CN107299394A - The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face - Google Patents

The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face Download PDF

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CN107299394A
CN107299394A CN201710405520.4A CN201710405520A CN107299394A CN 107299394 A CN107299394 A CN 107299394A CN 201710405520 A CN201710405520 A CN 201710405520A CN 107299394 A CN107299394 A CN 107299394A
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substrate
msub
mrow
melt
thin film
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杨青慧
郝俊祥
张怀武
马博
饶毅恒
金立川
文岐业
李明明
刘元昆
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University of Electronic Science and Technology of China
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/28Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B19/00Liquid-phase epitaxial-layer growth
    • C30B19/02Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
    • C30B19/04Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux the solvent being a component of the crystal composition

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Abstract

The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:Prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3Melt is prepared for raw material;Clean substrate;Substrate after cleaning is put into melt, at a temperature of 935 DEG C, substrate rotating speed be 120rpm, grow 1~5min, after the completion of growth, cleaning remove residual, obtain easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face of the present invention.The magneto-optic thin film that the present invention is prepared can be applied to spin logical device.The present invention has drawn suitable oxide proportioning, and combines the characteristics of oxide is matched, the submicron order monocrystalline Bi prepared using the high-revolving method of Seedling height temperature:TmIG films, its film thickness is 100~1000nm, with the easy magnetizing axis perpendicular to film surface (outside face).

Description

Outside submicron order face prepared by the liquid phase epitaxy of easy magnetization monocrystalline garnet magneto-optic thin film Method
Technical field
The present invention relates to technical field of electronic materials, and in particular to easy magnetization monocrystalline garnet magnetic outside a kind of submicron order face The liquid phase epitaxy preparation method of optical thin film.
Background technology
Since the sixties in last century five, the fast development of microwave communication techniques has driven the demand to basic material, MAGNETIC GARNET FILMS GROWN is set to also become a big study hotspot.Afterwards with the development of Fibre Optical Communication Technology, make magneto optic garnets Monocrystal thin films are aroused great concern.Found that YIG materials can be as the perfact conductor for conducting spin wave, section from 2010 Educational circles is absorbed in the exploration that YIG materials are applied in spin field always.American scholar C.O.Avci et.al exist within 2016《From So》Upper report TmIG magneto-optic memory techniques equally can make magneto-optic memory technique answering in spin field as the perfact conductor for conducting spin wave Turn into new focus with research.Research is found, although TmIG magneto-optic thin films are a kind of current insulator in itself, and spin current still can be Wherein transmit, spinning electron enters in magnetic insulator, and a microcosmic torque (spin transfer torque) can be produced to magnetic moment, profit The upset to magnetic moment can be realized with this spin transfer torque.This case utilizes the submicrometer-thick Bi of liquid phase epitaxy:TmIG Easy magnetization characteristic outside the face of film, it is possible to achieve the Magnetic moment reversal of relatively low spin current size induction, for exploitation room temperature low-power consumption certainly Rotation electronic device has established important material foundation.But magnetize outside thicker face in TmIG garnets, realize spin current There is very big difficulty in Magnetic moment reversal, cause it can not be applied to spin logical device.Therefore, magnetize outside the face of self-spining device application TmIG films, thickness needs to control in submicron order even nanoscale.In addition, although TmIG films are easy magnetization materials outside face Material, but saturation magnetic field is larger, and how to reduce saturation field is also one of difficult point.
Liquid phase epitaxy technology be in the most important a kind of technology of Grown monocrystal thin films or thick film, can be by suitable When the proportioning of oxide in control melt, the performance of thin-film material is adjusted.It is usually in gadolinium gallium by taking monocrystalline garnet as an example Garnet (GGG) Grown microwave monocrystalline or magneto optical single crystal.
At present, the thickness of magneto optical single crystal film prepared by liquid phase epitaxy is micron order mostly, and submicron order is not prepared also The effective ways of magneto optical single crystal film.Main reason is that:1st, suitable oxide proportioning is not found at present;2nd, make at present The conventional thinking of the magneto-optic thin film of standby thinner thickness is low growth rate (extremely low degree of supercooling), short growth time, yet with mistake The driving force of the cold extremely low generation of degree is smaller, and substrate surface is difficult Quick uniform nucleation and crystallization, and this to prepare submicron order The monocrystalline garnet magneto-optic thin film of thickness turns into a technical barrier.
The content of the invention
For defect of the prior art, the present invention provides easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face Liquid phase epitaxy preparation method, to obtain thickness as 100nm~1000nm, the compact structure of film, the monocrystalline stone stone of surfacing Garnet magneto-optic thin film.
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, using R factor methods of completing the square (Blank- Nielsen Y-factor method Ys) carry out dispensing and obtain melt, the R factors being related to have R1, R2, R3, the relations of three factors it is following (mole Than):
Wherein, Garnetoxides refers to the component oxide for constituting garnet, and Garnetoxides+Flux refers to Constitute the component oxide and Bi of garnet2O3The total amount of flux.
S2, cleaning substrate;
S3, step S2 is cleaned after substrate be put into melt, at a temperature of 935 DEG C, substrate rotating speed be 120rpm, it is raw Long 1~5min, cleaning removes residual after the completion of growth, obtains easy magnetization monocrystalline garnet magnetic outside submicron order face of the present invention Optical thin film.
In the present invention, as a kind of perferred technical scheme, step S1 detailed process is:Precise raw material Ga2O3、 Tm2O3、Fe2O3、Bi2O3, it is placed in platinum crucible after ground and mixed, 20~24h is melted at 1050~1080 DEG C, then 980 10~12h is stirred at~1000 DEG C, improving uniformity of melt is obtained.
In the present invention, as a kind of perferred technical scheme, the substrate that step S2 is used is Gd-Ga garnet (GGG) base Piece.
In the present invention, as a kind of perferred technical scheme, the detailed process of cleaning substrate is:GGG substrates are existed successively Ultrasound is respectively washed twice in deionized water, acetone, alcohol;Then it is 1 in volume ratio:1 concentrated sulfuric acid and the mixed liquor of nitric acid In boil 10~30min;Finally use deionized water rinsing substrate 3~5 times, dry for standby.
In the present invention, as a kind of perferred technical scheme, in step S3, the detailed process that cleaning removes residual is:It is raw After the completion of length, by the quick lift-off of substrate to away from being rotated at a high speed at 20~30mm of melt liquid level and with 180~200 rpm speed, To get rid of the remaining melt on substrate, substrate is then slowly withdrawn from epitaxial furnace to avoid because film is opened caused by thermal expansion Split;Finally obtained membrane substrate is cleaned to remove the fluxing agent of residual in hot nitric acid.
Easy magnetization monocrystalline garnet magneto-optic thin film is in spin logical device energy outside the submicron order face that the present invention is prepared Enough applied, it can be used as the part component of spin logic device, and therefore not to repeat here.
Due to using above technical scheme, the present invention has the advantages that:
Inventor has drawn suitable oxide proportioning, and combine the spy that oxide is matched by experiment largely repeatedly Point, the submicron order monocrystalline Bi prepared using the high-revolving method of Seedling height temperature:TmIG films, are monocrystalline state, and its is thin Film thickness is 100~1000nm, with the easy magnetizing axis perpendicular to film surface (outside face);And compact structure, the surface of film It is smooth, it is a kind of good material that can be applied to spin logical device.
When the conventional thinking for the magneto-optic thin film for preparing thinner thickness at present is low growth rate (extremely low degree of supercooling), short growth Between.Smaller yet with the driving force of the extremely low generation of degree of supercooling, substrate surface is difficult Quick uniform nucleation and crystallization, and this hair It is bright by increase film grow when substrate rotating speed, while using suitable oxide match, make substrate at a high speed rotation produce Interface driving force increase, further promotes substrate surface nucleation and crystallization, while effectively extending growth time, surface nucleation is had foot Enough time homogenization, finally give uniform submicron order monocrystalline Bi:TmIG magneto-optic thin films.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art The accompanying drawing used required in embodiment or description of the prior art is briefly described.In all of the figs, similar element Or part is general by similar reference mark.In accompanying drawing, each element or part might not be drawn according to actual ratio.
Fig. 1 is the structural representation for the liquid phase epitaxy stove that liquid phase epitaxial method of the present invention is used;
Fig. 2 is the graph of a relation of rheotaxial growth temperature of the present invention and growth rate (growth rotating speed is 60rpm);
Fig. 3 is the Bi that the embodiment of the present invention is prepared:The AFM figures of TmIG films;
Fig. 4 is the Bi that the embodiment of the present invention is prepared:The VSM test curves of TmIG films.
Embodiment
Technical solution of the present invention is described in detail below in conjunction with specific embodiment.Following examples are only used for more Plus technical scheme is clearly demonstrated, therefore example is only used as, and can not be limited the scope of the invention with this.
Embodiment 1
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, dispensing is carried out using R factors method of completing the square and obtained Melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
In the present embodiment, Ga2O3、Tm2O3、Fe2O3、Bi2O3Mass ratio be 1:2.08:8.027:130.9, ground and mixed After be placed in platinum crucible, at 1050 DEG C melt 20~24h, then stir 10h at 980 DEG C, obtain improving uniformity of melt;
S2, the substrate used clean substrate for Gd-Ga garnet (GGG) substrate:By GGG substrates successively deionized water, Ultrasound is respectively washed twice in acetone, alcohol;Then it is 1 in volume ratio:Boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid 10min;Finally use deionized water rinsing substrate 3 times, dry for standby;
S3, step 2 is cleaned after substrate be put into melt, at a temperature of 935 DEG C, substrate rotating speed be 120rpm, growth 1min, after the completion of growth, by the quick lift-off of substrate to away from being rotated at a high speed at melt liquid level 20mm and with 180rpm speed, to get rid of Fall the remaining melt on substrate, substrate is then slowly withdrawn from epitaxial furnace to avoid due to film peeling caused by thermal expansion; Finally obtained membrane substrate is cleaned to remove the fluxing agent of residual in hot nitric acid, obtain sub-micron of the present invention Easy magnetization monocrystalline garnet magneto-optic thin film outside level face.
Embodiment 2
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, dispensing is carried out using R factors method of completing the square and obtained Melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
In the present embodiment, Ga2O3、Tm2O3、Fe2O3、Bi2O3Mass ratio be 1:2.08:8.027:130.9, ground and mixed After be placed in platinum crucible, 24h is melted at 1080 DEG C, then 12h is stirred at 1000 DEG C, obtains improving uniformity of melt;
S2, the substrate used clean substrate for Gd-Ga garnet (GGG) substrate:By GGG substrates successively deionized water, Ultrasound is respectively washed twice in acetone, alcohol;Then it is 1 in volume ratio:Boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid 30min;Finally use deionized water rinsing substrate 5 times, dry for standby;
S3, step S2 is cleaned after substrate be fixed on platinum support, keep substrate and melt liquid level to have one small Substrate slow (being put into the time control of completion in 2min) is put into melt by 10 ° of angle;Growth temperature is 935 DEG C, and substrate turns Speed is 120rpm, and growth time is 5min, and substrate changes a direction of rotation every 5s, after the completion of growth, by substrate quick (3 In second) lift-off is at away from melt liquid level 30mm, and the substrate that upper step is obtained is rotated at a high speed with 200rpm speed to be got rid of on substrate Remaining melt, then slow from epitaxial furnace (deadline was controlled at 5 minutes) lifts substrate to avoid because thermal expansion is drawn The film peeling risen;Finally the obtained substrate with monocrystal thin films is cleaned to remove residual in the hot nitric acid close to boiling Fluxing agent, obtains easy magnetization monocrystalline Bi outside submicron order face of the present invention:TmIG magneto-optic thin films.
Embodiment 3
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, dispensing is carried out using R factors method of completing the square and obtained Melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
In the present embodiment, Ga2O3、Tm2O3、Fe2O3、Bi2O3Mass ratio be 1:2.08:8.027:130.9, ground and mixed After be placed in platinum crucible, at 1050~1080 DEG C melt 20~24h, then at 980~1000 DEG C stir 10~12h, obtain To improving uniformity of melt;
S2, the substrate used is Gd-Ga garnet (GGG) substrates, by GGG substrates successively in deionized water, acetone, alcohol Middle ultrasonic cleaning is twice;Then it is 1 in volume ratio:15min is boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid;Finally use and go Ionized water rinse substrate 5 times, dry for standby;
S3, the growth temperature of liquid phase epitaxial method growth monocrystalline garnet are a temperature range, different growth temperature The different growth rate of degree point correspondence, the higher growth rate of relatively low growth temperature correspondence, higher growth temperature correspondence compared with Low speed, the present invention selects minimum growth rate to grow monocrystal thin films, therefore, and the growth temperature that the present invention chooses is can The maximum temperature point for maintaining film continuously to grow.As shown in Fig. 2 the temperature range that the achievable film of the present invention continuously grows is 920~935 DEG C, the present embodiment growth selection monocrystalline Bi:The growth temperature of TmIG magneto-optic garnet films is chosen for maximum temperature 935 DEG C are put, concrete operation method is:Substrate after step S2 is cleaned is fixed on platinum support, keeps substrate and melt liquid Face has 10 ° small of an angle that substrate slow (being put into the time control of completion in 2min) is put into melt;Growth temperature is 935 DEG C, substrate rotating speed is 120rpm, and growth time is 2min, and substrate changes a direction of rotation every 5s, after the completion of growth, By quick (in the 3 seconds) lift-off of substrate at away from melt liquid level 20mm, the substrate that upper step is obtained is revolved at a high speed with 200rpm speed Turn to get rid of the remaining melt on substrate, then slow from epitaxial furnace (deadline was controlled at 5 minutes) lifts substrate to avoid Due to film peeling caused by thermal expansion;Finally the obtained substrate with monocrystal thin films is cleaned in the hot nitric acid close to boiling To remove the fluxing agent of residual, easy magnetization monocrystalline Bi outside submicron order face of the present invention is obtained:TmIG magneto-optic thin films.
Embodiment 4
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, dispensing is carried out using R factors method of completing the square and obtained Melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
In the present embodiment, Ga2O3、Tm2O3、Fe2O3、Bi2O3Mass ratio be 1:2.08:8.027:130.9, ground and mixed After be placed in platinum crucible, 22h is melted at 1060 DEG C, then 11h is stirred at 990 DEG C, obtains improving uniformity of melt;
S2, the substrate used clean substrate for Gd-Ga garnet (GGG) substrate:By GGG substrates successively deionized water, Ultrasound is respectively washed twice in acetone, alcohol;Then it is 1 in volume ratio:Boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid 20min;Finally use deionized water rinsing substrate 4 times, dry for standby;
S3, step S2 is cleaned after substrate be fixed on platinum support, keep substrate and melt liquid level to have one small Substrate slow (being put into the time control of completion in 2min) is put into melt by 10 ° of angle;Growth temperature is 935 DEG C, and substrate turns Speed is 120rpm, and growth time is 2min, and substrate changes a direction of rotation every 5s, after the completion of growth, by substrate quick (3 In second) lift-off is at away from melt liquid level 25mm, and the substrate that upper step is obtained is rotated at a high speed with 190rpm speed to be got rid of on substrate Remaining melt, then slow from epitaxial furnace (deadline was controlled at 5 minutes) lifts substrate to avoid because thermal expansion is drawn The film peeling risen;Finally the obtained substrate with monocrystal thin films is cleaned to remove residual in the hot nitric acid close to boiling Fluxing agent, obtains easy magnetization monocrystalline Bi outside submicron order face of the present invention:TmIG magneto-optic thin films.
Embodiment 5
The liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film, comprises the following steps outside submicron order face:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be molten Agent, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, dispensing is carried out using R factors method of completing the square and obtained Melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
In the present embodiment, Ga2O3、Tm2O3、Fe2O3、Bi2O3Mass ratio be 1:2.08:8.027:130.9, ground and mixed After be placed in platinum crucible, 24h is melted at 1055 DEG C, then 12h is stirred at 985 DEG C, obtains improving uniformity of melt;
S2, the substrate used clean substrate for Gd-Ga garnet (GGG) substrate:By GGG substrates successively deionized water, Ultrasound is respectively washed twice in acetone, alcohol;Then it is 1 in volume ratio:Boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid 25min;Finally use deionized water rinsing substrate 5 times, dry for standby;
S3, step S2 is cleaned after substrate be fixed on platinum support, keep substrate and melt liquid level to have one small Substrate slow (being put into the time control of completion in 2min) is put into melt by 10 ° of angle;Growth temperature is 935 DEG C, and substrate turns Speed is 120rpm, and growth time is 3min, and substrate changes a direction of rotation every 5s, after the completion of growth, by substrate quick (3 In second) lift-off is at away from melt liquid level 20mm, and the substrate that upper step is obtained is rotated at a high speed with 200rpm speed to be got rid of on substrate Remaining melt, then slow from epitaxial furnace (deadline was controlled at 5 minutes) lifts substrate to avoid because thermal expansion is drawn The film peeling risen;Finally the obtained substrate with monocrystal thin films is cleaned to remove residual in the hot nitric acid close to boiling Fluxing agent, obtains easy magnetization monocrystalline Bi outside submicron order face of the present invention:TmIG magneto-optic thin films.
Above example liquid phase epitaxy preparation method is carried out using the liquid phase epitaxy stove such as Fig. 1 structures, and melt 5 is placed in In crucible 4, and heated using heater 3, clamp GGG substrates 2 using ceramic lifting rod 6 and put it into melt 5, Open motor 1 simultaneously, drive GGG substrates 2 to rotate by rotary shaft 7, after the completion of utilize the ceramic lifting of lifting rod 6 GGG substrates 2。
Select the monocrystalline Bi that embodiment 3 is prepared:TmIG magneto-optic thin films are detected.
Fig. 3 is the monocrystalline Bi that the embodiment of the present invention 3 is obtained:The AFM figures of TmIG magneto-optic thin films, from Fig. 3, the present invention The compact structure of obtained film, surfacing, the smaller RMS=0.42nm of roughness.Fig. 4 is what the embodiment of the present invention 3 was obtained Bi:The VSM test curves of TmIG monocrystal thin films, as shown in Figure 4, the Bi that the present invention is obtained:The easy magnetizing axis of TmIG monocrystal thin films Outside face, magnetized saturation field is less than 40Oe outside face.
Finally it should be noted that:Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations;To the greatest extent The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that:Its according to The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered Row equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology The scope of scheme, it all should cover among the claim of the present invention and the scope of specification.

Claims (5)

1. the liquid phase epitaxy preparation method of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face, it is characterised in that including Following steps:
S1, prepare melt:With Ga2O3、Tm2O3、Fe2O3、Bi2O3For raw material, Bi2O3Not only provide composition for film but also be flux, Ga2O3To reduce saturation field;
According to formula:(BixTm3-x)(GayFe5-y)O12, 0<x<3,0<y<5, using R factors method of completing the square (Blank-Nielsen systems Number methods) carry out dispensing and obtain melt, the R factors being related to have R1, R2, R3, and the relation of three factors is following (mol ratio):
<mrow> <mi>R</mi> <mn>1</mn> <mo>=</mo> <mfrac> <mrow> <msub> <mi>Tm</mi> <mn>2</mn> </msub> <msub> <mi>O</mi> <mn>3</mn> </msub> </mrow> <mrow> <msub> <mi>Fe</mi> <mn>2</mn> </msub> <msub> <mi>O</mi> <mn>3</mn> </msub> </mrow> </mfrac> <mo>=</mo> <mn>0.1</mn> <mo>~</mo> <mn>0.2</mn> <mo>;</mo> <mi>R</mi> <mn>2</mn> <mo>=</mo> <mfrac> <mrow> <msub> <mi>Ga</mi> <mn>2</mn> </msub> <msub> <mi>O</mi> <mn>3</mn> </msub> </mrow> <mrow> <msub> <mi>Fe</mi> <mn>2</mn> </msub> <msub> <mi>O</mi> <mn>3</mn> </msub> </mrow> </mfrac> <mo>=</mo> <mn>0.1</mn> <mo>~</mo> <mn>0.135</mn> <mo>;</mo> <mi>R</mi> <mn>3</mn> <mo>=</mo> <mfrac> <mrow> <mi>G</mi> <mi>a</mi> <mi>r</mi> <mi>n</mi> <mi>e</mi> <mi>t</mi> <mi>o</mi> <mi>x</mi> <mi>i</mi> <mi>d</mi> <mi>e</mi> <mi>s</mi> </mrow> <mrow> <mi>G</mi> <mi>a</mi> <mi>r</mi> <mi>n</mi> <mi>e</mi> <mi>t</mi> <mi>o</mi> <mi>x</mi> <mi>i</mi> <mi>d</mi> <mi>e</mi> <mi>s</mi> <mo>+</mo> <mi>F</mi> <mi>l</mi> <mi>u</mi> <mi>x</mi> </mrow> </mfrac> <mo>=</mo> <mn>0.1</mn> <mo>~</mo> <mn>0.2</mn> <mo>;</mo> </mrow>
S2, cleaning substrate;
S3, by step S2 clean after substrate be put into melt, at a temperature of 935 DEG C, substrate rotating speed be 120rpm, growth 1~ 5min, after the completion of growth, cleaning removes residual, obtains easy magnetization monocrystalline garnet magneto-optic outside submicron order face of the present invention thin Film.
2. the liquid phase epitaxy preparation side of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face according to claim 1 Method, it is characterised in that step S1 detailed process is:Precise raw material Ga2O3、Tm2O3、Fe2O3、Bi2O3, after ground and mixed It is placed in platinum crucible, 20~24h is melted at 1050~1080 DEG C, 10~12h is then stirred at 980~1000 DEG C, is obtained Improving uniformity of melt.
3. the liquid phase epitaxy preparation side of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face according to claim 1 Method, it is characterised in that the substrate that step S2 is used is Gd-Ga garnet (GGG) substrate.
4. the liquid phase epitaxy preparation side of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face according to claim 3 Method, it is characterised in that cleaning substrate detailed process be:By the GGG substrates successively ultrasound point in deionized water, acetone, alcohol Do not clean twice;Then it is 1 in volume ratio:10~30min is boiled in 1 concentrated sulfuric acid and the mixed liquor of nitric acid;Finally use and go Ionized water rinse substrate 3~5 times, dry for standby.
5. the liquid phase epitaxy preparation side of easy magnetization monocrystalline garnet magneto-optic thin film outside submicron order face according to claim 1 Method, it is characterised in that in step S3, cleaning removes the detailed process remained and is:After the completion of growth, by the quick lift-off of substrate to away from Rotated at a high speed at 20~30mm of melt liquid level and with 180~200rpm speed, to get rid of the remaining melt on substrate, Ran Houcong Substrate is slowly withdrawn in epitaxial furnace to avoid due to film peeling caused by thermal expansion;Finally obtained membrane substrate is existed Clean to remove the fluxing agent of residual in hot nitric acid.
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