CN103361614A - Method for preparing Terahertz modulator film material based on flexible substrate - Google Patents
Method for preparing Terahertz modulator film material based on flexible substrate Download PDFInfo
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- CN103361614A CN103361614A CN2013102723617A CN201310272361A CN103361614A CN 103361614 A CN103361614 A CN 103361614A CN 2013102723617 A CN2013102723617 A CN 2013102723617A CN 201310272361 A CN201310272361 A CN 201310272361A CN 103361614 A CN103361614 A CN 103361614A
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Abstract
The invention discloses a method for preparing a Terahertz modulator film material based on a flexible substrate. The method comprises the following steps of: cleaning polyimide used as a flexible substrate and depositing a vanadium metal nano-film with the thickness of 50-300nm on the surface of he flexible substrate; performing rapid heat treatment on the vanadium metal nano-film, thereby forming a vanadium metal film with the thickness of 100-600nm. By means of laser excitation, modulation of Terahertz waves is realized by changing properties of the material, the operability of the modulator film material on the flexible substrate is realized, and an application basis is provided for a novel flexible substrate integrated circuit device.
Description
Technical field
The present invention relates to the semiconductor microelectronics technical field, be specifically related to a kind of preparation method of the Terahertz modulator mould material based on flexible substrates.
Background technology
Terahertz (THz) ripple (frequency is positioned at the hertzian wave of 0.1～10THz wave band) is in the specific position between millimeter wave and the infrared rays, is last the empty frequency range in the electromagnetic spectrum.All has potential application at aspects such as short-distance wireless communication, bio-sensing, medical diagnosis, material behavior spectral detection and non-damage type detections.Promote further developing and practical application of Terahertz Technology, not only to solve well reliable and stable THz source, the THz detector of highly sensitive high s/n ratio, also need simultaneously to provide the Terahertz functional device of high-performance, high integration, cheapness, such as new function devices such as THz polarization, beam splitting, filtering, switch, modulation.
Yet THz communication technology is not the transplanting of the technology of micro-wave communication or optical communication, has very many novel characteristics.Existing optics and electron device are difficult to directly Terahertz be transmitted control.The shortage of Terahertz materials and devices has seriously restricted the practical developing direction of Terahertz Technology, becomes one of key issue that the Terahertz field needs to be resolved hurrily.Especially the modulation device of Terahertz communication all greatly differs from each other with microwave and lightwave communication technology in structure, size, performance and mode of operation, needs new development.U.S. Los Alamos National Laboratory has proposed a kind of Terahertz modulation device based on metal mold electromagnetism metamaterial.This device is to make up the metal electric magnetic resonance unit at Si or GaAs semiconductor substrate, thereby changes the Terahertz resonance amplitude that the semiconductor substrate carrier concentration affects the electromagentic resonance unit by extra electric field, realizes the modulation to the THz wave transmission signal.[H.T.Chen,et?al,Nature,444,597-600,(2006)]。(CN101943803A) employing as substrate, utilizes vanadium dioxide film to make the electromagentic resonance array to the dielectric material silica glass of THz wave highly transparent, realizes the modulation to terahertz signal.(CN102393571A) silicon photonic crystal post array surface plating one deck vanadium dioxide film of linear defect wave-guide is being arranged, utilize the medium of the phase-change characteristic of vanadium dioxide film and same structure different with the conduction band of metal photonic crystal waveguide, realize light-operated high-speed wideband Terahertz intensity modulated and frequency modulation.
At present relevant flexible Terahertz modulator report is less, mainly be because organic functions layer material and flexible substrates generally can not with the CMOS process compatible, generally all prepare on non-flexible substrates, can not reach pliable and tough flexible effect.Along with the manufacturing of flexible substrates unicircuit also needs novel flexible functional devices.
Summary of the invention
Purpose of the present invention is the shortcoming and defect that overcomes prior art.Adopt the get everything ready VO of phase-change characteristic of burning legal system based on flexible substrates
2Nano thin-film adopts light stimulus base flexible substrates vanadium oxide that THz wave is modulated.Provide a kind of preparation process simple, be easy to control, the preparation method of the novel Terahertz modulator mould material based on flexible substrates under the reliable and stable low optical power.
The present invention is achieved by following technical solution.
A kind of preparation method of the Terahertz modulator mould material based on flexible substrates has following steps:
(1) cleaning of flexible substrates PI:
Used flexible substrates is polyimide, is called for short PI, and it is put into the respectively ultrasonic cleaning 20 minutes of deionized water, acetone solvent and dehydrated alcohol successively, puts into subsequently massfraction and is 5% acetum and soaked 15 minutes, removes surface organic matter impurity; Clean again dry for standby with deionized water;
(2) preparation vanadium metal nano thin-film:
The cleaned PI of step (1) is placed the vacuum chamber of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment, adopt quality purity be 99.99% vanadium metal as target, take the argon gas of quality purity as 99.999% as working gas, base vacuum degree 4～6 * 10
-4Pa, substrate temperature are room temperature, and the argon gas flow is 45-48mL/min, and the sputter operating air pressure is 0.5～2Pa, sputtering power 135～150W, and sputtering time 10～60min is at PI surface deposition vanadium metal nano thin-film;
(3) based on the thermal treatment of flexible substrates vanadium metal nano thin-film
The vanadium metal nano thin-film that step (2) is made places fast heat treatment device, adopting quality purity is that 99.999% oxygen is as working gas, the oxygen gas flow is 30～50sccm, and thermal treatment temp is 250～300 ℃, and heat treatment time is 30～180s;
(4) modulation characteristic of the 8-fTHz time-domain spectral system testing base flexible substrates vanadium oxide film of employing standard, it is 200-600mW that institute adds laser power.
The specific inductivity of the flexible substrates PI of described step (1) is 3.4, high temperature resistantly reaches 400 ℃.
The specification of described step (1) flexible substrates PI is the rectangle of 2cm * 1cm;
The vanadium metal film thickness of described step (2) preparation is 50～300nm, and the vacuum chamber of high vacuum facing-target magnetron sputtering system equipment is the vacuum chamber of DPS-III type ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment.
Film after described step (3) thermal treatment is vanadium dioxide or Vanadium Pentoxide in FLAKES.
The fast heat treatment device of described step (3) is AG610 series, and the vanadium oxide film thickness that forms after the thermal treatment is 100～600nm.
Compared with prior art, beneficial effect of the present invention is:
1) mould material of modulating based on the THz wave of flexible substrates provided by the invention by means of laser pumping, is realized the Terahertz wave modulation by the character that changes material itself.
2) with respect to the modulator of existing non-flexible substrates, the present invention has realized the operability of modulator mould material on flexible substrates, for flexible substrates unicircuit new device provides application foundation.
Description of drawings
Fig. 1 is vanadium dioxide film electron scanning micrograph on the flexible substrates among the embodiment 1;
Fig. 2 is vanadium dioxide film Terahertz modulation spectrum figure on the flexible substrates among the embodiment 1;
Fig. 3 is vanadium dioxide film Terahertz modulation spectrum figure on the flexible substrates among the embodiment 2.
Embodiment
Embodiment 1
(1) used flexible substrates is polyimide (Polyimide), be called for short PI, it is put into deionized water, acetone solvent successively, the difference ultrasonic cleaning is 20 minutes in the dehydrated alcohol, put into subsequently massfraction and be 5% acetum and soaked 15 minutes, remove surface organic matter impurity; Clean with deionized water again, at last with the PI dry for standby;
The specification of PI flexible substrates is the rectangle of 2cm * 1cm;
(2) adopt the standby vanadium metal film of magnetic control beam sputtering legal system, adopt quality purity be 99.99% vanadium metal as target, take the argon gas of quality purity as 99.999% as working gas, base vacuum degree 4 * 10
-4Pa, substrate temperature are room temperature, and the argon gas flow is 45mL/min, and the sputter operating air pressure is 2Pa, sputtering power 135W, and sputtering time 10min is 50nm at surface deposition vanadium metal nano thin-film;
(3) the vanadium metal nano thin-film is placed fast heat treatment device AG610, adopt quality purity be 99.999% oxygen as working gas, the oxygen gas flow is 30sccm, thermal treatment temp is 300 ℃, heat treatment time is 180s; The vanadium dioxide film thickness that forms after the thermal treatment is 100nm.From the electron micrograph of Fig. 1 vanadium oxide film, can find out the smooth and even particle size of prepared film surface.
(4) adopt the 8-fTHz time-domain spectral system of standard to test, embodiment 1 makes the flexible substrates vanadium dioxide film THz wave is had stable modulating action, be 2.1THz in frequency, the variation of repeatedly measuring its modulation amplitude when laser power is 600mW is 40%, as shown in Figure 2.
Embodiment 2
Embodiment 2 is with the difference of embodiment 1:
Thermal treatment temp is 250 ℃ in the step (3).Embodiment 2 makes the flexible substrates vanadium dioxide film THz wave is had stable modulating action, is 2.1THz in frequency, and the variation of repeatedly measuring its modulation amplitude when laser power is 400mW is 40%, as shown in Figure 3.
Embodiment 3
Embodiment 3 is with the difference of embodiment 1:
Laser power is 300mW in the step (4).Embodiment 3 makes the flexible substrates vanadium dioxide film THz wave is had stable modulating action, is 2.1THz in frequency, and the variation of repeatedly measuring its modulation amplitude when laser power is 300mW is 30%.
Embodiment 4
Embodiment 4 is with the difference of embodiment 1:
Laser power is 400mW in the step (4).Embodiment 4 makes the flexible substrates vanadium dioxide film THz wave is had stable modulating action, is 2.1THz in frequency, and the variation of repeatedly measuring its modulation amplitude when laser power is 400mW is 35%.
The present invention is not limited to above-described embodiment, and is within the spirit and principles in the present invention all, any modification of making, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. preparation method based on the Terahertz modulator mould material of flexible substrates has following steps:
(1) cleaning of flexible substrates PI:
Used flexible substrates is polyimide, is called for short PI, and it is put into the respectively ultrasonic cleaning 20 minutes of deionized water, acetone solvent and dehydrated alcohol successively, puts into subsequently massfraction and is 5% acetum and soaked 15 minutes, removes surface organic matter impurity; Clean again dry for standby with deionized water;
(2) preparation vanadium metal nano thin-film:
The cleaned PI of step (1) is placed the vacuum chamber of ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment, adopt quality purity be 99.99% vanadium metal as target, take the argon gas of quality purity as 99.999% as working gas, base vacuum degree 4～6 * 10
-4Pa, substrate temperature are room temperature, and the argon gas flow is 45-48mL/min, and the sputter operating air pressure is 0.5～2Pa, sputtering power 135～150W, and sputtering time 10～60min is at PI surface deposition vanadium metal nano thin-film;
(3) based on the thermal treatment of flexible substrates vanadium metal nano thin-film
The vanadium metal nano thin-film that step (2) is made places fast heat treatment device, adopting quality purity is that 99.999% oxygen is as working gas, the oxygen gas flow is 30～50sccm, and thermal treatment temp is 250～300 ℃, and heat treatment time is 30～180s;
(4) modulation characteristic of the 8-fTHz time-domain spectral system testing base flexible substrates vanadium oxide film of employing standard, it is 200-600mW that institute adds laser power.
2. according to claim 1 a kind of preparation method of the Terahertz modulator mould material based on flexible substrates is characterized in that the specific inductivity of the flexible substrates PI of described step (1) is 3.4, high temperature resistantly reaches 400 ℃.
3. according to claim 1 a kind of preparation method of the Terahertz modulator mould material based on flexible substrates is characterized in that the specification of described step (1) flexible substrates PI is the rectangle of 2cm * 1cm.
4. according to claim 1 a kind of preparation method of the Terahertz modulator mould material based on flexible substrates, it is characterized in that, the vanadium metal film thickness of described step (2) preparation is 50～300nm, and the vacuum chamber of high vacuum facing-target magnetron sputtering system equipment is the vacuum chamber of DPS-III type ultrahigh vacuum(HHV) facing-target magnetron sputtering system equipment.
5. according to claim 1 a kind of preparation method of the Terahertz modulator mould material based on flexible substrates is characterized in that the film after described step (3) thermal treatment is vanadium dioxide or Vanadium Pentoxide in FLAKES.
6. according to claim 1 a kind of preparation method of the Terahertz modulator mould material based on flexible substrates, it is characterized in that, the fast heat treatment device of described step (3) is AG610 series, and the vanadium oxide film thickness that forms after the thermal treatment is 100～600nm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108258568A (en) * | 2018-01-12 | 2018-07-06 | 北京工业大学 | It is a kind of to use phase-change material and the film Terahertz light source of magnetostriction materials |
| CN109188730A (en) * | 2018-10-10 | 2019-01-11 | 桂林电子科技大学 | A kind of broadband terahertz wave modulator, preparation method and modulating system |
| WO2020125439A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Method for preparing flexible vanadium oxide composite thin film by means of low-temperature buffer layer technology |
| CN112462536A (en) * | 2021-01-20 | 2021-03-09 | 电子科技大学 | Terahertz wave phase adjustment and control method based on organic solvent |
| CN113652640A (en) * | 2021-08-20 | 2021-11-16 | 电子科技大学 | Method for preparing nano composite phase vanadium oxide flexible film by sputtering and film |
| CN116103623A (en) * | 2023-02-13 | 2023-05-12 | 天津理工大学 | Preparation method of intelligent window coating material with novel structure |
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| CN102212782A (en) * | 2011-05-24 | 2011-10-12 | 天津大学 | Quick thermal treatment method for preparing vanadium dioxide film |
| CN102274973A (en) * | 2010-12-25 | 2011-12-14 | 河南科技大学 | Method for generating nano-copper particles on surface of copper alloy thin film |
| WO2012108265A1 (en) * | 2011-02-10 | 2012-08-16 | Jx日鉱日石金属株式会社 | Two-layered copper-clad laminate material, and method for producing same |
| CN102732847A (en) * | 2012-06-18 | 2012-10-17 | 天津大学 | Phase change vanadium dioxide film prepared by rapid thermal oxidation method |
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| CN1752270A (en) * | 2005-07-12 | 2006-03-29 | 天津大学 | Opposite target reaction magnetocontrol sputtering method for preparing vanadium oxide film |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108258568A (en) * | 2018-01-12 | 2018-07-06 | 北京工业大学 | It is a kind of to use phase-change material and the film Terahertz light source of magnetostriction materials |
| CN108258568B (en) * | 2018-01-12 | 2020-04-17 | 北京工业大学 | Thin film terahertz light source using phase change material and magnetostrictive material |
| CN109188730A (en) * | 2018-10-10 | 2019-01-11 | 桂林电子科技大学 | A kind of broadband terahertz wave modulator, preparation method and modulating system |
| WO2020125439A1 (en) * | 2018-12-18 | 2020-06-25 | 深圳先进技术研究院 | Method for preparing flexible vanadium oxide composite thin film by means of low-temperature buffer layer technology |
| CN112462536A (en) * | 2021-01-20 | 2021-03-09 | 电子科技大学 | Terahertz wave phase adjustment and control method based on organic solvent |
| CN112462536B (en) * | 2021-01-20 | 2022-01-14 | 电子科技大学 | Terahertz wave phase adjustment and control method based on organic solvent |
| CN113652640A (en) * | 2021-08-20 | 2021-11-16 | 电子科技大学 | Method for preparing nano composite phase vanadium oxide flexible film by sputtering and film |
| CN113652640B (en) * | 2021-08-20 | 2022-10-04 | 电子科技大学 | Method for preparing nano composite phase vanadium oxide flexible film by sputtering and film |
| CN116103623A (en) * | 2023-02-13 | 2023-05-12 | 天津理工大学 | Preparation method of intelligent window coating material with novel structure |
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Application publication date: 20131023 |