CN102212782A - Quick thermal treatment method for preparing vanadium dioxide film - Google Patents
Quick thermal treatment method for preparing vanadium dioxide film Download PDFInfo
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- CN102212782A CN102212782A CN 201110136230 CN201110136230A CN102212782A CN 102212782 A CN102212782 A CN 102212782A CN 201110136230 CN201110136230 CN 201110136230 CN 201110136230 A CN201110136230 A CN 201110136230A CN 102212782 A CN102212782 A CN 102212782A
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Abstract
The invention discloses a quick thermal treatment method for preparing a vanadium dioxide film. The method comprises the following steps of: (1) cutting a silicon chip to form a substrate, and cleaning and drying the silicon substrate; (2) placing the silicon substrate of the step (1) in a vacuum chamber, and depositing a vanadium dioxide film on the silicon substrate by adopting a target magnetron sputtering method, wherein the target is 99.99 percent metallic vanadium, argon is used as a working gas and oxygen is used as a reaction gas; (3) putting the vanadium dioxide film product sputtered in the step (2) into a quick annealing furnace to prepare a vanadium dioxide film, wherein the annealing temperature is 500 to 550 DEG C, the heating rate is 50 DEG C per second, the heat preservation time is 10 to 30 seconds, cooling is performed within 3 minutes, and the protective gas is nitrogen; and (4) measuring. By the method, the thermal treatment time is shortened, and obvious phase change property can be obtained after the vanadium dioxide film product is quickly and thermally treated for 10 to 30 seconds; the method is simple in process control, high in repeatability and suitable for large-area production; and electric and optical properties of the vanadium dioxide film are optimized. The method is widely applied in the fields of infrared detectors, memories, optical communications and the like.
Description
Technical field
It is heat treated to the invention relates to film, relates in particular to the quick heat treatment method of vanadium oxide film.
Background technology
Vanadium dioxide is a kind of temperature-sensitive and photochromics.Vanadium dioxide is the monocline rutile structure when low temperature; Change cubic rutile structure during high temperature into, transformation temperature is 68 ℃.The resistivity of vanadium dioxide, susceptibility and all reversible mutation can take place near transformation temperature to optical transmission rate etc.Because vanadium dioxide has these characteristics, it has a wide range of applications at aspects such as infrared eye, storer, optical communication and smart window.
The method for preparing vanadium dioxide film mainly contains magnetron sputtering method, method of evaporation, sol-gel method and pulsed laser deposition.The vanadium dioxide sample that obtains need just can have phase-change characteristic through Overheating Treatment.Because the tetravalence vanadium is a valence state in the middle of, process window is very narrow in preparation process, so preparation process need accurately control processing condition, could obtain the vanadium oxide film based on the tetravalence vanadium.Vanadium oxide without Overheating Treatment does not possess phase-change characteristic.
At present, domestic mainly is to adopt nitrogen protection thermal treatment and these two kinds of conventional heat treating methods of vacuum heat treatment, and these two kinds of heat treating methods need spend a few hours in intensification, insulation and temperature-fall period, and vacuum heat treatment also needs spended time to vacuumize.
Rapid thermal process is a kind of heat treating method efficiently.Because heating mechanism is different, the short annealing device can be heated to nearly thousand degrees centigrade with sample in the several seconds, and heat-up rate is exceedingly fast.Simultaneously the thermal treatment soaking time is also very short, generally all in several minutes, and short then several seconds.Process time and cycle have been shortened greatly.
The Technology that adopts the rapid thermal process method to handle vanadium dioxide film and obtain its phase-change characteristic does not also have report.
Summary of the invention
The heat treating method fast and efficiently that the purpose of this invention is to provide a kind of vanadium dioxide film, thus optimize the purpose that vanadium dioxide film crystallization and composition improve its electricity and optical property, shortening heat treatment time and process cycle, efficient energy-saving to reach.
The present invention is achieved by following technical solution.
Have following steps:
(1) silicon chip is cut into the substrate of regulation shape, be soaked in the dehydrated alcohol, ultrasonic cleaning 10 minutes is rinsed well with deionized water again, oven dry;
(2) cleaned silicon substrate in the step (1) is placed vacuum chamber, adopt facing-target magnetron sputtering system method deposit one deck vanadium oxide film on the silicon substrate of cleaning; Used target is that quality purity is 99.99% vanadium metal, takes out body vacuum to 2.5 * 10
-4Pa; Feeding argon gas and oxygen, is working gas with the argon gas, is reactant gases with oxygen, and argon gas and oxygen flow are respectively 30-55sccm and 0.8-1.3sccm; Begin sputter when regulating operating pressure to 1.0-2.0Pa, sputtering time is 10-30 minute;
(3) step (2) sputter is intact vanadium oxide film goods are put in the quick anneal oven, it is 500 ℃-550 ℃ that annealing temperature is set, temperature rise rate is 50 ℃/s, soaking time 10-30s, temperature fall time is in 3 minutes, and shielding gas is a nitrogen, and nitrogen flow is 10slpm during cooling, nitrogen flow is 3slpm when intensification and insulation, makes vanadium dioxide film;
(4) measure goods temperature coefficient of resistance and Terahertz transmitance.
The substrate dimension of described step (1) is the square substrate of 2cm * 2cm.
The deposit vanadium oxide film of described step (2) adopts DPS-III type ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment.
The argon gas of described step (2) and the quality purity of oxygen are 99.999%.
The AG610 type quick anneal oven that the annealing furnace of described step (3) adopts Allwin21 corp.USA company to produce.
The quality purity of the nitrogen of described step (3) is 99.999%.
The invention has the beneficial effects as follows, a kind of heat treating method fast and efficiently of vanadium dioxide film is provided, shortened heat treatment period greatly, can obtain tangible phase-change characteristic vanadium dioxide film goods rapid thermal process 10-30s (soaking time); Technology controlling and process is simple repeatable high, is applicable to big area production, has obtained optimization under the electricity of vanadium dioxide film and the optical property rapid thermal process condition simultaneously.
Description of drawings
Fig. 1 is the resistance-temperature curve of embodiment 1;
Fig. 2 is the Terahertz transmittance curve of embodiment 1;
Fig. 3 is the resistance-temperature curve of embodiment 2;
Fig. 4 is the Terahertz transmittance curve of embodiment 2;
Fig. 5 is embodiment 3 sample resistance-temperature curves;
Fig. 6 is the Terahertz transmittance curve of embodiment 3.
Embodiment
Below by specific embodiment the present invention is further described.
(1) silicon chip is cut into the square substrate that is of a size of 2cm * 2cm, be soaked in dehydrated alcohol, ultrasonic cleaning 10 minutes is rinsed well with deionized water again, oven dry;
(2) silicon substrate cleaned in the step 1) is placed vacuum chamber, take out body vacuum to 2.5 * 10
-4Pa.Feed argon gas and oxygen, argon gas and oxygen flow are respectively 30sccm and 0.8sccm; Begin sputter when regulating operating pressure to 1.0Pa, sputtering time is 15 minutes;
(3) with step 2) sample puts in the quick anneal oven, and it is 500 ℃ that annealing temperature is set; Temperature rise rate is 50 ℃/s; Soaking time 10s.Shielding gas nitrogen during cooling (quality purity is 99.999%) flow is 10slpm, and nitrogen flow is 3slpm when intensification and insulation;
(4) measure this sample temperature coefficient of resistance (TCR) and Terahertz transmitance, as Fig. 1 and Fig. 2.As can be seen from the figure vanadium dioxide film has modulating action to THz wave before and after having had tangible phase-change characteristic and phase transformation, and promptly Terahertz baud transmitance obviously reduces during high temperature.
Operation steps is with embodiment 1, and the processing condition correspondence changes to: argon gas and oxygen flow are respectively 55sccm and 1.3sccm; Operating pressure is to 2.0Pa; Sputtering time 30 minutes; 550 ℃ of annealing temperatures, soaking time 30s.
Measure this sample temperature coefficient of resistance (TCR) and Terahertz transmittance curve, as Fig. 3 and Fig. 4.As can be seen from the figure obviously to move to low temperature be 47 ℃ to transformation temperature, more near room temperature.Generally could realize the reduction of transformation temperature, just can realize by change rapid thermal process condition now by vanadium dioxide is mixed.
Implement real 3
Operation steps is with embodiment 1, and the processing condition correspondence changes to: argon gas and oxygen flow are respectively 48sccm and 1.2sccm; Operating pressure is to 2.0Pa; Sputtering time 15 minutes; 500 ℃ of annealing temperatures, soaking time 15s.
Measure this sample temperature coefficient of resistance (TCR) and Terahertz transmittance curve, as Fig. 5 and Fig. 6.
Claims (6)
1. one kind prepares vanadium dioxide film quick heat treatment method, has following steps:
(1) silicon chip is cut into the substrate of regulation shape, be soaked in the dehydrated alcohol, ultrasonic cleaning 10 minutes is rinsed well with deionized water again, oven dry;
(2) cleaned silicon substrate in the step (1) is placed vacuum chamber, adopt facing-target magnetron sputtering system method deposit one deck vanadium oxide film on the silicon substrate of cleaning; Used target is that quality purity is 99.99% vanadium metal, takes out body vacuum to 2.5 * 10
-4Pa; Feeding argon gas and oxygen, is working gas with the argon gas, is reactant gases with oxygen, and argon gas and oxygen flow are respectively 30-55sccm and 0.8-1.3sccm; Begin sputter when regulating operating pressure to 1.0-2.0Pa, sputtering time is 10-30 minute;
(3) step (2) sputter is intact vanadium oxide film goods are put in the quick anneal oven, it is 500 ℃-550 ℃ that annealing temperature is set, temperature rise rate is 50 ℃/s, soaking time 10-30s, temperature fall time is in 3 minutes, and shielding gas is a nitrogen, and nitrogen flow is 10slpm during cooling, nitrogen flow is 3slpm when intensification and insulation, makes vanadium dioxide film;
(4) measure goods temperature coefficient of resistance and Terahertz transmitance.
2. according to the preparation vanadium dioxide film quick heat treatment method of claim 1, it is characterized in that the substrate dimension of described step (1) is the square substrate of 2cm * 2cm.
3. according to the preparation vanadium dioxide film quick heat treatment method of claim 1, it is characterized in that the deposit vanadium oxide film of described step (2) adopts DPS-III type ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment.
4. according to the preparation vanadium dioxide film quick heat treatment method of claim 1, it is characterized in that the argon gas of described step (2) and the quality purity of oxygen are 99.999%.
5. according to the preparation vanadium dioxide film quick heat treatment method of claim 1, it is characterized in that the AG610 type quick anneal oven that the annealing furnace of described step (3) adopts Allwin21 corp.USA company to produce.
6. according to the preparation vanadium dioxide film quick heat treatment method of claim 1, it is characterized in that the quality purity of the nitrogen of described step (3) is 99.999%.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732847A (en) * | 2012-06-18 | 2012-10-17 | 天津大学 | Phase change vanadium dioxide film prepared by rapid thermal oxidation method |
| CN102912308A (en) * | 2012-10-25 | 2013-02-06 | 深圳大学 | Process for manufacturing vanadium dioxide thin film with low phase-transition temperature |
| CN103361614A (en) * | 2013-06-29 | 2013-10-23 | 天津大学 | Method for preparing Terahertz modulator film material based on flexible substrate |
| CN103882399A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Preparation method of flexible substrate based nano vanadium oxide functional film with phase transition characteristic |
| CN104914211A (en) * | 2015-04-10 | 2015-09-16 | 天津大学 | Preparation method of particle and short rod-like vanadium oxide film |
| CN105256280A (en) * | 2015-11-24 | 2016-01-20 | 天津大学 | Method for regulating and controlling phase transition temperature of vanadium dioxide through fast heat treatment |
| CN106048532A (en) * | 2016-06-17 | 2016-10-26 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for vanadium dioxide nano-particle film |
| CN104611670B (en) * | 2015-01-21 | 2017-04-12 | 中国科学院半导体研究所 | Preparation method of vanadium oxide film with high resistance temperature coefficient |
| CN109207927A (en) * | 2018-11-20 | 2019-01-15 | 中国科学技术大学 | A kind of preparation method of vanadium oxide monocrystal thin films |
| CN110791740A (en) * | 2019-12-02 | 2020-02-14 | 武汉理工大学 | Preparation method of high-performance ZIF-L/vanadium dioxide composite film |
| CN114059032A (en) * | 2021-11-18 | 2022-02-18 | 吉林大学 | Preparation method of vanadium dioxide film |
| CN114772546A (en) * | 2022-04-13 | 2022-07-22 | 成都市精鹰光电技术有限责任公司 | Method for improving contact between vanadium oxide and titanium electrode in microbolometer |
| CN117026193A (en) * | 2023-09-07 | 2023-11-10 | 无锡尚积半导体科技有限公司 | High-phase-change-performance vanadium dioxide film and preparation method thereof |
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| CN1598040A (en) * | 2004-08-25 | 2005-03-23 | 华中科技大学 | Process for preparing vanadium oxide film capable of regulating phase change temp. |
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| CN101174671A (en) * | 2007-10-18 | 2008-05-07 | 天津大学 | Production method for vanadium dioxide nano thin film with phase-change characteristic |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732847A (en) * | 2012-06-18 | 2012-10-17 | 天津大学 | Phase change vanadium dioxide film prepared by rapid thermal oxidation method |
| CN102912308A (en) * | 2012-10-25 | 2013-02-06 | 深圳大学 | Process for manufacturing vanadium dioxide thin film with low phase-transition temperature |
| CN102912308B (en) * | 2012-10-25 | 2014-07-09 | 深圳大学 | Process for manufacturing vanadium dioxide thin film with low phase-transition temperature |
| CN103361614A (en) * | 2013-06-29 | 2013-10-23 | 天津大学 | Method for preparing Terahertz modulator film material based on flexible substrate |
| CN103882399A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Preparation method of flexible substrate based nano vanadium oxide functional film with phase transition characteristic |
| CN104611670B (en) * | 2015-01-21 | 2017-04-12 | 中国科学院半导体研究所 | Preparation method of vanadium oxide film with high resistance temperature coefficient |
| CN104914211A (en) * | 2015-04-10 | 2015-09-16 | 天津大学 | Preparation method of particle and short rod-like vanadium oxide film |
| CN105256280A (en) * | 2015-11-24 | 2016-01-20 | 天津大学 | Method for regulating and controlling phase transition temperature of vanadium dioxide through fast heat treatment |
| CN106048532A (en) * | 2016-06-17 | 2016-10-26 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for vanadium dioxide nano-particle film |
| CN106048532B (en) * | 2016-06-17 | 2018-08-03 | 中国航空工业集团公司北京航空材料研究院 | A kind of preparation method of vanadium dioxide nano membrana granulosa |
| CN109207927A (en) * | 2018-11-20 | 2019-01-15 | 中国科学技术大学 | A kind of preparation method of vanadium oxide monocrystal thin films |
| CN109207927B (en) * | 2018-11-20 | 2020-05-19 | 中国科学技术大学 | Preparation method of vanadium oxide single crystal film |
| CN110791740A (en) * | 2019-12-02 | 2020-02-14 | 武汉理工大学 | Preparation method of high-performance ZIF-L/vanadium dioxide composite film |
| CN110791740B (en) * | 2019-12-02 | 2021-08-24 | 武汉理工大学 | Preparation method of high-performance ZIF-L/vanadium dioxide composite film |
| CN114059032A (en) * | 2021-11-18 | 2022-02-18 | 吉林大学 | Preparation method of vanadium dioxide film |
| CN114772546A (en) * | 2022-04-13 | 2022-07-22 | 成都市精鹰光电技术有限责任公司 | Method for improving contact between vanadium oxide and titanium electrode in microbolometer |
| CN117026193A (en) * | 2023-09-07 | 2023-11-10 | 无锡尚积半导体科技有限公司 | High-phase-change-performance vanadium dioxide film and preparation method thereof |
| CN117026193B (en) * | 2023-09-07 | 2024-09-24 | 无锡尚积半导体科技有限公司 | High-phase-change-performance vanadium dioxide film and preparation method thereof |
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Application publication date: 20111012 |