CN101311374A - Yttrium-iron-garnet film structure and preparation method - Google Patents

Yttrium-iron-garnet film structure and preparation method Download PDF

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CN101311374A
CN101311374A CNA2008100443023A CN200810044302A CN101311374A CN 101311374 A CN101311374 A CN 101311374A CN A2008100443023 A CNA2008100443023 A CN A2008100443023A CN 200810044302 A CN200810044302 A CN 200810044302A CN 101311374 A CN101311374 A CN 101311374A
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substrate
yttrium
iron
ceo
transition layer
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CN101311374B (en
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杨青慧
张怀武
刘颖力
文岐业
李元勋
贾利军
唐晓莉
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Abstract

The invention relates to an yttrium iron garnet film structure which belongs to the field of electronic material, in particularly to a method for preparing radio frequency magnetron sputtering of yttrium iron garnet film materials. The film structure consists of a Si substrate and an yttrium iron garnet film layer, wherein a CeO2 transient layer is also arranged between the Si substrate and the yttrium iron garnet film layer. The yttrium iron garnet film structure has the advantages that: surface of the film is improved greatly, surface roughness is reduced obviously, saturation magnetization and remnant magnetization of the film is improved, and coercive force is reduced.

Description

Yttrium-iron-garnet film structure and preparation method
Technical field
The invention belongs to field of electronic materials, it is particularly related to the rf magnetron sputtering preparation method of Yttrium-iron garnet thin film material.
Background technology
The garnet film is because its excellent Faraday effect and low transmission loss are considered to a kind of very promising material in the nonreciprocal waveguide device of high-performance, integrated magneto-optical device and microwave device.Si occupies critical role in unicircuit simultaneously, is that its research preparation of film of substrate becomes very popular with Si, because it may realize the integrated of Si base microelectronic device and optical waveguide.Preparation on the Si substrate has had a lot of documents to mention about garnet, and the garnet film is on the Si substrate and unlike preparing on other substrates, as quartz, GGG, Al 2O 3Substrate etc., like that easy to be complete by crystallization, so its magnetic property and magneto-optical property are than there being very big gap.
Summary of the invention
Technical problem to be solved by this invention is, a kind of new Yttrium-iron-garnet film structure is provided, and than prior art, the specific magnetising moment and residual magnetization all have significant improvement, the coercive force of film reduces, and the surfaceness of film has greatly improved simultaneously.
Another technical problem to be solved by this invention is that the preparation method of aforementioned Yttrium-iron-garnet film structure is provided.
The technical scheme that the present invention solve the technical problem employing is that Yttrium-iron-garnet film structure comprises Si substrate and the yttrium iron garnet thin film layer on it, it is characterized in that, also has CeO between Si substrate and yttrium iron garnet thin film layer 2Transition layer.CeO 2Transition layer is for being coated on the Si substrate.
The present invention also provides the Yttrium-iron-garnet film structure preparation method, may further comprise the steps:
The surface of step 1, cleaning Si substrate;
Step 2, cleaned Si substrate is placed vacuum chamber, vacuumize;
Step 3, on the Si substrate sputter CeO 2Transition layer;
Step 4, having CeO 2Sputter yttrium iron garnet film on the Si substrate of transition layer;
Step 5, anneal.
Step is more specifically:
Step 1, at first pre-treatment is carried out on the surface of substrate, cleaning step is:
(1) uses the deionized water ultrasonic cleaning; (2) use the acetone ultrasonic cleaning; (3) with the clear ultrasonic cleaning of wine; (4) with purified rinse water and oven dry;
Step 2, cleaned substrate is placed on the sputtering unit of vacuum chamber pumping high vacuum.
Step 3, sputter CeO 2Transition layer: when vacuum tightness reaches 5 * 10 -4When Pa is following, charge into argon gas, make pressure maintain 7 * 10 -1Pa, sputter CeO 2
Step 4, be coated with the yttrium iron garnet film;
Step 5, anneal: the film of sputtering sedimentation put into handle stove, during less than 10-2, heat up insulation for some time postcooling in vacuum tightness.
The invention has the beneficial effects as follows and do not have CeO 2The garnet thin film material of transition layer is compared, and the present invention has the following advantages:
The surface of film is improved significantly, and surfaceness obviously reduces.
The saturation magnetization of film and residual magnetization improve, and coercive force descends.
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 rf magnetron sputtering device structure synoptic diagram.
Wherein, substrate 1, target 2, film putting-down chamber 3, vacuum pump 4, radio frequency source 5, recirculated cooling water 6, baffle plate 7, Ar gas inlet 8, O 2Gas inlet 9, vacuumometer 10.
Fig. 2 garnet film is at the Si substrate that does not have transition layer and CeO is arranged 2Crystallization state correlation curve figure on the Si substrate of transition layer.
Fig. 3 garnet film is at the Si substrate that does not have transition layer and CeO is arranged 2Surfaceness photo contrast on the Si substrate of transition layer.
Fig. 4 garnet film is at the Si substrate that does not have transition layer and CeO is arranged 2Magnetic hysteresis loop correlation curve figure on the Si substrate of transition layer.
Fig. 5 garnet film is at the Si substrate that does not have transition layer and CeO is arranged 2Saturation magnetization, residual magnetization and coercive force on the Si substrate of transition layer is with the variation correlation curve figure of annealing atmosphere.
Fig. 6 is a Yttrium-iron-garnet film structure synoptic diagram of the present invention.
Embodiment
The invention provides a kind of Yttrium-iron-garnet film structure, comprise Si substrate and the yttrium iron garnet thin film layer on it, between Si substrate and yttrium iron garnet thin film layer, also have CeO 2Transition layer.CeO 2Transition layer is for being coated on the Si substrate.
The present invention adopts equipment shown in Figure 1.The Yttrium-iron-garnet film structure preparation method is:
Step 1, at first pre-treatment is carried out on the surface of substrate, cleaning step is:
(1) with deionized water ultrasonic cleaning 15min;
(2) repeat (1);
(3) with acetone ultrasonic cleaning 15min;
(4) repeat (3);
(5) with the clear ultrasonic cleaning 15min of wine.
(6) repeat (5); (7) spend flushing of lot of pure water and oven dry.
Step 2, be fixed on cleaned substrate on the pallet and place on the sputtering unit of vacuum chamber.At first start mechanical pump, open low valve, open vacuumometer after two minutes; Treat that vacuum tightness reaches 2Pa when following, turn off low valve, open pre-valve, open turbomolecular pump after 5 minutes; When treating that the molecular pump frequency reaches 400Hz, open high valve, promptly begin pumping high vacuum.
Step 3, sputter CeO 2Transition layer: when vacuum tightness reaches 5 * 10 -4When Pa is following, open gas cylinder, open valve control switch, charge into argon gas, adjust under meter, make pressure maintain 7 * 10 -1Pa opens CeO 2The radio-frequency sputtering power source is adjusted coupling, and it is minimum that reflection is dropped to, and sees that the vacuum chamber build-up of luminance then illustrates and successfully begins sputter if see through glass port, carries out sputter with the power of 60W, stop after 20 minutes, this moment CeO 2The thickness of layer is about 15nm;
Step 4, be coated with the yttrium iron garnet film: same, open yttrium iron garnet radio-frequency sputtering power source, adjust coupling, it is minimum that reflection is dropped to, see that the vacuum chamber build-up of luminance then illustrates and successfully begin sputter if see through glass port, carry out sputter with the power of 90W, in order to prevent that substrate temperature is too high and to damage target, need in the sputter procedure every two hours to stop once, after 30 minutes, continue sputter again.After sputter finishes, close radio frequency power source, the shut-off valve control screws gas cylinder, turn off under meter, close high valve, press turbomolecular pump " OFF " switch, wait for its frequency reduce to zero after the closure molecule pumping source, close pre-valve, turn off vacuumometer, turn off mechanical pump, turn off master switch.
Step 5, the film that obtains by sputter are amorphous, must make its crystallization by anneal.The present invention adopts rta technique.The film of sputtering sedimentation put into handles stove, in vacuum tightness less than 10 -2The time, being warming up to certain assigned temperature, insulation for some time is in cooling, so that the film chemical composition, microstructure on surface etc. change, thereby reaches the purpose of improving property of thin film.
Membrane structure synoptic diagram such as Fig. 6 of preparation gained.61 is the Si substrate, and 62 is CeO 2Transition layer, 63 is the yttrium iron garnet thin film layer.
As seen from Figure 2, do not add the YIG film of transition layer, have amorphous phase to exist after the annealing crystallization; Had after the CeO2 transition layer, the crystallization state of film obviously improves, and crystallization is complete.
As seen from Figure 3, the YIG film surfaceness that does not have transition layer is obviously greater than the film that adds transition layer, and this is because the CeO2 transition layer has suppressed growing up of film crystal grain.
As seen from Figure 4, add after the transition layer, the saturation magnetization of YIG film and residual magnetization increase, and coercive force slightly descends simultaneously.
As seen from Figure 5, along with the increase of annealing atmosphere air pressure, the saturation magnetization of two kinds of films, residual magnetization and coercive force are all increasing.Under different annealing gas pressures, there are the saturation magnetization and the residual magnetization of the YIG film of transition layer to increase simultaneously than the film that does not have transition layer, on the contrary and coercitive result.

Claims (4)

1, Yttrium-iron-garnet film structure comprises Si substrate and the yttrium iron garnet thin film layer on it, it is characterized in that, also has CeO between Si substrate and yttrium iron garnet thin film layer 2Transition layer.
2, Yttrium-iron-garnet film structure as claimed in claim 1 is characterized in that, CeO 2Transition layer is for being coated on the Si substrate.
3, the Yttrium-iron-garnet film structure preparation method is characterized in that, may further comprise the steps:
The surface of step 1, cleaning Si substrate;
Step 2, cleaned Si substrate is placed vacuum chamber, vacuumize;
Step 3, on the Si substrate sputter CeO 2Transition layer;
Step 4, having CeO 2Sputter yttrium iron garnet film on the Si substrate of transition layer;
Step 5, anneal.
4, Yttrium-iron-garnet film structure preparation method as claimed in claim 3 is characterized in that, concrete steps are:
Step 1, at first pre-treatment is carried out on the surface of substrate, cleaning step is:
(1) uses the deionized water ultrasonic cleaning; (2) use the acetone ultrasonic cleaning; (3) with the clear ultrasonic cleaning of wine; (4) with purified rinse water and oven dry;
Step 2, cleaned substrate is placed on the sputtering unit of vacuum chamber pumping high vacuum.
Step 3, sputter CeO 2Transition layer: when vacuum tightness reaches 5 * 10 -4When Pa is following, charge into argon gas, make pressure maintain 7 * 10 -1Pa, sputter CeO 2
Step 4, be coated with the yttrium iron garnet film;
Step 5, anneal: the film of sputtering sedimentation put into handles stove, in vacuum tightness less than 10 -2The time, heat up insulation for some time postcooling.
CN2008100443023A 2008-04-28 2008-04-28 Yttrium-iron-garnet film structure and preparation method Expired - Fee Related CN101311374B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010075808A1 (en) * 2009-01-04 2010-07-08 上海舜宇海逸光电技术有限公司 Magneto-optic crystal, method of making the same, and application apparatus thereof
CN103526284A (en) * 2013-09-30 2014-01-22 西安交通大学 Ferrite niobate titanate or ferrite niobate epitaxial thin film, and preparation method and application thereof
CN103840081A (en) * 2014-03-19 2014-06-04 中国科学院微电子研究所 Non-volatilization resistance transformation type memorizer based on yttrium iron garnet and manufacturing method thereof
CN105331942A (en) * 2015-10-10 2016-02-17 中国科学院上海硅酸盐研究所 Yttrium iron garnet film material and preparing method thereof
CN105714379A (en) * 2016-02-26 2016-06-29 电子科技大学 Preparation method for directly growing highly-doped yttrium iron garnet film on silicon
CN106048726A (en) * 2016-07-04 2016-10-26 南京大学 Epitaxial growth method of yttrium iron garnet film
CN108239768A (en) * 2018-01-23 2018-07-03 河北工业大学 A kind of preparation method of Si bases yttrium iron garnet film
CN109164603A (en) * 2018-07-31 2019-01-08 电子科技大学 A method of low temperature on silicon is printed upon based on transfer and integrates garnet

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148753A (en) * 2007-10-10 2008-03-26 电子科技大学 Yttrium-iron garnet thin film material and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010075808A1 (en) * 2009-01-04 2010-07-08 上海舜宇海逸光电技术有限公司 Magneto-optic crystal, method of making the same, and application apparatus thereof
CN103526284A (en) * 2013-09-30 2014-01-22 西安交通大学 Ferrite niobate titanate or ferrite niobate epitaxial thin film, and preparation method and application thereof
CN103526284B (en) * 2013-09-30 2016-04-27 西安交通大学 A kind of titanium ferro-niobium hydrochlorate or ferro-niobium hydrochlorate epitaxial film and its preparation method and application
CN103840081A (en) * 2014-03-19 2014-06-04 中国科学院微电子研究所 Non-volatilization resistance transformation type memorizer based on yttrium iron garnet and manufacturing method thereof
CN103840081B (en) * 2014-03-19 2016-04-13 中国科学院微电子研究所 Based on the non-volatile resistor transition type memory and preparation method thereof of yttrium iron garnet
CN105331942A (en) * 2015-10-10 2016-02-17 中国科学院上海硅酸盐研究所 Yttrium iron garnet film material and preparing method thereof
CN105331942B (en) * 2015-10-10 2018-02-06 中国科学院上海硅酸盐研究所 Yttrium-iron garnet thin film material and preparation method thereof
CN105714379A (en) * 2016-02-26 2016-06-29 电子科技大学 Preparation method for directly growing highly-doped yttrium iron garnet film on silicon
CN105714379B (en) * 2016-02-26 2018-07-27 电子科技大学 The preparation method of highly doped yttrium iron garnet film is directly grown on a kind of silicon
CN106048726A (en) * 2016-07-04 2016-10-26 南京大学 Epitaxial growth method of yttrium iron garnet film
CN108239768A (en) * 2018-01-23 2018-07-03 河北工业大学 A kind of preparation method of Si bases yttrium iron garnet film
CN109164603A (en) * 2018-07-31 2019-01-08 电子科技大学 A method of low temperature on silicon is printed upon based on transfer and integrates garnet

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