CN109023527A - Anisotropy MAGNETIC GARNET FILMS GROWN and preparation method thereof outside a kind of face - Google Patents
Anisotropy MAGNETIC GARNET FILMS GROWN and preparation method thereof outside a kind of face Download PDFInfo
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- CN109023527A CN109023527A CN201811000028.XA CN201811000028A CN109023527A CN 109023527 A CN109023527 A CN 109023527A CN 201811000028 A CN201811000028 A CN 201811000028A CN 109023527 A CN109023527 A CN 109023527A
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- 239000002223 garnet Substances 0.000 title claims abstract description 54
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 59
- 239000010408 film Substances 0.000 claims abstract description 51
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 34
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 28
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910003443 lutetium oxide Inorganic materials 0.000 claims abstract description 17
- 239000010409 thin film Substances 0.000 claims abstract description 9
- 239000004615 ingredient Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 239000007791 liquid phase Substances 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 238000002955 isolation Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000012776 electronic material Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000002242 deionisation method Methods 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 4
- 229960002415 trichloroethylene Drugs 0.000 description 4
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004943 liquid phase epitaxy Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 241000219991 Lythraceae Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- CMMUKUYEPRGBFB-UHFFFAOYSA-L dichromic acid Chemical compound O[Cr](=O)(=O)O[Cr](O)(=O)=O CMMUKUYEPRGBFB-UHFFFAOYSA-L 0.000 description 1
- 230000005350 ferromagnetic resonance Effects 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Thin Magnetic Films (AREA)
Abstract
Anisotropy MAGNETIC GARNET FILMS GROWN and preparation method thereof, belongs to technical field of electronic materials outside a kind of face.The ingredient of the monocrystal thin films is Y3‑(a+b+c)BiaLubCacFe5‑dGedO12, wherein 0 < a <, 0.5,0 < b <, 1.0,0 < c <, 1.0,0 < d < 1.0, and c=d.The present invention is with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3As raw material, the method for placing raw material using layering has obtained anisotropy MAGNETIC GARNET FILMS GROWN outside the face that thickness minimum can reach 170nm on Gd-Ga garnet substrate；And non-linear relation is presented in the growth rate of obtained film and growth temperature, and anisotropy outside face is presented, and can be applied in spin logical device.
Description
Technical field
The invention belongs to technical field of electronic materials, and in particular to anisotropy pomegranate outside the face of one kind of multiple element dopings
Stone film and its liquid phase epitaxy preparation method.
Background technique
With the continuous reduction of size of electronic devices, the influence of quantum effect is more obvious, and research workers are by electronics
Another attribute --- spin is introduced into electronic device, realize the accuracy controlling to electron transport using spin, or
The carrier directly stored and transmitted using electron spin as information can not only be such that device size further decreases, moreover it is possible into one
Step reduces power consumption.Yttrium iron garnet (YIG) is used as a kind of non-magnetic insulators, low resistance, ferromagnetic resonance line width be small, spin transport away from
From it is long the advantages that make its spin logical device in be widely used.
Presently found various spin effects, such as logic gates, inverse logic gates, spin Hall magnetic resistance, anti-
Normal logic gates etc. are all related with the magnetospheric direction of magnetization, therefore the anisotropy of garnet will affect film and exist
Application in spin direction, and to realize the magnetic overturning of garnet, outside face needed for anisotropic garnet
The driving current wanted is smaller.This also means that the spin logical device obtained based on anisotropy garnet outside face,
Power consumption can further decrease, development important in inhibiting of this discovery to device miniaturization, low-power consumption.There is document confirmation to only have
In thin garnet, the spin(-)orbit torque of thin film magnetic switching characteristic being only with spin correlation is dominated；But with
The easy magnetizing axis of the reduction of film thickness, film is gradually intended in face, therefore is difficult anisotropic garnet outside preparation face
Film.
Currently, anisotropy garnet outside the face being applied in self-spining device, mostly uses greatly magnetron sputtering or swashs
The methods of light pulse deposition adjusts stress suffered by film, and then changes the anisotropy of film.Liquid phase epitaxial method preparation
Garnet be high quality monocrystal thin films, defect is few and is easily achieved mass production.But extension strain is in its energy
Enough generating sufficiently large anisotropy, just relaxation, obtained film have been mostly intra-face anisotropy before；And liquid phase epitaxy work
Skill is immersion growth, and the thickness of obtained garnet is mostly micron order.It is thin how thickness to be obtained by liquid phase epitaxial method
And having anisotropic garnet outside face is current one of difficult point.
Summary of the invention
In view of the defects in the background art, the present invention proposes anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face and its
Preparation method.Non-linear relation is presented in the growth rate and growth temperature of monocrystalline garnet of the present invention, and the thickness of film is most
It is small to can reach 170nm, and anisotropy outside face is presented, it can be applied in spin logical device.
Technical scheme is as follows:
Anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, which is characterized in that the ingredient of the monocrystal thin films is Y3-(a+b+c)
BiaLubCacFe5-dGedO12, wherein 0 < a <, 0.5,0 < b <, 1.0,0 < c <, 1.0,0 < d < 1.0, and c=d.
The preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, comprising the following steps:
The preparation of step 1, melt: with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3It is accurate to claim for raw material
Take above-mentioned raw materials, wherein Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3Mass ratio be (0.07~0.10):
(0.10~0.15): (5~7): (0.7~1): (0.1~0.15): (70~76): (10~15): (4~7)；By above-mentioned raw materials
Layering is put into crucible, melt, is uniformly mixed, is obtained melt；
Step 2, cleaning substrate；
Step 3, liquid phase epitaxial method growing film: the substrate after step 2 cleaning is put into melt, using liquid phase epitaxial method
Monocrystal thin films are grown, growth temperature is 800~890 DEG C, and substrate revolving speed is 40~100 revs/min, after the completion of growth, cleaning
Obtain anisotropy MAGNETIC GARNET FILMS GROWN outside the face.
Further, in the preparation process of melt described in step 1, after weighing raw material, raw material layering is put into crucible, is made
PbO and MoO3Isolation, the placement order of other raw materials are not particularly limited.This is because PbO and MoO3It can react, PbO is gone back
Original is at metal.
Further, in the preparation process of melt described in step 1, after weighing raw material, raw material layering is put into crucible, point
Layer sequence specifically: the 1st layer of PbO for one third, the 2nd layer of Fe for half2O3, the 3rd layer is Y2O3、Lu2O3、
GeO2、MoO3With the Fe of remaining half2O3Mixed powder, the 4th layer be half Bi2O3, the 5th layer be CaO, the 6th
Layer is the Bi of remaining half2O3, the 7th layer of PbO for one third；Then 2h is kept the temperature at 1000~1100 DEG C, be cooled to
After 200 DEG C or less, then by the PbO addition crucible of remaining one third, 2h is kept the temperature at 1000~1100 DEG C；Finally,
12h is stirred at a temperature of 1000~1100 DEG C, is uniformly mixed, obtains melt.
Further, substrate described in step 2 is Gd-Ga garnet substrate (GGG), the cleaning process of substrate are as follows: by gadolinium gallium stone
Garnet substrate impregnates 3~10min in 70~80 DEG C of trichloro ethylene, then in 70~80 DEG C of deionized water impregnate 3~
10min；By upper step, treated that substrate embathes 10~15 in the mixed liquor of 70~80 DEG C of potassium bichromate, the concentrated sulfuric acid and water
Secondary, embathing the time every time is 1~2s, wherein the mass concentration of potassium bichromate is 18~20g/L, the concentrated sulfuric acid in the mixed liquor
Molar concentration be 10~15mol/L, then in 70~80 DEG C of deionized water impregnate 2~8min, another 70 after taking-up
3~10min is impregnated in~80 DEG C of deionized water；Sodium phosphate, sodium carbonate and potassium hydroxide that mass ratio is 1:1:1 are configured to
Solute mass concentration is the mixed alkali liquor of 10~15g/L, by upper step treated substrate in the lye of 70~80 DEG C of preparation
3~10min is impregnated, 3~10min is then impregnated in 70~80 DEG C of deionized water；By upper step, treated that substrate is put into room
3~10min of soaking and washing in the ammonia spirit that volumn concentration under temperature is 20~30%, then in deionized water at room temperature
Impregnate 3~10min；Upper step treated substrate is cleaned into 3~10min under the conditions of IPA vapor is condensed back.
Further, the detailed process of step 3 liquid phase epitaxial method growing film are as follows: be put into the substrate after step 2 cleaning
3~10min is preheated in melt, under conditions of growth temperature is 800~890 DEG C, substrate revolving speed is 40~100 revs/min, growth
After more than ten seconds to a few houres, quick lift-off melt simultaneously stops rotating, to obtain the film of different-thickness；Stand 3~10min minutes
Afterwards, substrate is slowly withdrawn from furnace body；The membrane substrate of taking-up is cleaned into remaining melt in hot acetic acid, can be obtained
Anisotropy MAGNETIC GARNET FILMS GROWN outside the face.
The invention has the benefit that
The present invention provides a kind of preparation methods of anisotropy MAGNETIC GARNET FILMS GROWN outside face, with Y2O3、Lu2O3、
Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3As raw material, the method for placing raw material using layering, on Gd-Ga garnet substrate
Having obtained thickness minimum can reach anisotropy MAGNETIC GARNET FILMS GROWN outside the face of 170nm.The monocrystalline stone that the present invention is prepared
Non-linear relation is presented in the growth rate and growth temperature of garnet film, and the thickness minimum of film can reach 170nm, with substrate
Lattice constant match is good, and anisotropy outside face is presented, and can be applied in spin logical device.
Detailed description of the invention
Fig. 1 is the knot of the liquid phase epitaxy furnace used when anisotropy MAGNETIC GARNET FILMS GROWN preparation outside face provided by the invention
Structure schematic diagram；In figure, 1 is motor, and 2 be GGG substrate, and 3 be heater, and 4 be crucible, and 5 be melt, and 6 be ceramic lifting rod, 7
For rotary shaft；
When Fig. 2 is that liquid phase epitaxial method provided by the invention prepares MAGNETIC GARNET FILMS GROWN, growth temperature and growth rate
Relational graph；
Fig. 3 is the VSM figure for the MAGNETIC GARNET FILMS GROWN that the embodiment of the present invention 1 is prepared；
Fig. 4 is the VSM figure for the MAGNETIC GARNET FILMS GROWN that the embodiment of the present invention 2 is prepared.
Specific embodiment
Technical solution of the present invention is explained in detail below in conjunction with specific embodiment.Following embodiment is only used for
It is more detailed to illustrate technical solution of the present invention, therefore it is only used as example, and cannot be used as a limitation and limit protection model of the invention
It encloses.
The preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, comprising the following steps:
Step 1, raw material weigh: with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3It is accurate to claim for raw material
Take above-mentioned raw materials, wherein Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3Mass ratio be (0.07~0.10):
(0.10~0.15): (5~7): (0.7~1): (0.1~0.15): (70~76): (10~15): (4~7)；
The preparation of step 2, melt: the weighed raw material layering of step 1 is put into crucible, hierarchical sequence specifically: the 1st layer
For the PbO of one third, the 2nd layer of Fe for half2O3, the 3rd layer is Y2O3、Lu2O3、GeO2、MoO3With remaining half
Fe2O3Mixed powder, the 4th layer be half Bi2O3, the 5th layer is CaO, the 6th layer of Bi for remaining half2O3,
The 7th layer of PbO for one third；Then keep the temperature 2h at 1000~1100 DEG C, after being cooled to 200 DEG C or less, then by residue three
/ mono- PbO is added in crucible, keeps the temperature 2h at 1000~1100 DEG C；Finally, being stirred at a temperature of 1000~1100 DEG C
12h is uniformly mixed, obtains melt；
Step 3, cleaning substrate: Gd-Ga garnet substrate is impregnated into 3~10min in 70~80 DEG C of trichloro ethylene, so
3~10min is impregnated in 70~80 DEG C of deionized water afterwards；By upper step treated substrate 70~80 DEG C potassium bichromate,
It is embathed in the mixed liquor of the concentrated sulfuric acid and water 10~15 times, embathing the time every time is 1~2s, wherein dichromic acid in the mixed liquor
The mass concentration of potassium is 18~20g/L, and the molar concentration of the concentrated sulfuric acid is 10~15mol/L, then in 70~80 DEG C of deionization
2~8min is impregnated in water, impregnates 3~10min after taking-up in another 70~80 DEG C of deionized water；It is 1:1:1 by mass ratio
Sodium phosphate, sodium carbonate and potassium hydroxide be configured to Solute mass concentration be 10~15g/L mixed alkali liquor, by upper step processing after
Substrate 3~10min is impregnated in the lye of 70~80 DEG C of preparation, then in 70~80 DEG C of deionized water impregnate 3~
10min；It is impregnated in the ammonia spirit for being 20~30% by upper step treated substrate is put into volumn concentration at room temperature clear
3~10min is washed, 3~10min is then impregnated in deionized water at room temperature；By upper step, treated that substrate is cold in IPA vapor
3~10min is cleaned under solidifying counterflow condition；
Step 4, liquid phase epitaxial method growing film: the substrate after step 3 cleaning is put into melt, using liquid phase epitaxial method
Monocrystal thin films are grown, growth temperature is 800~890 DEG C, and substrate revolving speed is 40~100 revs/min, after the completion of growth, cleaning
Obtain anisotropy MAGNETIC GARNET FILMS GROWN outside the face.
Embodiment 1
The preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, comprising the following steps:
Step 1, raw material weigh: with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3It is accurate to claim for raw material
Take above-mentioned raw materials, wherein Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3Mass ratio be 0.09:0.14:
5.29:0.85:0.12:75.63:11.77:6.11；
The preparation of step 2, melt: the weighed raw material layering of step 1 is put into crucible, hierarchical sequence specifically: the 1st layer
For the PbO of one third, the 2nd layer of Fe for half2O3, the 3rd layer is Y2O3、Lu2O3、GeO2、MoO3With remaining half
Fe2O3Mixed powder, the 4th layer be half Bi2O3, the 5th layer is CaO, the 6th layer of Bi for remaining half2O3,
The 7th layer of PbO for one third；Then 2h is kept the temperature at 1050 DEG C, after being cooled to 200 DEG C or less, then by remaining one third
PbO be added crucible in, keep the temperature 2h at 1080 DEG C；Finally, stirring 12h at a temperature of 1080 DEG C, it is uniformly mixed, is melted
Body；
Step 3, cleaning substrate: Gd-Ga garnet substrate is impregnated into 5min in 80 DEG C of trichloro ethylene, then at 80 DEG C
Deionized water in impregnate 5min；By upper step treated substrate in the mixed liquor of 80 DEG C of potassium bichromate, the concentrated sulfuric acid and water
It embathes 10 times, embathing the time every time is 1~2s, wherein the mass concentration of potassium bichromate is 18g/L, dense sulphur in the mixed liquor
The molar concentration of acid is 10mol/L, 2min is then impregnated in 80 DEG C of deionized water, in another 80 DEG C of deionization after taking-up
5min is impregnated in water；It is 15g/ that sodium phosphate, sodium carbonate and potassium hydroxide that mass ratio is 1:1:1, which are configured to Solute mass concentration,
The mixed alkali liquor of L, by upper step, treated that substrate impregnates 5min in the lye of 80 DEG C of preparation, then in 80 DEG C of deionization
5min is impregnated in water；It is impregnated in the ammonia spirit for being 25% by upper step treated substrate is put into volumn concentration at room temperature
5min is cleaned, 5min is then impregnated in deionized water at room temperature；Upper step treated substrate is condensed back in IPA vapor
Under the conditions of clean 5min；
Step 4, liquid phase epitaxial method growing film: the substrate after step 2 cleaning is put into melt and preheats 5min, is being grown
Under conditions of temperature is 858 DEG C, substrate revolving speed is 60 revs/min, after growing 30s, quick lift-off melt simultaneously stops rotating；It stands
After 5min, substrate is slowly withdrawn from furnace body；The membrane substrate of taking-up is cleaned in 113 DEG C of hot acetic acid remaining molten
Anisotropic Y outside the face can be obtained in body1.32Bi0.14Lu0.96Ca0.58Fe4.42Ge0.58O12MAGNETIC GARNET FILMS GROWN.
As shown in figure 3, the Y with a thickness of 170nm obtained for embodiment 11.32Bi0.14Lu0.96Ca0.58Fe4.42Ge0.58O12Stone
The VSM test chart of garnet single crystal film；Fig. 3 shows outside the face for the MAGNETIC GARNET FILMS GROWN that embodiment 1 obtains in saturation field specific surface
The small 400Oe of saturation field, is presented anisotropy outside apparent face.
Embodiment 2
The preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, comprising the following steps:
Step 1, raw material weigh: with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3It is accurate to claim for raw material
Take above-mentioned raw materials, wherein Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3Mass ratio be 0.08:0.14:
6.19:0.87:0.14:73.15:14.30:5.13；
The preparation of step 2, melt: the weighed raw material layering of step 1 is put into crucible, hierarchical sequence specifically: the 1st layer
For the PbO of one third, the 2nd layer of Fe for half2O3, the 3rd layer is Y2O3、Lu2O3、GeO2、MoO3With remaining half
Fe2O3Mixed powder, the 4th layer be half Bi2O3, the 5th layer is CaO, the 6th layer of Bi for remaining half2O3,
The 7th layer of PbO for one third；Then 2h is kept the temperature at 1050 DEG C, after being cooled to 200 DEG C or less, then by remaining one third
PbO be added crucible in, keep the temperature 2h at 1080 DEG C；Finally, stirring 12h at a temperature of 1080 DEG C, it is uniformly mixed, is melted
Body；
Step 3, cleaning substrate: Gd-Ga garnet substrate is impregnated into 5min in 80 DEG C of trichloro ethylene, then at 80 DEG C
Deionized water in impregnate 5min；By upper step treated substrate in the mixed liquor of 80 DEG C of potassium bichromate, the concentrated sulfuric acid and water
It embathes 10 times, embathing the time every time is 1~2s, wherein the mass concentration of potassium bichromate is 18g/L, dense sulphur in the mixed liquor
The molar concentration of acid is 10mol/L, 2min is then impregnated in 80 DEG C of deionized water, in another 80 DEG C of deionization after taking-up
5min is impregnated in water；It is 15g/ that sodium phosphate, sodium carbonate and potassium hydroxide that mass ratio is 1:1:1, which are configured to Solute mass concentration,
The mixed alkali liquor of L, by upper step, treated that substrate impregnates 5min in the lye of 80 DEG C of preparation, then in 80 DEG C of deionization
5min is impregnated in water；It is impregnated in the ammonia spirit for being 25% by upper step treated substrate is put into volumn concentration at room temperature
5min is cleaned, 5min is then impregnated in deionized water at room temperature；Upper step treated substrate is condensed back in IPA vapor
Under the conditions of clean 5min；
Step 4, liquid phase epitaxial method growing film: the substrate after step 2 cleaning is put into melt and preheats 5min, is being grown
Under conditions of temperature is 866 DEG C, substrate revolving speed is 60 revs/min, after growing 2min, quick lift-off melt simultaneously stops rotating；It stands
After 5min, substrate is slowly withdrawn from furnace body；The membrane substrate of taking-up is cleaned in 113 DEG C of hot acetic acid remaining molten
Anisotropic Y outside the face can be obtained in body1.26Bi0.16Lu0.96Ca0.62Fe4.38Ge0.62O12MAGNETIC GARNET FILMS GROWN.
As shown in figure 4, the Y with a thickness of 670nm obtained for embodiment 21.26Bi0.16Lu0.96Ca0.62Fe4.38Ge0.62O12Stone
The VSM test chart of garnet single crystal film；Fig. 4 shows outside the face for the MAGNETIC GARNET FILMS GROWN that embodiment 2 obtains in saturation field specific surface
The small 220Oe of saturation field, is presented anisotropy outside apparent face.
Outside face provided by the invention in the preparation method of anisotropy MAGNETIC GARNET FILMS GROWN, PbO-Bi2O3-MoO3It is fluxing
Agent effectively reduces the viscosity of melt, and the lattice constant and matched coefficients of thermal expansion between monocrystal thin films and substrate obtained are good,
Show mirror effect；Non-linear relation is presented in growth rate and growth temperature, and the thickness minimum of film can reach 170nm；And
The outer anisotropy in presentation face can be applied in spin logical device.
Claims (5)
1. anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, which is characterized in that the ingredient of the monocrystal thin films is Y3-(a+b+c)
BiaLubCacFe5-dGedO12, wherein 0 < a <, 0.5,0 < b <, 1.0,0 < c <, 1.0,0 < d < 1.0, and c=d.
2. the preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside a kind of face, comprising the following steps:
The preparation of step 1, melt: with Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3For raw material, accurately weigh
State raw material, wherein Y2O3、Lu2O3、Fe2O3、GeO2、CaO、PbO、Bi2O3、MoO3Mass ratio be (0.07~0.10): (0.10
~0.15): (5~7): (0.7~1): (0.1~0.15): (70~76): (10~15): (4~7)；Above-mentioned raw materials layering is put
Enter in crucible, melt, is uniformly mixed, obtains melt；
Step 2, cleaning substrate；
Step 3, liquid phase epitaxial method growing film: the substrate after step 2 cleaning is put into melt, is grown using liquid phase epitaxial method
Monocrystal thin films, growth temperature are 800~890 DEG C, and substrate revolving speed is 40~100 revs/min, after the completion of growth, and cleaning can be obtained
Anisotropy MAGNETIC GARNET FILMS GROWN outside the face.
3. the preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside face according to claim 2, which is characterized in that step
In the preparation process of 1 melt, after weighing raw material, raw material layering is put into crucible, PbO and MoO are made3Isolation.
4. the preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside face according to claim 2, which is characterized in that step
In the preparation process of 1 melt, after weighing raw material, raw material layering is put into crucible, hierarchical sequence are as follows: the 1st layer is three points
One of PbO, the 2nd layer be half Fe2O3, the 3rd layer is Y2O3、Lu2O3、GeO2、MoO3With remaining half
Fe2O3Mixed powder, the 4th layer be half Bi2O3, the 5th layer is CaO, the 6th layer of Bi for remaining half2O3, the
7 layers of PbO for one third；Then 2h is kept the temperature at 1000~1100 DEG C, after being cooled to 200 DEG C or less, then will be three points remaining
One of PbO be added crucible in, keep the temperature 2h at 1000~1100 DEG C；Finally, 12h is stirred at a temperature of 1000~1100 DEG C,
It is uniformly mixed, obtains melt.
5. the preparation method of anisotropy MAGNETIC GARNET FILMS GROWN outside face according to claim 2, which is characterized in that step
2 substrates are Gd-Ga garnet substrate, the cleaning process of substrate are as follows: three chloroethenes by Gd-Ga garnet substrate at 70~80 DEG C
3~10min is impregnated in alkene, and 3~10min is then impregnated in 70~80 DEG C of deionized water；By upper step, treated that substrate exists
It is embathed 10~15 times in the mixed liquor of 70~80 DEG C of potassium bichromate, the concentrated sulfuric acid and water, embathing the time every time is 1~2s, wherein
The mass concentration of potassium bichromate is 18~20g/L in the mixed liquor, and the molar concentration of the concentrated sulfuric acid is 10~15mol/L, then
In 70~80 DEG C of deionized water impregnate 2~8min, after taking-up in another 70~80 DEG C of deionized water impregnate 3~
10min；It is 10~15g/L's that sodium phosphate, sodium carbonate and potassium hydroxide that mass ratio is 1:1:1, which are configured to Solute mass concentration,
Mixed alkali liquor, by upper step, treated that substrate impregnates 3~10min in the lye of 70~80 DEG C of preparation, then 70~80
DEG C deionized water in impregnate 3~10min；Treated that substrate is put into that volumn concentration at room temperature is 20 by upper step~
Then 3~10min of soaking and washing in 30% ammonia spirit impregnates 3~10min in deionized water at room temperature；Upper step is handled
Substrate afterwards cleans 3~10min under the conditions of IPA vapor is condensed back.
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