CN111399255A - Chalcogenide phase change film for multispectral active optical regulation and control and preparation method thereof - Google Patents

Chalcogenide phase change film for multispectral active optical regulation and control and preparation method thereof Download PDF

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Publication number
CN111399255A
CN111399255A CN202010164514.6A CN202010164514A CN111399255A CN 111399255 A CN111399255 A CN 111399255A CN 202010164514 A CN202010164514 A CN 202010164514A CN 111399255 A CN111399255 A CN 111399255A
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phase change
film
change film
chalcogenide phase
heating
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张斌
杨泽林
李朝晖
曾平羊
夏迪
吴家越
孙耀东
宋景翠
朱莺
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Sun Yat Sen University
National Sun Yat Sen University
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    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/0147—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on thermo-optic effects
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/0009—Materials therefor
    • G02F1/009—Thermal properties

Abstract

The invention relates to a chalcogenide phase change film for multispectral active optical regulation and a preparation method thereof, belonging to the field of optical films and optical phase change materials. The component chemical formula of the phase change film is SbxS100‑x，20<x<50; the optical film is prepared by adopting a high-vacuum rapid thermal deposition method to obtain the amorphous high-quality optical film. The film can be reversibly transformed between a high refractive index (amorphous state) and a low refractive index (crystalline state) under the action of heat of an external field. The material film has a crystalline state in the range of 0.55-25 μm andthe amorphous state has obvious difference in refractive index and good light transmittance, can be used for preparing a multi-spectral-segment light field active regulating and controlling device, and is favorable for meeting the development requirements of integration, miniaturization and multiple functions of the traditional light field regulating and controlling device.

Description

Chalcogenide phase change film for multispectral active optical regulation and control and preparation method thereof
Technical Field
The invention belongs to the technical field of optical films and phase-change optical materials, and particularly relates to a chalcogenide phase-change film for multispectral active optical regulation and control and a preparation method thereof.
Background
With the explosive increase of people's demand for information capacity, the demand for new electronic components for mobile internet and internet of things technology increases remarkably. Particularly, the advance of 5G industry is facing to new industries, and new optoelectronic devices adopting new processes or new materials are gaining high attention from the industry and the scientific research community. In particular to the development requirements of miniaturization, integration and multi-functionalization of on-chip integrated optoelectronic devices. Based on the development requirements, how to realize the feeding of multiple paths of optical signals in a limited space and realize the processing of large-capacity information becomes a key for further promoting the development of on-chip integrated optoelectronic devices.
In recent years, nonvolatile phase change materials can exhibit both crystalline and amorphous states, and have a great contrast in refractive index and transmittance, and thus have been widely focused and studied in applications of optical switches, optical logic devices, and optical memory devices. Such as classical Ge2Sb2Te5Chalcogenide phase change materials, as a nonvolatile phase change material with excellent performance, have been widely researched and applied in the fields of information storage, all-optical signal processing, all-optical switches, and the like. However, due to the material groupThe transmission band of the material is limited to the middle infrared band which is larger than 2 microns, and the transmissivity is very low due to high absorption coefficient in the visible light and communication bands. This is not favorable for the preparation of optoelectronic integrated devices in the visible and communication bands. Therefore, how to design and prepare a novel phase-change material with optical working wave band capable of covering multiple spectrum bands and obvious optical property change before and after phase change can expand the application wave band of the phase-change material, and is the basis of the development demand of the optical field regulation device to integration, miniaturization and multiple functions.
Disclosure of Invention
The invention provides a chalcogenide phase change film for active optical control of multiple spectral bands and a preparation method thereof, aiming at overcoming the defects in the prior art, solving the problem that the current phase change material film is opaque in visible and near-infrared bands, and widening the transmission band of the traditional phase change material.
In order to solve the technical problems, the invention adopts the technical scheme that: a chalcogenide phase-change film for active optical regulation of multiple spectral bands is prepared from SbxS100-x，20<x is less than or equal to 50, the chalcogenide film has a crystalline state and an amorphous state, and the two states can be subjected to reversible transformation under the action of external field heat; the crystalline state and the amorphous state can present two refractive indexes within the range of 0.55-25 mu m, and the refractive index difference is more than or equal to 0.5. The film has good light transmission performance, and can be used for preparing an active regulation and control device for regulating and controlling a multi-spectral-band light field.
Preferably, x is 40, and the chemical composition of the chalcogenide thin film is Sb2S3。
The invention also provides a preparation method of the chalcogenide phase change film for active optical regulation of multiple spectral bands, which is characterized in that the obtained phase change material powder is deposited on a substrate by a high vacuum rapid thermal evaporation method to obtain an amorphous film, and the preparation method specifically comprises the following steps:
s1, preparing Sb in a quartz ampoule tube by a traditional melting-quenching methodxS100-x(20<x is less than or equal to 50), grinding the block into powder, and putting the powder into a heating boat of high vacuum evaporation equipment, wherein the particle size of the powder is not more than 200 mu m; lining a filmThe bottom is arranged on a rotating disc in the evaporation cavity at a height of 30-50cm away from the heating boat source, and cold water is introduced into the rotating disc to control the temperature to be less than or equal to 20 ℃;
s2, vacuumizing the cavity of the evaporation equipment to 10 DEG-6Pa, heating the evaporation boat to raise the temperature, setting the evaporation rate to be more than or equal to 10nm/min and keeping the evaporation rate stable, and rotating the rotating disc at a rotating speed of not less than 30 revolutions per minute;
s3, stopping heating after the thickness of the film reaches a preset value, and stopping rotating the rotating disc and controlling the temperature through water cooling; taking out the sample after the temperature of the cavity is cooled to room temperature to obtain the amorphous film of the chalcogenide phase change material; the obtained phase change film is changed into a crystalline state through the thermal action of the external field, and the reversible transformation of the phase change film between the crystalline state and the amorphous state is realized by repeating the action of the external field.
Preferably, the substrate comprises a flexible substrate and a hard substrate, and the flexible substrate comprises PMMA, PET; the hard substrate comprises silicon oxide, silicon and sapphire.
Preferably, the thickness of the prepared chalcogenide phase change film is 10nm to 1 um.
Preferably, the external field effect comprises heating plate heating, motor heating, laser pulse heating or electron beam heating.
Compared with the prior art, the beneficial effects are: the chalcogenide phase change film for active optical regulation of multispectral segments and the preparation method thereof provided by the invention have the advantages that the film can be reversibly transformed between a high refractive index (amorphous state) and a low refractive index (crystalline state) under the thermal action of an external field, the crystalline state and the amorphous state of the material have obvious difference in refractive index within the range of 0.55-25 mu m, the light transmittance is good, the material can be used for preparing an active regulation multispectral segment light field regulation device, the difficult problems of integration and miniaturization of the traditional light field regulation device in multispectral segment regulation application can be solved, and the development requirements of the on-chip light field regulation device on integration, multiple functions and miniaturization are met.
Drawings
FIG. 1 is a scanning electron microscope photograph of chalcogenide phase change thin films that can be used for active optical modulation of multiple bands according to the present invention.
FIG. 2 is a comparison of X-ray diffraction patterns before and after phase transition of the chalcogenide phase transition thin film for multi-spectral active optical control provided by the invention.
FIG. 3 is a comparison of the transmittance of the Ge-Sb-Se-Te chalcogenide phase-change film as a low-absorption phase-change material before and after phase change.
FIG. 4 is a comparison of the transmittance of the chalcogenide phase change film for multispectral active optical modulation before and after phase change.
FIG. 5 is a comparison of refractive indices of chalcogenide phase change films useful for multispectral active optical modulation before and after phase change.
Detailed Description
The drawings are for illustration purposes only and are not to be construed as limiting the invention; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted. The positional relationships depicted in the drawings are for illustrative purposes only and are not to be construed as limiting the invention.
Example 1:
the chemical general formula of the chalcogenide phase change film prepared in the embodiment and capable of being used for active optical control of multiple spectrums is SbxS100-xIn this example, x is 40.
Sb2S3The film is prepared by thermal evaporation method, and the vacuum degree is less than 10-6In a vacuum cabin body with pressure of Pa, a quartz substrate is placed on a sample loading table of a vacuum coating machine, and Sb is heated by a heating evaporation boat2S3The specific preparation method of the target glass comprises the following steps:
s1, preparing Sb in a quartz ampoule tube by a traditional melting-quenching method2S3Grinding the block into powder, and placing the powder into a heating boat of a high vacuum evaporation device, wherein the powder particles are not more than 200 mu m; placing the film substrate on a rotating disk in the evaporation cavity at a position 30-50cm away from the heating boat source, and introducing cold water into the rotating disk to control the temperature to be less than or equal to 20 ℃;
s2, evaporating platingThe equipment cavity is vacuumized to 10-6Pa, heating the evaporation boat to raise the temperature, setting the evaporation rate to be more than or equal to 10nm/min and keeping the evaporation rate stable, and rotating the rotating disc at a rotating speed of not less than 30 revolutions per minute;
s3, stopping heating after the thickness of the film reaches a preset value, and stopping rotating the rotating disc and controlling the temperature through water cooling; and taking out the sample after the temperature of the cavity is cooled to room temperature, enabling the obtained amorphous film of the chalcogenide phase change material to be changed into a crystalline state through the thermal action of an external field, and repeating the action of the external field to realize reversible transformation of the phase change film between the crystalline state and the amorphous state.
Sb of the above example 12S3Carry out the test
Referring to FIG. 1, from the photograph of the SEM, Sb for active optical modulation of multiple bands is obtained by the above steps2S3The chalcogenide phase change film has uniform thickness and smooth surface, which proves that the steps and parameter setting of the high vacuum rapid thermal deposition method are reasonable.
Referring to FIG. 2, Sb was heated with a hot plate under nitrogen2S3Heating the film at 300 deg.C for 30 min to obtain crystalline state, and obtaining Sb by X-ray diffraction2S3The X-ray diffraction pattern before and after the phase change of the film can show that Sb is heated for 30 minutes at 300 DEG C2S3The film already fully exhibits a crystalline phase, and thermal evaporation deposits Sb2S3The film has no obvious sharp diffraction peak and also indicates that Sb is deposited by thermal evaporation2S3The film is amorphous and can show Sb2S3The film can realize the conversion from the amorphous state to the crystalline state by heating, which also proves that the material can be used as an actively-controlled phase change device.
Referring to fig. 3, the transmittances of crystalline and amorphous Ge-Sb-Se-Te before and after phase change in a wavelength band of 550 nm to 2.5 μm are shown, as comparative data of the chalcogenide phase change thin film for active optical control in multiple spectral bands provided by the present invention, it can be found that the short-wave cut-off edge of the material red-shifts to 1 μm after phase change into crystalline, and the overall transmittance is also below 40%, such lower transmittance also leads to such difficulties as integration and miniaturization of the conventional optical field control device in the multiple spectral bands control application.
Please refer to fig. 4, which shows the crystalline and amorphous Sb before and after the phase change2S3The transmittance of the film in a 550 nm to 25 micron wave band is realized, wherein a substrate with the light transmission range of 2.5 to 25 micron wave band can not be selected, so that the Fresnel equation is utilized to simulate the material in the 2.5 to 25 micron wave band, the influence of in-film reflection is considered, the far infrared transmittance in the material is finally obtained, the short-wave cut-off edge of the material is 500 nm, the transmittance of more than 60 percent can be kept in the whole visible light and near infrared region before and after phase change, and the value has huge breakthrough compared with the conventional Ge-Sb-Se-Te phase change material with lower transmittance in the region, which means that Sb-Se-Te phase change material has huge breakthrough2S3The film breaks through the defect that the transmittance of the original phase change material Ge-Sb-Se-Te is lower in the region, so that the performance of the traditional phase change material can be improved, and the application range of the device is greatly expanded.
Please refer to fig. 5, which shows the crystalline and amorphous Sb before and after the phase change2S3The film utilizes the refractive index of a 550 nm to 25 micron wave band measured by an ellipsometer, wherein two ellipsometer detectors are used for detecting the refractive index, the working wavelengths of the two detectors are respectively 500 nm to 1.6 microns and 1.7 microns to 25 microns, according to test data, the refractive index difference of the phase-change material before and after phase change can be kept to be more than or equal to 0.5 and stable before and after the phase change in the whole transmission wave band, and the characteristic is favorable for the stability of the phase-change device before and after the phase change in the application of a plurality of wave bands.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. The chalcogenide phase change film for active optical control of multiple spectrums is characterized in that the chemical composition of the chalcogenide phase change film is SbxS100-x，20<x≤50。
2. The chalcogenide phase change film for active multi-spectral optical modulation according to claim 1, wherein the chalcogenide phase change film has a crystalline state and an amorphous state, and the two states can be reversibly transformed under the action of external field heat.
3. The chalcogenide phase change film for active multi-spectral optical modulation according to claim 2, wherein the crystalline state and the amorphous state of the chalcogenide phase change film can exhibit two refractive indexes in the range of 0.55 μm to 25 μm.
4. The chalcogenide phase change film for active optical modulation of multiple spectral bands according to claim 3, wherein the difference between the refractive indices of the chalcogenide phase change film is greater than or equal to 0.5.
5. The chalcogenide phase change film for active optical modulation of multiple spectral bands according to claim 4, wherein x is 40, and the chalcogenide phase change film has a chemical composition of Sb2S3。
6. A preparation method of a chalcogenide phase change film for multispectral active optical regulation is characterized in that obtained phase change material powder is deposited on a substrate through a high-vacuum rapid thermal evaporation method to obtain an amorphous film, and specifically comprises the following steps:
s1, preparing Sb in a quartz ampoule tube by a traditional melting-quenching methodxS100-x(20<x is less than or equal to 50), grinding the block into powder, and putting the powder into a heating boat of high vacuum evaporation equipment, wherein the particle size of the powder is not more than 200 mu m; placing the film substrate on a rotating disk in the evaporation chamber at a height of 30-50cm from the heating boat source, and introducing cold water into the rotating diskControlling the temperature to be less than or equal to 20 ℃;
s2, vacuumizing the cavity of the evaporation equipment to 10 DEG-6Pa, heating the evaporation boat to raise the temperature, setting the evaporation rate to be more than or equal to 10nm/min and keeping the evaporation rate stable, and rotating the rotating disc at a rotating speed of not less than 30 revolutions per minute;
s3, stopping heating after the thickness of the film reaches a preset value, and stopping rotating the rotating disc and controlling the temperature through water cooling; taking out the sample after the temperature of the cavity is cooled to room temperature to obtain the amorphous film of the chalcogenide phase change material; the obtained phase change film is changed into a crystalline state through the thermal action of the external field, and the reversible transformation of the phase change film between the crystalline state and the amorphous state is realized by repeating the action of the external field.
7. The method for preparing the chalcogenide phase change film for active optical modulation of multiple spectral bands according to claim 6, wherein the substrate comprises a flexible substrate and a hard substrate.
8. The method for preparing the chalcogenide phase change film for multispectral active optical modulation according to claim 7, wherein the flexible substrate comprises PMMA and PET.
9. The method according to claim 7, wherein the hard substrate comprises silicon oxide, silicon, or sapphire.
10. The method of claim 6, wherein the external field effect comprises heating with a heating plate, laser pulse heating, or electron beam heating.
CN202010164514.6A 2020-03-11 2020-03-11 Chalcogenide phase change film for multispectral active optical regulation and control and preparation method thereof Pending CN111399255A (en)

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Cited By (6)

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CN113075802A (en) * 2021-02-23 2021-07-06 华南师范大学 Based on phase change material Sb2S3Near infrared thermal modulation zooming super-structure lens
CN113724759A (en) * 2021-09-01 2021-11-30 哈尔滨工程大学 Optical fiber memristor unit based on evanescent field
CN113777807A (en) * 2021-09-07 2021-12-10 哈尔滨工程大学 Based on Ge2Sb2Te5Nonvolatile echo wall mode all-optical switch of phase change material and manufacturing method thereof
CN113969395A (en) * 2021-09-14 2022-01-25 上海交大平湖智能光电研究院 Preparation method of phase change film based on pulse laser deposition
CN115128843A (en) * 2022-07-26 2022-09-30 中山大学 Phase change material and manufacturing method thereof
CN115522164A (en) * 2022-10-25 2022-12-27 吉林大学 Programmable color super-surface device and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113075802A (en) * 2021-02-23 2021-07-06 华南师范大学 Based on phase change material Sb2S3Near infrared thermal modulation zooming super-structure lens
CN113724759A (en) * 2021-09-01 2021-11-30 哈尔滨工程大学 Optical fiber memristor unit based on evanescent field
CN113724759B (en) * 2021-09-01 2023-07-14 哈尔滨工程大学 Optical fiber memristor unit based on evanescent field
CN113777807A (en) * 2021-09-07 2021-12-10 哈尔滨工程大学 Based on Ge2Sb2Te5Nonvolatile echo wall mode all-optical switch of phase change material and manufacturing method thereof
CN113969395A (en) * 2021-09-14 2022-01-25 上海交大平湖智能光电研究院 Preparation method of phase change film based on pulse laser deposition
CN113969395B (en) * 2021-09-14 2023-09-08 上海交大平湖智能光电研究院 Preparation method of phase-change film based on pulse laser deposition
CN115128843A (en) * 2022-07-26 2022-09-30 中山大学 Phase change material and manufacturing method thereof
CN115522164A (en) * 2022-10-25 2022-12-27 吉林大学 Programmable color super-surface device and preparation method thereof
CN115522164B (en) * 2022-10-25 2024-03-01 吉林大学 Programmable color super-surface device and preparation method thereof

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Application publication date: 20200710