CN106498352A - Doping yttrium iron garnet film pulse laser sediment method based on quartz substrate - Google Patents
Doping yttrium iron garnet film pulse laser sediment method based on quartz substrate Download PDFInfo
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- CN106498352A CN106498352A CN201611014033.7A CN201611014033A CN106498352A CN 106498352 A CN106498352 A CN 106498352A CN 201611014033 A CN201611014033 A CN 201611014033A CN 106498352 A CN106498352 A CN 106498352A
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- pulse laser
- method based
- yttrium iron
- quartz substrate
- iron garnet
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
Abstract
The invention belongs to magnetic oxide film growth techniques field, and in particular to a kind of doping yttrium iron garnet film pulse laser sediment method based on quartz substrate.The present invention presses the parameters such as 5 10Pas, laser frequency 2 10Hz, deposition rear film annealing temperature 700 850 DEG C and temperature retention time 10 30min with basal spacing from 4 8cm, 550 DEG C 750 DEG C of base reservoir temperature, oxygen by controlling target, can prepare the magneto-optic thin film of high-quality.In the optical communicating waveband of 1550nm, in SiO2The CeYIG film faraday anglecs of rotation of deposition on substrate can reach 1deg/ μm, meet requirement of the high-performance optical isolator to the high magneto-optical property of material, significant to the development for promoting integrated thin-film type optics.
Description
Technical field
The invention belongs to magnetic oxide film growth techniques field, and in particular to the doping yttrium iron stone based on quartz substrate
Garnet film pulse laser sediment method.
Background technology
Pulsed laser deposition（PLD）A kind of processes of physical vapor deposition, with flexibility high, material ranges are wide, deposition
The advantages of efficiency high, increasingly paid attention to by everybody.Compared with other film deposition techniques, PLD technology has incomparable
Advantage：First, laser energy is very high, it is possible to achieve conversion of most of material by target to film, it might even be possible to low
Growing film under the conditions of temperature；Secondly, the plasma that laser is produced after target material surface is reached can occur anti-with atmosphere in chamber
Should, by introducing atmosphere and adjusting the stoichiometric proportion that air pressure can control film composition；Finally, can select within the chamber same
When multiple targets are installed, not only facilitate a step deposition plural layers but also heterogeneity ratio can be studied to film performance and knot
The impact of structure.These advantages cause PLD before preparation and the research field of magnetic oxide thin-film material have wide application
Scape.
In recent years, with devices such as the development of optic communication, electric power, medical treatment and laser industry, optoisolator and magneto-optical sensors
Part causes lasting concern.Optoisolator and magneto-optic sensing can be made using the magneto-optic memory technique with Faraday effect
Device.Wherein, yttrium iron garnet（YIG）Thin-film material due to small volume, saturation magnetization be high, the low advantage of coercivity into
For studying one of widest magneto-optic memory technique.Although pure YIG film has certain Faraday effect, coefficient of rotary
The less requirement for being difficult to meet device.CeYIG thin-film materials have huge magnetic Faraday effect, and temperature stability is more preferably, thus
Become the optimal thin-film material for making the nonreciprocal waveguide device of high-performance, optoisolator and magneto-optical sensor.
At present, discrete block optoisolator is remained in the practical optoisolator of optical communication field.By contrast,
Integrated film-type optoisolator on semi-conductor silicon chip, little with size, it is easy to integrated, required applied field strengths are little, envelope
The advantage such as simple is filled, becomes the research direction of domestic and international integrated optical device.However, due to the lattice between Si and CeYIG normal
Number mismatches are larger, and the CeYIG film cracks so as to cause to grow in Si substrates are more, and degree of crystallinity is low, magnetic property and magneto-optic
Can be poor, constrain its application in integrated optical device.
Quartz（SiO2）Can be grown on a si substrate, with good chemical stability and electric insulation by multiple methods
Property.Good optical property can be had based on the waveguide of quartz, and cheap, it is to realize the one of integrated optical device in future
The application direction of individual great potential.In past document report, research is concentrated mainly on gallium gadolinium garnet substrate, process for sapphire-based
Garnet magneto-optic thin film is prepared on piece, and considerably less to preparing the research of CeYIG films based on quartz substrate.Therefore, develop
Prepare in amorphous quartz substrate and have the CeYIG thin film preparation processes of high Figure of merit high performance integrated for preparing
Optoisolator tool is of great significance.
Content of the invention
For above-mentioned problem, the present invention proposes the doping yttrium iron garnet film pulse based on quartz substrate and swashs
Light deposition method, with solve low in the integrated doping yttrium iron garnet film crystal unity of silicon base, magnetic property and magneto-optical property poor
Problem, be that the practical offer material of integrated thin-film type optics is supported.
Doping yttrium iron garnet film pulse laser sediment method based on quartz substrate of the present invention, including following
Step：
Step one：Cleaning substrate；
Step 2：Substrate and target are placed in vacuum chamber, are vacuumized；
Step 3：Substrate is heated, and is filled with atmosphere adjusting gas flow and pressure；
Step 4：Sputter-deposited thin films on substrate；
Step 5：Annealing film.
Specifically, in the step one, cleaning substrate is SiO2, adopt acetone, isopropanol, deionized water, anhydrous second successively
Alcohol is cleaned by ultrasonic 10-15min in Ultrasound Instrument, after the completion of cleaning, is dried up with nitrogen in dustless interior rapidly.
In the step 2, target is CeYIG targets, by cleaned SiO2Substrate is placed on sample stage center, during operation
Note disposable glove to be worn, it is to avoid bring greasy dirt and dust pollution substrate and target into.Successively will using mechanical pump and molecular pump
In vacuum room, vacuum is extracted into 10-4Below Pa, it is that 4-8cm is uniform to ensure film forming to adjust target with the distance of substrate.
In the step 3, SiO is controlled2The temperature of substrate is 550 DEG C -750 DEG C, and temperature is low or too high is all unfavorable for film
Crystallization and epitaxial growth.Atmosphere is filled with for O2, oxygen pressure select between 5-10Pa, for keeping composition in CeYIG films
Stoicheiometry, and reduce the kinetic energy of the beam-plasma that target material surface is excited.
In the step 4, range of laser energy is from 160mJ to 320mJ.The too low film deposition rate of energy is slow and crystallizes
Degree is bad, and energy is too high, easily forms island structure, membrane thickness unevenness in film.Laser frequency is 2-10Hz, high laser frequency
It is difficult in SiO2CeYIG films are deposited in substrate.
In the step 5, CeYIG films are mainly amorphous state through above-mentioned deposition, anneal for the crystallization of film is weighed very much
Will.Sample is made annealing treatment after taking out.Annealing atmosphere selects air, argon gas or hydrogen.Annealing Crystallization temperature is 700-850
DEG C, temperature retention time 10-30min.
A kind of doping yttrium iron garnet film pulse laser sediment method based on quartz substrate of the present invention, passes through
Control target and basal spacing from, depositing temperature, atmospheric condition, laser energy, laser frequency, deposition rear film annealing temperature and
The parameters such as time, can prepare the magneto-optic thin film of high-quality.In the optical communicating waveband of 1550nm, in SiO2Deposition on substrate
The Faraday rotation angle of CeYIG films reaches 1deg/ μm, meets requirement of the optoisolator to the high magneto-optical property of material, Ke Yishi
Its application in integrated thin-film type optics existing.
Description of the drawings
Fig. 1 is the preparation technology flow chart of the present invention；
Fig. 2 is PLD system schematics；
Wherein, including KFr excimer lasers 1, lens 2, quartz window 3, target position 4, observation window 5, substrate warm table 6；
Fig. 3 is difference SiO2The XRD of CeYIG films is deposited under substrate heating-up temperature；
Fig. 4 is different component CeYIG targets（CexY3-xFe5O12, x=0.1,0.5,1）, deposit the hysteresis curve of CeYIG films
Figure；
Fig. 5 is the Faraday curve map of film CeYIG films under the conditions of different annealing temperature, the 10min that anneals；
Fig. 6 is the Faraday curve map of gained CeYIG films under 800 DEG C of annealing temperatures in different annealing times.
Specific embodiment
Specific embodiment one：The described doping yttrium iron garnet film pulse laser based on quartz substrate of this enforcement sinks
Product method, referring to Fig. 1 and Fig. 2, comprises the following steps：
Step one：Cleaning SiO2Substrate；
Step 2：Cleaned quartz substrate is dried up and successively vacuum chamber is placed in CeYIG targets, vacuumize；
Step 3：Substrate is heated, and is filled with atmosphere adjusting gas flow and pressure；
Step 4：Sputtering sedimentation CeYIG films on quartz substrate；
Step 5：Annealing CeYIG films.
Specific embodiment two：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, and in present embodiment, cleans SiO2Substrate, adopts third successively
Ketone, isopropanol, deionized water, absolute ethyl alcohol are cleaned by ultrasonic 10-15min in Ultrasound Instrument.
Specific embodiment three：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, and in present embodiment, in vacuum room, vacuum is 10-4Pa with
Under, target is 4-8cm with the distance of substrate.
Specific embodiment four：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, and in present embodiment, reacting gas is O2, oxygen pressure 5-10Pa.
Specific embodiment five：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, in present embodiment, range of laser energy from 160mJ to
320mJ, laser frequency are 2-10Hz.
Specific embodiment six：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, and in present embodiment, annealing atmosphere selects air, argon gas or hydrogen
Gas.
Specific embodiment seven：Present embodiment is to the doping yttrium iron based on quartz substrate described in specific embodiment one
Garnet pulse laser sediment method is described further, and in present embodiment, annealing temperature is 700-850 DEG C, annealing
Time is 10-30min.
Accompanying drawing 3,4,5,6 is used for one embodiment of the present of invention is described.
Fig. 3 is difference SiO2Substrate heating-up temperature deposits the XRD of CeYIG films.As seen from the figure, substrate heating-up temperature exists
When 550 DEG C and 750 DEG C, film all occurs in that the diffraction maximum of garnet crystalline phase, and at a high temperature of 750 DEG C film degree of crystallinity more
Good.
Fig. 4 is different component CeYIG targets（CexY3-xFe5O12, x=0.1,0.5,1）, deposit the magnetic hysteresis time of CeYIG films
Line chart.The saturation magnetization of the CeYIG films of the gained of x=0.1,0.5,1 be respectively 159emu/cc, 180emu/cc and
142emu/cc, coercivity are respectively 26Oe, 18Oe and 35Oe.
Fig. 5 is the Faraday curve map of film CeYIG films under the conditions of different annealing temperature, the 10min that anneals.By
Figure understands, when annealing temperature is 700 DEG C and 850 DEG C, the saturation faraday anglec of rotation of CeYIG films is respectively 0.4deg/ μm
With 0.8deg/ μm.
Fig. 6 is the Faraday curve map of gained CeYIG films under 800 DEG C of annealing temperatures in different annealing times.By
Figure understands that the saturation faraday anglec of rotation of CeYIG films is respectively 1.0deg/ μm when annealing time is respectively 10min, 30min
With 0.8deg/ μm.
From above-described embodiment, ceramic and thin compared to YIG by the quartzy base CeYIG films prepared by the present invention
Film, have the advantages that saturation magnetization big, coercivity is low, bigger than Faraday rotation angle, can be applicable to make high performance collection
Into optoisolator.
Claims (10)
1. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate, it is characterised in that including following step
Suddenly：
Step one：Cleaning substrate；
Step 2：Substrate and target are placed in vacuum chamber, are vacuumized；
Step 3：Substrate is heated, and is filled with atmosphere adjusting gas flow and pressure；
Step 4：Sputter-deposited thin films on substrate；
Step 5：Annealing film.
2. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, in step one, substrate for use is SiO2.
3. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, in step one, is cleaned by ultrasonic SiO2Substrate adopts acetone, isopropanol, deionized water, absolute ethyl alcohol successively, and ultrasound is clear
The time of washing is respectively 10-15min.
4. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, the target described in step 2 is CeYIG targets, meets chemical formula CexY3-xFe5O12, 0.1≤x≤1, x are Ce3+From
Sub- content.
5. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, the distance between target and substrate are 4-8cm.
6. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, the SiO described in step 32The temperature of substrate is 550 DEG C -750 DEG C.
7. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
Be characterised by, atmosphere is filled with described in step 3 for O2, oxygen pressure selection is between 5-10Pa.
8. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, from 160mJ to 320mJ, laser frequency is 2-10Hz to range of laser energy.
9. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, in step 5, annealing atmosphere selects air, argon gas or hydrogen.
10. the doping yttrium iron garnet film pulse laser sediment method based on quartz substrate according to claim 1, its
It is characterised by, in step 5, Annealing Crystallization temperature is 700-850 DEG C, temperature retention time 10-30min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190321A (en) * | 2017-05-11 | 2017-09-22 | 电子科技大学 | Nonreciprocal spin wave hetero-junctions waveguide material and its production and use |
| CN110904411A (en) * | 2019-12-13 | 2020-03-24 | 河北环亚线缆有限公司 | Method for manufacturing superconducting cable conductor film |
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| CN101148753A (en) * | 2007-10-10 | 2008-03-26 | 电子科技大学 | Yttrium-iron garnet thin film material and preparation method thereof |
| CN104988470A (en) * | 2015-07-30 | 2015-10-21 | 哈尔滨工业大学 | Method for depositing multilayer magneto-optical films through one-step pulse laser |
| 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 |
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2016
- 2016-11-18 CN CN201611014033.7A patent/CN106498352A/en active Pending
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| CN101148753A (en) * | 2007-10-10 | 2008-03-26 | 电子科技大学 | Yttrium-iron garnet thin film material and preparation method thereof |
| CN104988470A (en) * | 2015-07-30 | 2015-10-21 | 哈尔滨工业大学 | Method for depositing multilayer magneto-optical films through one-step pulse laser |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190321A (en) * | 2017-05-11 | 2017-09-22 | 电子科技大学 | Nonreciprocal spin wave hetero-junctions waveguide material and its production and use |
| CN110904411A (en) * | 2019-12-13 | 2020-03-24 | 河北环亚线缆有限公司 | Method for manufacturing superconducting cable conductor film |
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