700 Oe perpendicular to this template, there is the control software control pulse electrical signal generator of card by the LAI200-PC104 random waveform on computer, elect as-1.2V of current potential, temperature is 20 DEG C, in the time that electric current sharply increases suddenly, the hole that records this template is deposited time 9765s completely used, the electrochemical deposition speed that draws the NiFe alloy of ferromagnetic free layer under this condition is 10 μ m ÷ 9765s ≈ 1.024nm/s, analogize with the method, calculate the speed of the different materials electrochemical deposition of every one deck of nanometer Spin Valve,
Described FeSO 47H 2o, MnSO 4, (NH 4) 2sO 4, NiSO 46H 2o, CoSO 47H 2o, CuSO 45H 2o and C 6h 5na 3o 72H 2it is pure that O is analysis; Described H 3bO 3content be 99.999%.
2. the preparation method of nanometer Spin Valve array according to claim 1, is characterized in that, concrete steps are:
One, choose porous anodic alumina template, aperture 40nm, pitch of holes 100nm, surface density 10 11/ cm 2;
Two, the preliminary treatment of porous anodic alumina template:
(1) porous anodic alumina template is placed in magnetron sputtering, the Au film that is 500nm at surface sputtering last layer thickness of porous anodic alumina template, the then thick Ta film of sputter 15 nm again on Au film;
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed in acetone, absolute ethyl alcohol, deionized water and is soaked 10 minutes, Ultrasonic Cleaning 5 minutes;
Three, with groove 1, groove 2 and 4 three electroplating bath electrochemical deposition nanometer Spin Valves of groove, method is that each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2electrode; (3) work electrode: the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 40nm, and successively, (1), antiferromagnetic pinning layer, be made up of FeMn alloy five layers, thickness 10nm, and wherein, in alloy, Mn accounts for 51%; (2), ferromagnetic nailed layer, formed by NiFe alloy, thickness 8nm, wherein, in alloy, Ni accounts for 82%; (3), nonmagnetic metal separator, formed thickness 3nm by Cu; (4), ferromagnetic free layer, formed by NiFe alloy, thickness 5nm, wherein, in alloy, Ni accounts for 82%; (5), protective layer, formed thickness 15nm by Cu;
In groove 1, have by FeSO 47H 2o 0.36 mol, MnSO 40.47mol, (NH 4) 2sO 40.22 mol and C 6h 5na 3o 72H 2o 0.09 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In groove 2, have by FeSO 47H 2o 0.07mol, H 3bO 30.52mol, NiSO 46H 2o 0.68mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter of electroplating solution of making PH value 3.5;
In groove 4, have by CuSO 45H 2o 0.07mol and H 3bO 30.47 mol adds water to 1 liter of electroplating solution of making PH value 3.5;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; Groove 2: be used for respectively the ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, adds the even external magnetic field of 700 Oe;
(2) use the LAI200-PC104 random waveform on computer that the control software control pulse electrical signal generator blocking, the antiferromagnetic pinning layer of electrochemical deposition, elect as-1.3V of current potential occur; The ferromagnetic nailed layer of electrochemical deposition and ferromagnetic free layer, all elect as-1.2V of current potential; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential;
(3) according to the speed of the every layer material electrochemical deposition of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of electro-deposition, control the thickness that every layer material is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture, antiferromagnetic pinning layer electrodepositing speed 1.472nm/s, sedimentation time 6.78s, deposit thickness 10nm; Ferromagnetic nailed layer, deposition rate is 1.024nm/s, sedimentation time 7.81s, deposit thickness 8nm; Nonmagnetic metal separator, deposition rate 0.957nm/s, sedimentation time 3.13s, deposit thickness 3nm; Ferromagnetic free layer, deposition rate 1.024nm/s, sedimentation time 4.88s, deposit thickness 5nm; Protective layer Cu deposition rate 0.957nm/s, sedimentation time 15.67s, deposit thickness 15nm;
(4) temperature of electrochemical deposition is 20 DEG C;
(5) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(6) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer, electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array.
3. the preparation method of nanometer Spin Valve array according to claim 1, is characterized in that, concrete steps are:
One, select porous anodic alumina template, aperture 80nm, pitch of holes 95nm, surface density is 10 11/ cm 2;
Two, the preliminary treatment of porous anodic alumina template:
(1) porous anodic alumina template is placed in magnetron sputtering, the Au film that is 800nm at surface sputtering last layer thickness of porous anodic alumina template, the then thick Ta film of sputter 20 nm again on Au film;
(2) porous anodic alumina template of above-mentioned sputter Au film and Ta film is successively placed in acetone, absolute ethyl alcohol, deionized water and is soaked 10 minutes, Ultrasonic Cleaning 5 minutes;
Three, with groove 1, groove 2, groove 3 and groove 4 totally four electroplating bath electrochemical deposition nanometer Spin Valves, method is that each electroplating bath is equipped with three electrodes: (1) reference electrode: saturated calomel electrode; (2) auxiliary electrode: Ru0 2/ Ti0 2electrode; (3) work electrode: the pretreated porous anodic alumina template making in (2) in above-mentioned steps two; Nanometer Spin Valve is made up of five bottom-up being stacked of layer, and diameter is 80nm, and successively, (1), antiferromagnetic pinning layer, be made up of FeMn alloy five layers, thickness 11nm, and wherein, in alloy, Mn accounts for 49%; (2), ferromagnetic nailed layer, formed by NiFe alloy, thickness 7nm, wherein, in alloy, Ni accounts for 78%; (3), nonmagnetic metal separator, formed thickness 3nm by Cu; (4), ferromagnetic free layer, formed thickness 4nm by Co; (5), protective layer, formed thickness 15nm by Cu;
In described groove 1, there is FeSO 47H 2o 0.38 mol, MnSO 40.42mol, (NH 4) 2sO 40.22 mol and C 6h 5na 3o 72H 2o 0.09 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
Described groove 2 is interior by FeSO 47H 2o 0.08 mol, H 3bO 30.52 mol, NiSO 46H 2o 0.63mol and C 6h 5na 3o 72H 2o 0.17mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In described groove 3, have by CoSO 47H 2o 0.42mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
In described groove 4, have by CuSO 45H 2o 0.07mol and H 3bO 30.47 mol adds water to 1 liter, and to make pH value be 3.5 electroplating solution;
Groove 1: be used for the antiferromagnetic pinning layer of electrochemical deposition; Groove 2: be used for the ferromagnetic nailed layer of electrochemical deposition; Groove 3: be used for electrochemical deposition ferromagnetic free layer; Groove 4: be used for respectively electrochemical deposition nonmagnetic metal separator and protective layer;
Four, electrochemical deposition:
(1) in the time of electrochemical deposition, by the pretreated porous anodic alumina template making in (2) in above-mentioned steps two, wherein there is the surface of film down, place upward on another surface, perpendicular to the direction of this template, adds the even external magnetic field of 1000 Oe;
(2) there is the control software control pulse electrical signal generator blocking, the antiferromagnetic pinning layer of electrochemical deposition, elect as-1.3V of current potential by the LAI200-PC104 random waveform on computer; The ferromagnetic nailed layer of electrochemical deposition, elect as-1.2V of current potential; Electrochemical deposition ferromagnetic free layer, elect as-1.2V of current potential; Electrochemical deposition nonmagnetic metal separator and protective layer, elect as-0.3V of current potential;
(3) according to the speed of the every layer material electrochemical deposition of nanometer Spin Valve, the control software that occurs to block by the LAI200-PC104 random waveform on computer is controlled respectively the time of electro-deposition, control the thickness that every layer material is deposited on every one deck of nanometer Spin Valve in pretreated porous anodic alumina template inside aperture, antiferromagnetic pinning layer electrodepositing speed 1.473nm/s, sedimentation time 7.47s, deposit thickness 11nm; Ferromagnetic nailed layer deposition rate is 1.025nm/s, sedimentation time 6.84s, deposit thickness 7nm; Nonmagnetic metal separator deposition rate 0.957nm/s, sedimentation time 3.13s, deposit thickness 3nm; Ferromagnetic free layer deposition rate 1.124nm/s, sedimentation time 3.56s, deposit thickness 4nm; Protective layer Cu deposition rate 0.957nm/s, sedimentation time 15.67s, deposit thickness 15nm;
(4) temperature of electrochemical deposition is 25 DEG C;
(5) one deck of the complete nanometer Spin Valve of every electrochemical deposition, changes groove, while changing groove, the template of electrochemical deposition is cleaned 5 minutes in deionized water for ultrasonic;
(6) electrochemical deposition carries out in the following order: antiferromagnetic pinning layer, ferromagnetic nailed layer, nonmagnetic metal separator, ferromagnetic free layer, protective layer electrochemical deposition under these conditions successively, obtains nanometer Spin Valve array.
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