CN106435472A - Preparation method of gold triangular nanoparticle array and vanadium dioxide film composite embedded structure - Google Patents

Preparation method of gold triangular nanoparticle array and vanadium dioxide film composite embedded structure Download PDF

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CN106435472A
CN106435472A CN201610910921.0A CN201610910921A CN106435472A CN 106435472 A CN106435472 A CN 106435472A CN 201610910921 A CN201610910921 A CN 201610910921A CN 106435472 A CN106435472 A CN 106435472A
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vanadium dioxide
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CN106435472B (en
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梁继然
宋晓龙
周立伟
李景朋
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Tianjin University
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    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • 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
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
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    • 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
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    • 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
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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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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Abstract

The invention discloses a preparation method of a gold triangular nanoparticle array and vanadium dioxide film composite embedded structure. The preparation method comprises six steps of cleaning of a sapphire substrate, preparation of a monodispersion SiO2 mask layer, preparation of a gold triangular nanoparticle array structure, preparation of a vanadium film, preparation of a vanadium dioxide film and preparation of a gold reflection layer. The prepared film consists of the gold triangular nanoparticle array, the vanadium dioxide film and the gold reflection layer; and through adjustment of the preparation sequence, the gold triangular nanoparticle array can be embedded in the vanadium dioxide film to realize adjustment of resonant wavelengths. A film preparation absorber has such advantages as wider adjustment of visible light-near infrared band resonant wavelengths, high absorption efficiency, simple structure and small size, and can be applied to such aspects as light detection, electromagnetic switches and sensors.

Description

A kind of Golden Triangle nano-grain array and vanadium dioxide film are combined the system of nested structure Preparation Method
Technical field
The present invention relates to the preparation method of a kind of vanadium dioxide film, especially relate to a kind of by Golden Triangle nano particle battle array The preparation method of the vanadium dioxide film of row, vanadium dioxide film and gold reflecting layer composition.
Background technology
In recent years, Meta Materials is increasingly becoming as a kind of special artificial composite structure or composite, its optical property One of focus direction of domestic and international optical field research so that it is have widely in fields such as absorber, sensor, electromagnetic surveyings Application prospect.Meta-material absorber, as its important research direction, can not only realize rationally collecting and utilizing to resource, And have important application in optical detection and sensory field.The optical characteristics of absorber is limited to physical dimension and lattice list Unit's size, traditional meta-material absorber structure is once it is determined that get off, and optical characteristics is difficult to change and working frequency range is narrower, is Expand the scope of application and the wide usage of meta-material absorber, phase-change material is incorporated in meta-material absorber, to realize right The dynamic regulation of absorber optical characteristics.Vanadium dioxide (VO2) it is a kind of temperature-sensitive material, can occur by semiconductor at 68 DEG C Arriving the change of metal phase mutually, in phase transition process, crystal structure is become high temperature four directions rutile knot from low temperature monocline rutile structure Structure, VO before and after phase transformation2Optically and electrically performance there is reversible rapid mutation, especially near infrared band VO2Transmission occur By the highly transmissive transformation to low transmission, obvious on an off two states occurs.Owing to having the excellent of this optical property altering Gesture so that VO2Become to prepare the ideal material of tunability meta-material absorber.
In order to obtain more preferable absorption characteristic, domestic and international researcher's great majority are devoted to the innovation of metamaterial structure, knot Close VO2Phase-change characteristic, inquire into its special optical characteristic in different operating frequency range.Flat film structure, nano-wire array knot Structure and the application of nanometer disk composite construction, it is achieved dynamically adjustable to absorber absorption intensity；Split ring resonator array/thin The application of membrane structure, grating/dielectric layer/membrane structure and film/noble metal/membrane structure, it is achieved that absorber is absorbed The dynamic regulation of wavelength.Current research situation both domestic and external is also few for the adjustability research of absorber absorbing wavelength, especially Relatively fewer in the research work of visible ray-near infrared band, and the tuning range of current resonant wavelength only up to About 30%, have greatly improved space.
Content of the invention
In order to solve problems of the prior art, the present invention provides a kind of Golden Triangle nano-grain array/titanium dioxide The preparation method of vanadium film, overcomes the problem that in prior art, meta-material absorber wavelength regulation scope is little.
The technical solution used in the present invention is：A kind of Golden Triangle nano-grain array nested knot compound with vanadium dioxide film The preparation method of structure, comprises the following steps：
(1) cleaning of sapphire substrates：
Sapphire sheet is sequentially placed in deionized water, acetone and absolute ethyl alcohol ultrasonic cleaning respectively, by indigo plant after cleaning Sapphire substrates is put in absolute ethyl alcohol standby；
(2) single dispersing SiO is prepared2Mask layer：
Drainage piece oblique cutting is entered in deionized water, then uses liquid-transfering gun by SiO2-ethanol solution is added drop-wise to drainage On piece, and make it slowly flow on the water surface, form high density, large-area individual layer SiO2Array, thus be configured to lift liquid；Quiet Put after liquid level stabilizing, lentamente sapphire substrate is immersed in lifting liquid with plated film pulling machine, and carries vertically and lentamente Pull-out liquid level, obtains single dispersing SiO2Mask layer；
(3) Golden Triangle nanoparticle array structure is prepared：
Surface prepared by step (2) had single dispersing SiO2The sapphire substrate of mask layer is placed in high vacuum evaporation plated film In machine, evaporate one layer of noble metal Au；Then, above-mentioned print is placed sonic oscillation in absolute ethyl alcohol and process 10s～20s, to incite somebody to action SiO2Mask layer is got rid of, and obtains Golden Triangle nanoparticle array structure；
(4) vanadium film is prepared：
The sapphire substrate that surface prepared by step (3) has Golden Triangle nanoparticle array structure is placed in ultrahigh vacuum The vacuum chamber sputtering of facing-target magnetron sputtering system equipment, at the vanadium film that surface deposit thickness is 70-120 nanometer；
(5) preparation of vanadium dioxide film：
It is put in the vanadium film that step (4) prepares in quick anneal oven and carry out Quick Oxidation thermal annealing；
(6) preparation in gold reflecting layer：
Step (5) is prepared print be placed in high vacuum evaporation coating machine, evaporate one layer of noble metal Au.
Described step (2) pull rate controls between 80-180 μm/min.
The vacuum chamber of described step (4) ultrahigh vacuum facing-target magnetron sputtering system equipment is that DPS-III type ultrahigh vacuum is to target magnetic control The vacuum chamber of sputtering equipment, sputtering condition is：Background vacuum 4 × 10-4Pa, substrate temperature is room temperature, and argon gas flow is 48mL/min, sputtering operating air pressure is 2Pa, sputtering power 135W, sputtering time 10min-25min.
In described step (5) quick anneal oven, annealing conditions is：Gas flow is 3slpm, and holding temperature is 450 DEG C, rises Temperature speed is determined by setting holding temperature and heating-up time, temperature retention time 70s-110s, temperature fall time 90s.
Described step (6) high vacuum evaporation coating machine condition is：Background vacuum 1 × 10-4Pa, vaporization voltage is 2.2V, Electric current is 110V.
The invention has the beneficial effects as follows：
1) Golden Triangle nano-grain array is nested in VO2The preparation of membrane structure, passes through FTIS Test, it shows wider resonant wavelength adjustability at visible ray-near infrared band.
2) present invention is based primarily upon skilled self-assembling technique and thin film preparation process, there is preparation simple, suitably big The advantage that technical scale produces, and the low requirement of preparation technology and low cost all imply that this imagination and system have bigger Advantage.
Film prepared by the present invention is made up of Golden Triangle nano-grain array, vanadium dioxide film and gold reflecting layer, By adjusting preparation order, enable Golden Triangle nano-grain array nested in vanadium dioxide film, it is achieved resonant wavelength Adjustability.The absorber of the film preparation of the application present invention has can the wider of visible ray near infrared band resonant wavelength Adjust, the advantages such as absorption efficiency height, simple in construction, volume are little, can be applicable to the aspects such as optical detection, electromagnetic switch and sensor.
Brief description
Fig. 1 is that Golden Triangle nano-grain array is nested in VO2Membrane structure schematic diagram；
Fig. 2 is the single dispersing SiO obtaining under different pull rate2Mask layer；A, B, C, D corresponding pull rate respectively is 90 μm/min, 110 μm/min, 130 μm/min, the single dispersing SiO of 150 μm/min2Mask layer SEM schemes；
Fig. 3 is different-thickness Golden Triangle nano-grain array SEM structure chart；A, B are respectively the gold that thickness is 10nm, 30nm The structure chart of triarray；
Fig. 4 is made by the absorption spectrum curve that FTIS obtains；A, B are respectively vanadium dioxide thickness For 90nm, the absorption spectrum of corresponding 10nm, 30nm Golden Triangle nanoparticle array structure.
Detailed description of the invention
Describe the present invention with detailed description of the invention below in conjunction with the accompanying drawings.
The present invention is raw materials used all uses commercially available material, and preparation method comprises the steps：
(1) cleaning of sapphire substrates：
The sapphire substrates of double polishings that sapphire used is (001) crystal face, thickness is 0.45mm.By sapphire sheet once Put into difference ultrasonic cleaning 20 minutes in deionized water, acetone and absolute ethyl alcohol, remove the organic impurities on surface；Spend again from Sub-water is cleaned, and finally puts into sapphire substrate in absolute ethyl alcohol standby.
(2) single dispersing SiO is prepared2Mask layer：
First, entering in a certain amount of deionized water by clean slide oblique cutting, then particle diameter is by use liquid-transfering gun The SiO of 600nm2-ethanol solution is added drop-wise on drainage piece, and makes it slowly flow on the water surface, and uniform spreading launches to come, and is formed High density, large-area individual layer SiO2Array, thus be configured to lift liquid.Standing, after liquid level stabilizing, is delayed by plated film pulling machine Slowly sapphire substrate is immersed in lifting liquid, and lifts out liquid level vertically and lentamente, pull rate be defined as 110 μm/ Min, obtains the single dispersing SiO of better quality2Mask layer.
(3) Golden Triangle nanoparticle array structure is prepared：
Surface is had single dispersing SiO2The sapphire substrate of mask layer is placed in high vacuum evaporation coating machine, uses quality Purity is that the spun gold (Au) of 99.99% is as target, background vacuum 1 × 10-4Pa, vaporization voltage is 2.2V, and electric current is 110V, Evaporation a layer thickness is the noble metal Au of 10nm/30nm (show with crystal-vibration-chip and be as the criterion).Then, above-mentioned print is placed on density After the absolute ethyl alcohol of 0.17g/ml stands half an hour, carry out sonic oscillation to it and process 15s, with by SiO2Mask layer is removed Fall, obtain Golden Triangle nanoparticle array structure.
(4) vanadium (V) film is prepared：
The sapphire substrate that surface has Golden Triangle nanoparticle array structure is placed in ultrahigh vacuum facing-target magnetron sputtering system The vacuum chamber of equipment, use quality purity be the vanadium metal of 99.95% as target, with the argon gas that quality purity is 99.999% As working gas, background vacuum 4 × 10-4Pa, substrate temperature is room temperature, and argon gas flow is 48mL/min, sputters work It is 2Pa as air pressure, sputtering power 135W, sputtering time 15min are thin at the vanadium metal that deposition corresponding thickness in surface is 90 nanometers Film.
(5) preparation of vanadium dioxide film：
It is put in the vanadium film that step (4) prepares in quick anneal oven and carry out Quick Oxidation thermal annealing.It is passed through during thermal oxide Gas be high purity oxygen gas, gas flow is fixed as 3slpm, and holding temperature is 450 DEG C, heating rate by set holding temperature Determining with the heating-up time, its value is fixed as 50 DEG C/s, heating-up time 9s, temperature retention time 90s, temperature fall time 90s.
(6) preparation in gold reflecting layer：
Above-mentioned print is placed in high vacuum evaporation coating machine, spun gold (Au) conduct using quality purity to be 99.99% Target, background vacuum 1 × 10-4Pa, vaporization voltage is 2.2V, and electric current is 110V, and evaporation a layer thickness is that 100nm is (with crystal oscillator Piece show be as the criterion) noble metal Au.
The present invention prepares Golden Triangle nano-grain array and is nested in vanadium dioxide film composite construction, and is applied super In material absorber structure, can play the greater role effect of electromagnetic coupled, it is expensive that this nested form can be used for other Metal nanoparticle array structure and the combination of phase-change material, to develop the Meta Materials of more using value.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For Yuan, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (5)

1. a Golden Triangle nano-grain array and vanadium dioxide film are combined the preparation method of nested structure, it is characterised in that Comprise the following steps：
(1) cleaning of sapphire substrates：
Sapphire sheet is sequentially placed in deionized water, acetone and absolute ethyl alcohol ultrasonic cleaning respectively, by sapphire after cleaning Substrate is put in absolute ethyl alcohol standby；
(2) single dispersing SiO is prepared2Mask layer：
Drainage piece oblique cutting is entered in deionized water, then uses liquid-transfering gun by SiO2-ethanol solution is added drop-wise on drainage piece, And make it slowly flow on the water surface, form high density, large-area individual layer SiO2Array, thus be configured to lift liquid；Standing is treated After liquid level stabilizing, lentamente sapphire substrate is immersed in lifting liquid with plated film pulling machine, and lifts out vertically and lentamente Liquid level, obtains single dispersing SiO2Mask layer；
(3) Golden Triangle nanoparticle array structure is prepared：
Surface prepared by step (2) had single dispersing SiO2The sapphire substrate of mask layer is placed in high vacuum evaporation coating machine, Evaporate one layer of noble metal Au；Then, above-mentioned print is placed sonic oscillation in absolute ethyl alcohol and process 10s～20s, with by SiO2Cover Film layer is got rid of, and obtains Golden Triangle nanoparticle array structure；
(4) vanadium film is prepared：
The sapphire substrate that surface prepared by step (3) has Golden Triangle nanoparticle array structure is placed in ultrahigh vacuum to target The vacuum chamber sputtering of magnetron sputtering apparatus, at the vanadium film that surface deposit thickness is 70-120 nanometer；
(5) preparation of vanadium dioxide film：
It is put in the vanadium film that step (4) prepares in quick anneal oven and carry out Quick Oxidation thermal annealing；
(6) preparation in gold reflecting layer：
Step (5) is prepared print be placed in high vacuum evaporation coating machine, evaporate one layer of noble metal Au.
2. Golden Triangle nano-grain array and vanadium dioxide film are combined the preparation side of nested structure according to claim 1 Method, it is characterised in that described step (2) pull rate controls between 80-180 μm/min.
3. Golden Triangle nano-grain array and vanadium dioxide film are combined the preparation side of nested structure according to claim 1 Method, it is characterised in that the vacuum chamber of described step (4) ultrahigh vacuum facing-target magnetron sputtering system equipment is DPS-III type ultrahigh vacuum pair The vacuum chamber of target magnetic control sputtering equipment, sputtering condition is：Background vacuum 4 × 10-4Pa, substrate temperature is room temperature, argon gas Flow is 48mL/min, and sputtering operating air pressure is 2Pa, sputtering power 135W, sputtering time 10min-25min.
4. Golden Triangle nano-grain array and vanadium dioxide film are combined the preparation side of nested structure according to claim 1 Method, it is characterised in that in described step (5) quick anneal oven, annealing conditions is：Gas flow is 3slpm, and holding temperature is 450 DEG C, heating rate is determined by setting holding temperature and heating-up time, temperature retention time 70s-110s, temperature fall time 90s.
5. Golden Triangle nano-grain array and vanadium dioxide film are combined the preparation side of nested structure according to claim 1 Method, it is characterised in that described step (6) high vacuum evaporation coating machine condition is：Background vacuum 1 × 10-4Pa, vaporization voltage is 2.2V, electric current is 110V.
CN201610910921.0A 2016-10-18 2016-10-18 A kind of preparation method of Golden Triangle nano-grain array and the compound nested structure of vanadium dioxide film Expired - Fee Related CN106435472B (en)

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CN107201497A (en) * 2017-04-18 2017-09-26 天津大学 A kind of Golden Triangle and vanadium dioxide nano Particles dispersed array structure and preparation method
CN107858649A (en) * 2017-11-17 2018-03-30 天津大学 One kind can improve VO2Film sunshine regulates and controls the preparation method of efficiency
CN108179394A (en) * 2018-02-07 2018-06-19 天津大学 A kind of method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power
CN108385064A (en) * 2018-01-18 2018-08-10 天津大学 A method of vanadium dioxide transmitted spectrum is regulated and controled by gold nano grain
CN108950492A (en) * 2018-07-06 2018-12-07 中国航发北京航空材料研究院 A kind of VO with optical limiting properties2The preparation method of laminated film
CN110429388A (en) * 2019-08-06 2019-11-08 天津工业大学 A kind of wideband adjustable Terahertz absorber and preparation method thereof based on vanadium dioxide
CN113314851A (en) * 2021-05-19 2021-08-27 中南大学 Polarization insensitive frequency reconfigurable super-surface wave absorber
CN114488550A (en) * 2022-01-25 2022-05-13 秦皇岛本征晶体科技有限公司 Infrared multi-angle continuous variable splitting ratio coated fluoride spectroscope and manufacturing method thereof

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CN103981488A (en) * 2014-05-23 2014-08-13 天津大学 Method for preparing vanadium oxide nanoparticle array by rapid heat treatment

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CN103981500A (en) * 2014-05-23 2014-08-13 天津大学 Surface microstructure for improving phase change amplitude of vanadium dioxide thin film
CN103981488A (en) * 2014-05-23 2014-08-13 天津大学 Method for preparing vanadium oxide nanoparticle array by rapid heat treatment

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107201497A (en) * 2017-04-18 2017-09-26 天津大学 A kind of Golden Triangle and vanadium dioxide nano Particles dispersed array structure and preparation method
CN107858649A (en) * 2017-11-17 2018-03-30 天津大学 One kind can improve VO2Film sunshine regulates and controls the preparation method of efficiency
CN108385064A (en) * 2018-01-18 2018-08-10 天津大学 A method of vanadium dioxide transmitted spectrum is regulated and controled by gold nano grain
CN108179394A (en) * 2018-02-07 2018-06-19 天津大学 A kind of method for improving vanadium dioxide phase time-varying amplitude by regulating and controlling sputtering power
CN108950492A (en) * 2018-07-06 2018-12-07 中国航发北京航空材料研究院 A kind of VO with optical limiting properties2The preparation method of laminated film
CN108950492B (en) * 2018-07-06 2020-06-09 中国航发北京航空材料研究院 Preparation method of VO2 composite file with optical limiting performance
CN110429388A (en) * 2019-08-06 2019-11-08 天津工业大学 A kind of wideband adjustable Terahertz absorber and preparation method thereof based on vanadium dioxide
CN113314851A (en) * 2021-05-19 2021-08-27 中南大学 Polarization insensitive frequency reconfigurable super-surface wave absorber
CN114488550A (en) * 2022-01-25 2022-05-13 秦皇岛本征晶体科技有限公司 Infrared multi-angle continuous variable splitting ratio coated fluoride spectroscope and manufacturing method thereof
CN114488550B (en) * 2022-01-25 2024-02-06 秦皇岛本征晶体科技有限公司 Infrared multi-angle continuously variable spectral ratio coated fluoride spectroscope and manufacturing method thereof

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