CN106219484A - The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled - Google Patents
The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled Download PDFInfo
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Abstract
The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled, belongs to nano-particles self assemble field.First pass through fine process on substrate, form array groove；Then solution of magnetic nanoparticles is dripped in groove, after covering plastic sheet, put in culture dish；The culture dish that will be equipped with substrate is put in external magnetic field generator, is controlled the magnetocrystalline anisotropy of nano-particles self assemble array by the direction and size controlling external magnetic field；After solvent is evaporated, take out substrate.Nano-particles self assemble array of the present invention is by being dripped by solution of magnetic nanoparticles in array groove, and obtain after outside magnetic field generator evaporates solvent, by controlling size and the easy axis of the magnetocrystalline anisotropy of the size and Orientation controllable nano-particles self assemble array in the magnetic field that external magnetic field generator is formed, thus obtain the nano-particles self assemble array that magnetic anisotropy is notable and controlled.
Description
Technical field
The invention belongs to nano-particles self assemble field, be specifically related to a kind of even compact, large area, magnetic anisotropy
The preparation method of controlled three-dimensional magnetic nano-particles self assemble array.
Background technology
The self assembly of nano-particle refers to that the monomer of nanostructured is assembled into the macroscopic material of structure complexity, diverse in function
The monomer of process, such as nanostructured is assembled into orderly graphic array etc..The self-assembled material of nano-particle has excellence
Physical property, is widely used to the fields such as high density magnetic storage, sensor, flash player, field-effect transistor.Along with
The fast development of microelectric technique, proposes new requirement to magnetic device, and miniaturization, filming, array, performance are controlled etc.
Become new barrier and challenge, and the self-assembling technique of nano-particle is the key technology solving these technology barriers.
In recent years, nano-particles self assemble monofilm is the most successfully prepared and is used widely, but, due to monofilm pair
The response of external magnetic field signal is the most weak, which limits its application in many circumstances.Nano-particles self assemble multilayer film pair
The response of external magnetic field signal is relatively strong, can better adapt to the application demand under complex environment.Wen etc. (T.L.Wen, D.N.Zhang,
et al.(2015)."Magnetic nanoparticle assembly arrays prepared by hierarchical
Self-assembly on a patterned surface. " Nanoscale 7 (11): 4906-4911.) first at silicon chip
The groove of upper formation reverse pyramid, then in groove drip solution of magnetic nanoparticles, by control solution evaporation rate and
Direction, has obtained large area, inverted pyramid structure, uniform micron order magnetic nanoparticle charge transfer.The three of this array
Dimension body geometry major axis is easy magnetizing axis, although have magnetic anisotropy, but its magnetic anisotropy is inconspicuous, it is impossible to meet very
The application demand of polyelectron equipment, and the regulation and control of the size and Orientation of magnetic anisotropy can not be realized.
Summary of the invention
Present invention aims to the defect that background technology exists, propose the nanometer that a kind of magnetic anisotropy is controlled
The preparation method of particles self assemble array, to realize strengthening the magnetic anisotropy of nano-particles self assemble array, and to magnetic
Anisotropic size and Orientation carries out the purpose regulated and controled.
Technical scheme is as follows:
The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled, comprises the following steps:
Step 1: form patterned micron order array groove on substrate by photoetching and reactive ion etching；
Step 2: solution of magnetic nanoparticles is dripped in the groove that step 1 obtains, and after covering plastic sheet, put into training
Support in ware, cover sheet glass；Wherein, between plastic sheet and solution of magnetic nanoparticles and the most seamed between sheet glass and culture dish
Gap, for the evaporation of solvent, and can control direction and the speed of solvent evaporation by the position in gap and size；
Step 3: the culture dish equipped with substrate step 2 obtained is put in external magnetic field generator, described external magnetic field is produced
Generating apparatus includes permanent magnet, is positioned at the pair of parallel magnetic conductive board on permanent magnet, for supporting the non-magnetic metal of magnetic conductive board
Screw rod and non-magnetic metal nuts, described permanent magnet produces source as external magnetic field, is used for providing external magnetic field, the pair of magnetic conductive board
In base plate fit tightly with permanent magnet, can obtain being perpendicular to the magnetic field of magnetic conductive board plane, described non-magnetic metal nuts is used for
Regulate the distance between a pair magnetic conductive board, thus regulate and control the size in the magnetic field between two magnetic conductive boards；
Step 4: after solvent is evaporated, takes out substrate, polishes off the magnetic nanoparticle outside array groove,
To the magnetic nanoparticle charge transfer being deposited within array groove.
Further, described in step 1, micron order array groove is inverted pyramid, bar shaped, cylinder, annular etc..
The invention have the benefit that
1, nano-particles self assemble array of the present invention is by being dripped in array groove by solution of magnetic nanoparticles, and
Obtain after outside magnetic field generator evaporates solvent, by controlling size and the side in the magnetic field that external magnetic field generator is formed
To size and the easy axis of the magnetocrystalline anisotropy of controllable nano-particles self assemble array, thus obtain magnetic respectively to
The nano-particles self assemble array that the opposite sex is notable and controlled.
2, the magnetic anisotropy of nano-particles self assemble array of the present invention is obviously enhanced, can be by the overall magnetic to array
The test learning performance obtains weak output signal, the magnetic performance of the difficult array element detected.
3, the inventive method is simple to operate, low cost, reproducible, large-scale production can be realized, the magnetic obtained respectively to
The controlled nano-particles self assemble array of the opposite sex can be applicable to the fields such as magnetics microelectronic device, absorbing material, magnetic storage.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of the silicon chip with graphical micron order array groove；Wherein, (a), (b),
C () is respectively the scanning electron microscope diagram of the silicon substrate surface of band cylindrical grooves, strip groove, toroidal cavity；(d)、
E (), (f) are respectively the scanning electron microscope diagram in the silicon chip cross section of band cylindrical grooves, strip groove, toroidal cavity；
Fig. 2 is that the present invention forms nano-particles self assemble array and comparative example under externally-applied magnetic field under without externally-applied magnetic field
Form the process schematic of nano-particles self assemble array；Wherein, (A) is to drip on the silicon chip of band patterned cathode groove
Solution of magnetic nanoparticles, (B) is the process of lid plastic sheet and sheet glass, and (C) is the nanometer obtained after comparative example solvent volatilizees
Particles self assemble array, (D) obtains magnetic anisotropy significant nano-particles self assemble array under magnetic field in the horizontal direction,
(E) for obtain magnetic anisotropy significant nano-particles self assemble array under vertical direction magnetic field；
Fig. 3 is the scanning electron microscope of the controlled nano-particles self assemble array of magnetic anisotropy that embodiment obtains
Figure；Wherein, the magnetic anisotropy formed in (a), (b), (c) Correspondent cy linder shape groove, strip groove, toroidal cavity respectively
Controlled nano-particles self assemble array；
Fig. 4 is the VSM (vibrating specimen magnetometer) of the comparative example 2 nano-particles self assemble array without obtaining under externally-applied magnetic field
Test figure；Wherein, (a) is the schematic diagram of nano-particle magnetic moment arrangement at random, and (b) is the vibration sample of nano-particles self assemble array
Product gaussmeter (VSM) test figure, (c) is the partial enlarged drawing of vibrating specimen magnetometer (VSM) test figure；
Fig. 5 is VSM (vibrating specimen magnetometer) the test figure of the nano-particles self assemble array that embodiment 3,4 obtains；Its
In, (c) is that in the nano-particles self assemble array that embodiment 3 obtains, nano-particle magnetic moment is arranged schematic diagram along major axis, and (a) is real
Executing vibrating specimen magnetometer (VSM) the test figure of the nano-particles self assemble array that example 3 obtains, (d) is receiving of obtaining of embodiment 4
In rice grain charge transfer, nano-particle magnetic moment is arranged schematic diagram along short axle, and (b) is that the nano-particle that obtains of embodiment 4 is from group
Vibrating specimen magnetometer (VSM) the test figure of dress array.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, technical scheme is described in detail in detail.
The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled, comprises the following steps:
Step 1: use photoetching and reactive ion etching (RIE) silicon chip to be carried out microfabrication process, then at acetone
Photoresist is fallen in middle ultrasonic cleaning, then cleans in dehydrated alcohol, deionized water successively, and obtaining surface is patterned micron order battle array
The silicon chip of row groove, the distance between adjacent grooves is at least 100nm；Receive by controlling the controlled properties systems such as the length and width of groove
The shape anisotropy of rice grain charge transfer；
Step 2: use syringe to be dripped in the groove that step 1 is formed by solution of magnetic nanoparticles, to cover groove
And solution does not spills over and is advisable, cover fluorinated plastic sheet, between fluorinated plastic sheet and solution, reserve the gap evaporation for solvent；So
After the above-mentioned silicon chip being stamped plastic sheet is put in culture dish, at culture dish upper cover upper glass plate, sheet glass not exclusively covers
Culture dish, reserves the gap evaporation for solvent；After culture dish upper cover upper glass plate, the vapour concentration of solvent rises, evaporation speed
Rate slows down, and can regulate and control evaporation rate by the size controlling reserved gap；The gap that culture dish stays after covering sheet glass
The evaporation making solvent is carried out the most in one direction, and the solvent steam concentration causing this evaporation direction is on the low side, and evaporation rate is long-range
In other directions, thus evaporation direction can be controlled；
Step 3: the culture dish equipped with silicon chip step 2 obtained is put in external magnetic field generator, outside controlling
Add the direction in magnetic field and size to control the magnetocrystalline anisotropy of nano-particles self assemble array；Described external magnetic field generator bag
Include permanent magnet, be positioned at the pair of parallel magnetic conductive board on permanent magnet, for supporting the non-magnetic metal screw of magnetic conductive board and non-
Magnetic conductive metal nut, described permanent magnet produces source as external magnetic field, is used for providing external magnetic field, the base plate in the pair of magnetic conductive board
Fitting tightly with permanent magnet, can obtain being perpendicular to the magnetic field of magnetic conductive board plane, described non-magnetic metal nuts is for regulation a pair
Distance between magnetic conductive board, thus regulate and control the size in the magnetic field between two magnetic conductive boards, the placement that external magnetic field generator is different
The direction of mode controllable externally-applied magnetic field, such as Fig. 2 (D) and 2 (E), external magnetic field generator is disposed vertically available horizontal direction
Magnetic field, external magnetic field generator horizontal positioned can get the magnetic field of vertical direction；
Step 4: after solvent is evaporated, takes out substrate, polishes off the magnetic nanoparticle outside array groove,
To the magnetic nanoparticle charge transfer being deposited within array groove.
Further, described permanent magnet is ferro-aluminum boron rare-earth permanent magnet etc..
Comparative example 1
The preparation method of a kind of nano-particles self assemble array, comprises the following steps:
Step 1: by photoetching and reactive ion etching (RIE), silicon chip is carried out microfabrication, surpass the most in acetone
Sound washes photoresist, then cleans three times in dehydrated alcohol, deionized water successively, and obtaining surface is the silica-based of cylindrical grooves
Sheet, the basal diameter of described cylindrical grooves is 5 μm, a height of 2 μm, and the distance between adjacent grooves is 3 μm；
Step 2: by nanoparticle mass concentration be 10mg/mL, solvent be toluene solution of magnetic nanoparticles use micro-
Syringe is drawn 20 μ L and is dripped in the array groove that step 1 obtains, and does not spills over and is advisable covering groove and solution, covers fluorination
Plastic sheet, reserves the gap evaporation for toluene solvant between fluorinated plastic sheet and solution；Then by the above-mentioned plastic sheet of being stamped
Silicon chip is put in culture dish, and at culture dish upper cover upper glass plate, sheet glass not exclusively covers culture dish, reserves gap for first
The evaporation of benzene solvent；After toluene solvant is evaporated, takes out silicon chip, polish off the magnetic nanoparticle outside array groove,
I.e. can obtain being deposited on the magnetic nanoparticle charge transfer within array groove.
The existence of Brownian movement makes the magnetic moment direction of nano-particle be arrangement at random, there is not magnetocrystalline anisotropy, and
There is not shape anisotropy, therefore, the cylindric nano-particles self assemble that comparative example 1 obtains in cylindrical groove side all directions
Array side all directions do not possess magnetic anisotropy.
Comparative example 2
Comparative example 2 is only with the difference of comparative example 1: the groove of silicon substrate surface is bar shaped, a length of 40 μ of this strip groove
M, a width of 5 μm, a height of 2 μm, the distance between adjacent grooves is 3 μm, and remaining step is all identical with comparative example 1.
The existence of Brownian movement makes the magnetic moment direction arrangement at random of nano-particle, there is not magnetocrystalline anisotropy, receives simultaneously
Take on a different character on rice grain charge transfer unit horizontal direction size, there is shape anisotropy, thus has magnetic
Property anisotropy.
Embodiment 1
The preparation method of the nano-particles self assemble array that a kind of magnetic anisotropy is controlled, comprises the following steps:
Step 1: by photoetching and reactive ion etching (RIE), silicon chip is carried out microfabrication, surpass the most in acetone
Sound washes photoresist, then cleans three times in dehydrated alcohol, deionized water successively, and obtaining surface is the silica-based of cylindrical grooves
Sheet, the basal diameter of described cylindrical grooves is 5 μm, a height of 2 μm, and the distance between adjacent grooves is 3 μm；
Step 2: by nanoparticle mass concentration be 10mg/mL, solvent be toluene solution of magnetic nanoparticles use micro-
Syringe is drawn 20 μ L and is dripped in the array groove that step 1 obtains, and does not spills over and is advisable covering groove and solution, covers fluorination
Plastic sheet, reserves the gap evaporation for toluene solvant between fluorinated plastic sheet and solution；Then by the above-mentioned plastic sheet of being stamped
Silicon chip is put in culture dish, and at culture dish upper cover upper glass plate, sheet glass not exclusively covers culture dish, reserves gap for first
The evaporation of benzene solvent；
Step 3: the culture dish equipped with silicon chip step 2 obtained is put in the middle of external magnetic field generator, external magnetic field is produced
Distance between two magnetic conductive boards of generating apparatus is 3.5cm, and the magnetic conductive board Surface field size near permanent magnet is 0.12T, and two lead
Magnetic field size in the middle of magnetic sheet is 0.07T, and the magnetic field size away from permanent magnet one side close in the magnetic conductive board of permanent magnet is
0.05T；In cylindrical grooves, the bottom surface of cylinder is parallel to external magnetic field；
Step 4: after toluene solvant is evaporated, takes out silicon chip, polishes off the magnetic nanoparticle outside array groove,
I.e. can obtain being deposited on the magnetic nanoparticle charge transfer within array groove.
Embodiment 1 provides an external magnetic field being parallel to bottom cylindrical face in solvent evaporation process, although yet suffer from
Brownian movement, but powerful external magnetic field can make nano-particle rotate before solvent is evaporated, and after solvent is evaporated, receives
Rice grain is not rotated further by, and the magnetic moment that thus can control the nano-particle in nano-particles self assemble array points to a side
To, make the magnetocrystalline anisotropy of nano-particle be appeared, thus obtain the nano-particle that magnetic anisotropy is notable and controlled
Charge transfer.
Embodiment 2
The present embodiment is distinguished as with embodiment 1: controls the height of cylinder in cylindrical grooves in step 3 and is parallel to outer magnetic
, remaining step is the most same as in Example 1.
Embodiment 2 provides one in solvent evaporation process and is parallel to the external magnetic field that cylinder is high, although yet suffer from cloth
Bright motion, but powerful external magnetic field can make nano-particle rotate before solvent is evaporated, after solvent is evaporated, nanometer
Granule is not rotated further by, and the magnetic moment that thus can control the nano-particle in nano-particles self assemble array points to a direction,
The magnetocrystalline anisotropy making nano-particle is appeared, thus obtains the notable and controlled nano-particle of magnetic anisotropy from group
Dress array.
Embodiment 3
The present embodiment is distinguished as with embodiment 1: in step 1, the groove of silicon substrate surface is bar shaped, this strip groove
A length of 40 μm, a width of 5 μm, a height of 2 μm, the distance between adjacent grooves is 3 μm；In step 3, the length of control strip connected in star is parallel
In external magnetic field；Remaining step is the most same as in Example 1.
Embodiment 3 provides an external magnetic field being parallel to the long limit of strip groove in solvent evaporation process, although still
There is Brownian movement, but powerful external magnetic field can make nano-particle rotate before solvent is evaporated, and treats that solvent is evaporated
After, nano-particle is not rotated further by, and the magnetic moment that thus can control the nano-particle in nano-particles self assemble array points to one
Individual direction, makes the magnetocrystalline anisotropy of nano-particle be appeared；Simultaneously in nano-particles self assemble array element horizontal direction
Take on a different character size, there is shape anisotropy, thus can get the nanometer that magnetic anisotropy is notable and controlled
Grain charge transfer.
Embodiment 4
The present embodiment is distinguished as with embodiment 3: in step 3, the width of control strip connected in star is parallel to external magnetic field；Remaining step
Rapid the most same as in Example 3.
Embodiment 4 provides an external magnetic field being parallel to strip groove broadside in solvent evaporation process, although still
There is Brownian movement, but powerful external magnetic field can make nano-particle rotate before solvent is evaporated, and treats that solvent is evaporated
After, nano-particle is not rotated further by, and the magnetic moment that thus can control the nano-particle in nano-particles self assemble array points to one
Individual direction, makes the magnetocrystalline anisotropy of nano-particle be appeared；Although magnetocrystalline anisotropy is with shape anisotropy direction not
Unanimously, but the method can realize the change of magnetic anisotropy, still has bigger application prospect.
Embodiment 5
The present embodiment is distinguished as with embodiment 1: in step 1, the groove of silicon substrate surface is annular, and this annular is recessed
The overall diameter of groove be 14 μm, interior diameter be 4 μm, the degree of depth be 2 μm, the distance between adjacent grooves is 3 μm；Step 3 controls circle
The height of annular groove is parallel to external magnetic field；Remaining step is the most same as in Example 1.
Embodiment 6
The present embodiment is distinguished as with embodiment 5: the height controlling toroidal cavity in step 3 is perpendicular to external magnetic field；Remaining
Step is the most same as in Example 1.
Fig. 1 is the scanning electron microscope diagram of the silicon chip with graphical micron order array groove；Fig. 1 (a), (d) are right
The surface of the cylindrical grooves in ratio 1, embodiment 1, embodiment 2 and the scanning electron microscope diagram in cross section；Fig. 1 (b), (e)
Surface and the scanning electron microscope diagram in cross section for the strip groove in comparative example 2, embodiment 3, embodiment 4；Fig. 1 (c),
F () is surface and the scanning electron microscope diagram in cross section of toroidal cavity in embodiment 5, embodiment 6.
Fig. 2 is that the present invention forms nano-particles self assemble array and comparative example under externally-applied magnetic field under without externally-applied magnetic field
Form the process schematic of nano-particles self assemble array；Wherein, (A) is to drip on the silicon chip of band patterned cathode groove
Solution of magnetic nanoparticles, (B) is the process of lid plastic sheet and sheet glass, and (C) is the nanometer obtained after comparative example solvent volatilizees
Particles self assemble array, (D) obtains magnetic anisotropy significant nano-particles self assemble array under magnetic field in the horizontal direction,
(E) for obtain magnetic anisotropy significant nano-particles self assemble array under vertical direction magnetic field.
Fig. 3 is the scanning electron microscope of the controlled nano-particles self assemble array of magnetic anisotropy that embodiment obtains
Figure；Wherein, the magnetic anisotropy formed in (a), (b), (c) Correspondent cy linder shape groove, strip groove, toroidal cavity respectively
The scanning electron microscope diagram of controlled nano-particles self assemble array.From the figure 3, it may be seen that nano-particles self assemble array uniformly causes
Thickly fill up cylindrical grooves, strip groove, toroidal cavity, obtain the fine and close and nano-particles self assemble battle array of ordered arrangement
Row.
Fig. 4 is the VSM (vibrating specimen magnetometer) of the comparative example 2 nano-particles self assemble array without obtaining under externally-applied magnetic field
Test figure；Wherein, (a) is the schematic diagram of nano-particle magnetic moment arrangement at random, and (b) is the vibration sample of nano-particles self assemble array
Product gaussmeter (VSM) test figure, (c) is the partial enlarged drawing of vibrating specimen magnetometer (VSM) test figure；As shown in Figure 4, length and width
High different bar shaped nano-particles self assemble array has the magnetization complexity relevant to characteristic length, and characteristic length is the longest,
The most easily being magnetized to saturated, characteristic length is the shortest, is more difficult to be magnetized to saturated.
Fig. 5 is VSM (vibrating specimen magnetometer) the test figure of the nano-particles self assemble array that embodiment 3,4 obtains；Its
In, (c) is that in the nano-particles self assemble array that embodiment 3 obtains, nano-particle magnetic moment is arranged schematic diagram along major axis, and (a) is real
Executing vibrating specimen magnetometer (VSM) the test figure of the nano-particles self assemble array that example 3 obtains, (d) is receiving of obtaining of embodiment 4
In rice grain charge transfer, nano-particle magnetic moment is arranged schematic diagram along short axle, and (b) is that the nano-particle that obtains of embodiment 4 is from group
Vibrating specimen magnetometer (VSM) the test figure of dress array.From (a), (c) in Fig. 5, the nano-particle that embodiment 3 obtains is certainly
The magnetic anisotropy of assembly array is extremely obvious, and the long axis direction of bar shaped granule is magnetic anisotropy direction, for easy magnetization
Axle, compared with comparative example 2, its major axis is more easy to be magnetized to saturated.From (b), (d) in Fig. 5, the addition of external magnetic field makes shape
Anisotropic hard axis becomes the easiest axle of magnetocrystalline anisotropy, and magnetic anisotropy does not has in Fig. 5 (a) substantially, this be due to
Magnetocrystalline anisotropy and its shape anisotropy that magnetic moment ordered arrangement produces produce the result competed.
To sum up, the inventive method can prepare arrangement in order, dense uniform, controlled shape, magnetic anisotropy notable
And controlled, reproducible, with low cost and that can be mass-produced magnetic nanoparticle charge transfer.
Claims (2)
1. a preparation method for the nano-particles self assemble array that magnetic anisotropy is controlled, comprises the following steps:
Step 1: form patterned micron order array groove on substrate by photoetching and reactive ion etching；
Step 2: solution of magnetic nanoparticles is dripped in the groove that step 1 obtains, and after covering plastic sheet, put into culture dish
In, cover sheet glass；Wherein, between plastic sheet and solution of magnetic nanoparticles and between sheet glass and culture dish, all there is gap, use
Evaporation in solvent；
Step 3: the culture dish equipped with substrate step 2 obtained is put in external magnetic field generator, described external magnetic field produces dress
Put and include permanent magnet, be positioned at the pair of parallel magnetic conductive board on permanent magnet, for supporting the non-magnetic metal screw of magnetic conductive board
With non-magnetic metal nuts, described permanent magnet produces source as external magnetic field, is used for providing external magnetic field, described non-magnetic metal nuts
For regulating the distance between a pair magnetic conductive board, thus regulate and control the size in the magnetic field between two magnetic conductive boards；
Step 4: after solvent is evaporated, takes out substrate, polishes off the magnetic nanoparticle outside array groove, i.e. can be sunk
Amass the magnetic nanoparticle charge transfer within array groove.
The preparation method of the nano-particles self assemble array that magnetic anisotropy the most according to claim 1 is controlled, it is special
Levying and be, described in step 1, micron order array groove is inverted pyramid, bar shaped, cylinder or annular.
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| CN110600620A (en) * | 2018-06-12 | 2019-12-20 | Tcl集团股份有限公司 | Preparation method of quantum dot film |
| CN111333027A (en) * | 2020-03-16 | 2020-06-26 | 苏州微之纳智能科技有限公司 | Efficient injection molding machine for self-assembly of nano particles |
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