CN104060241A - Liquid-phase preparation method of high-oriented vanadium dioxide film - Google Patents

Liquid-phase preparation method of high-oriented vanadium dioxide film Download PDF

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CN104060241A
CN104060241A CN201410324869.1A CN201410324869A CN104060241A CN 104060241 A CN104060241 A CN 104060241A CN 201410324869 A CN201410324869 A CN 201410324869A CN 104060241 A CN104060241 A CN 104060241A
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vanadium dioxide
precursor
film
liquid
dioxide film
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CN104060241B (en
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郭玉献
徐海燕
童彬
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Anhui Jianzhu University
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Anhui Jianzhu University
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Abstract

The invention discloses a liquid-phase preparation method of a high-oriented vanadium dioxide film, belonging to the field of chemical function materials. The preparation method comprises the following steps: preparing precursor liquid by taking triisopropoxyvanadium oxide as solute, coating a sapphire substrate with the obtained precursor liquid to prepare a precursor film, and finally sintering the precursor film in a vacuum environment. According to the preparation method, the vanadium dioxide film is prepared by controlling vacuum sintering conditions on the basis of a liquid-phase method, the obtained film is good in growth orientation, the phase change temperature of the film is about 60 DEG C, and the change of electrical resistivity before and after the phase change is more than three orders of magnitude; in addition, the preparation process is simple and suitable for large-range popularization.

Description

A kind of liquid phase preparation process of high orientation vanadium dioxide film
Technical field
The liquid phase preparation process that the present invention relates to a kind of high orientation vanadium dioxide film, belongs to field of chemical functional materials.
Background technology
Vanadium dioxide (VO 2) be a kind of strong correlation electron material, body phase VO 2near 68 DEG C, occur from hot metal phase (rutile R phase) to the structural mutation of cryogenic semiconductor phase (monocline M phase), be accompanied by the great variety of its resistivity and infrared light transmission rate, and phase transition process is reversible.Because this material electricity, magnetic, optical property before and after phase transformation have larger variation, thereby have a wide range of applications demand at aspects such as photoelectric switch material, storage media and smart window materials.
VO 2film can experience phase transformation circulation repeatedly and not rupture, and therefore has application prospect more widely.High orientation VO 2film, because its crystal grain arrangement is more orderly than polycrystalline, causes it to have more remarkable phase-change characteristic, as change in resistance amplitude larger before and after phase transformation, and less transition temperature area scope etc.Common preparation method, except the physics film-forming methods such as pulsed laser deposition, magnetron sputtering, molecular beam epitaxy, also has the liquid phase methods such as sol-gel method.Comparatively speaking membrane structure densification, orientation that, prepared by Physical are better; And the film general structure of Liquid preparation methods is more loose, the film that obtains high growth orientation is more difficult, but have that technique is simple, cost is low, be easy to doping and can big area film forming etc. advantage.Undoubtedly, if can utilize liquid phase method, adopt the preparation technology who simplifies to obtain high orientation VO 2film, will have very important significance.For above-mentioned target, mainly there is the problem of following several respects in technology at present: (1) sintering process needs gas shield, comprises reducing gas, rare gas element and both mixed gass (CN201010126863.5) etc.; This need to increase the device of source of the gas, gas circuit and mixed gas, thereby makes equipment and manipulation become more complicated, has also increased cost of manufacture; (2) under vacuum environment, vacuum is required when sintering too high, the VO obtaining 2lack orientation; VO 2film oxide compound of some vanadium normally before sintering, prepares VO by vacuum sintering 2need vacuum tightness to be better than 10 -2pa(Surface & Coatings Technology, 201,2007,6772-6776), also having bibliographical information is 1-2Pa(Applied Surface Science, 191,2002,176-180); All in all, the VO of preparation 2purity is generally not high, also has the barium oxide of other phase to occur in X-ray diffraction spectrum, and film does not have growth orientation.The reason key that occurs above-mentioned phenomenon is that the homogeneity of reduction is inadequate, and in sintering process, film surface is different from the environment of the inner contact of film, causes occurring different vanadium oxide thing phases after sintering; In addition, substrate material choose the VO to preparing high growth orientation 2film is also extremely important.
Summary of the invention
The object of this invention is to provide a kind of liquid phase preparation process of high orientation vanadium dioxide film, to overcome the deficiencies in the prior art.
The invention provides a kind of liquid phase preparation process of high orientation vanadium dioxide film, its preparation method is the alkoxide preparation precursor liquid of first using vanadium, then precursor liquid is applied to substrate surface and prepares precursor film, finally precursor film is placed under vacuum condition and fires and form; Specific as follows:
(1), taking Triisopropoxyvanadium(V) oxide as solute, Virahol is solvent preparation precursor liquid;
(2) gained precursor solution is applied to Sapphire Substrate, makes precursor film;
(3) gained precursor film is placed in to vacuum oven sintering, is incubated 0.5 ~ 20 hour, obtain vanadium dioxide film, wherein, sintering temperature is controlled at 400 DEG C ~ 600 DEG C, and sintering environment vacuum degree control is at 3 Pa ~ 15 Pa.
Preferably, the soaking time scope in described step (3) is at 4h ~ 10h.
Preferably, the sintering range in described step (3) is at 430 DEG C ~ 590 DEG C.
Preferably, the sintering environment vacuum ranges in described step (3) is at 4Pa ~ 8Pa.
Described step (2) makes after precursor film, and it is carried out to drying and processing; Preferably, bake out temperature is no more than 300 DEG C, and drying time is no more than 15 minutes.
When described step (1) is prepared precursor liquid, add Glacial acetic acid as stablizer, the mass ratio of Glacial acetic acid and Triisopropoxyvanadium(V) oxide is 1:1 ~ 6:1.
In the precursor liquid of preparing in step (1), the mass volume ratio g:ml of Triisopropoxyvanadium(V) oxide and Virahol is 1-15:100.
As shown from the above technical solution: it is raw material that the present invention adopts Triisopropoxyvanadium(V) oxide, sapphire wafer is substrate, by controlling drying glue process, make to contain certain organic composition in the precursor film before sintering, these organic compositions can evenly reduce V in the time of vacuum sintering 5+obtain high orientation VO 2film, the requirement to vacuum while reducing sintering, and do not need other gas shield, for being orientated VO with Liquid preparation methods height 2film provides technical support.
The present invention has the following advantages:
1, the precursor film that prepared by the present invention, carrying out can carrying out short period of time oven drying at low temperature processing before vacuum sintering, also can not dry direct sintering; This processing mode makes organic composition remaining in film can in sintering process, play the effect of reductive agent, and its benefit has two: one, need under reductibility or protection of inert gas, not prepare VO 2film, has reduced the requirement to experimental installation, has also simplified operation sequence, and the 2nd, this reductive agent is evenly distributed on film inside, more even to the reduction ratio of film, can effectively reduce the generation of other valence state barium oxide; The use of Sapphire Substrate, makes interface crystal lattice coupling good, is conducive to obtain the VO of pure phase, high orientation 2film;
2, compared with prior art, due to the not filming equipment of value on demand costliness of method of the present invention, vacuum (3Pa ~ 15Pa) used belongs to rough vacuum, only needs common mechanical pump just can reach requirement; Owing to not needing to pass into any gas, operate simplyr, masking cost is lower;
3, the prepared vanadium dioxide film of the present invention, has higher quality, and macroscopical phase-change characteristic is remarkable, and before and after phase transformation, change in resistance reaches 3 more than magnitude;
4, experimental result shows, gained VO 2film, in x ray diffraction spectra, shows good growth orientation.
Brief description of the drawings
Fig. 1 is the high orientation VO that the embodiment of the present invention 1 prepares 2the x x ray diffration pattern x of film;
Fig. 2 is the high orientation VO that the embodiment of the present invention 1 prepares 2electrical resistance temperature changing curve diagram before and after thin film phase change critical temperature;
Fig. 3 is the high orientation VO that the embodiment of the present invention 2 prepares 2the x x ray diffration pattern x of film;
Fig. 4 is the high orientation VO that the embodiment of the present invention 2 prepares 2electrical resistance temperature changing curve diagram before and after thin film phase change critical temperature;
Fig. 5 is the high orientation VO that the embodiment of the present invention 3 prepares 2the x x ray diffration pattern x of film;
Fig. 6 is the high orientation VO that the embodiment of the present invention 3 prepares 2electrical resistance temperature changing curve diagram before and after thin film phase change critical temperature.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, instead of restriction to invention claim.
Embodiment 1
In the time of 430 DEG C of sintering temperatures, insulation 4 hours, vacuum tightness 5Pa, prepare vanadium dioxide film.
(1) precursor liquid preparation:
Get Triisopropoxyvanadium(V) oxide 0.8g, dissolve in 50ml Virahol, then drip 1.3g Glacial acetic acid formation mixing solutions, with glass stick stirring 10 minutes, obtain the precursor liquid of vanadium dioxide film.
(2) clean substrate:
Select sapphire wafer to do substrate, inserted respectively acetone, ethanol and deionized water for ultrasonic and clean 5 minutes, finally dry up with nitrogen, for subsequent use.
(3) precursor liquid plated film:
Choose the precursor liquid of above-mentioned steps (1) gained, with sol evenning machine spin coating plated film; Even glue process is: 200 revs/min of first low speed, keep 9 seconds; 2000 revolutions per seconds of high speeds, keep 20 seconds again; Then, the film obtaining is placed on to 250 DEG C of roasting Jiao Tai upper, dry 3 minutes, obtains vanadium dioxide precursor film.
(4) vanadium dioxide film sintering:
The precursor film that above-mentioned steps is obtained is put into vacuum oven, starts vacuum pump system vacuum degree is evacuated to below 3Pa, regulates the valve between vacuum pump and system, makes vacuum keep in 5Pa left and right; 430 DEG C of sintering temperatures are set, 6 DEG C/min of heat-up rate, soaking time 4 hours, after sintering completes, cooling naturally, finally obtains the vanadium dioxide film that about 20nm is thick.
Fig. 1 is the VO that embodiment 1 obtains 2the x ray diffraction spectra of film, 39.8 ° of diffraction angle correspondences VO 2(020) diffraction, in addition, do not find other obvious VO 2diffraction peak exists, and shows that film prepared by the present invention has good crystal property and high growth orientation.
Fig. 2 is the VO that embodiment 1 obtains 2before and after phase transformation, the change curve of resistivity, can find out, 1K Ω when 2M Ω when sheet resistance is from room temperature before and after phase transformation changes to 90 DEG C, and the variation of resistivity reaches 3 more than magnitude, and transformation temperature is 59.7 DEG C, and phase Trapezoidal is 9.4 DEG C.
Embodiment 2
In the time of 530 DEG C of sintering temperatures, insulation 7 hours, vacuum tightness 4Pa, prepare vanadium dioxide film.
(1) precursor liquid preparation:
Get Triisopropoxyvanadium(V) oxide 1.9g, dissolve in 50ml Virahol, then drip 6.3g Glacial acetic acid formation mixing solutions, with glass stick stirring 10 minutes, obtain the precursor liquid of vanadium dioxide film.
(2) clean substrate:
Select sapphire wafer to do substrate, inserted respectively acetone, ethanol and deionized water for ultrasonic and clean 5 minutes, finally dry up with nitrogen, for subsequent use.
(3) precursor liquid plated film:
Choose the precursor liquid of above-mentioned steps (1) gained, with sol evenning machine spin coating plated film; Even glue process is: 200 revs/min of first low speed, keep 9 seconds; 2000 revolutions per seconds of high speeds, keep 20 seconds again, obtain vanadium dioxide precursor film.
(4) vanadium dioxide film sintering:
The precursor film that above-mentioned steps is obtained is put into vacuum oven, starts vacuum pump system vacuum degree is evacuated to below 3Pa, regulates the valve between vacuum pump and system, makes vacuum keep in 4Pa left and right; 530 DEG C of sintering temperatures are set, 6 DEG C/min of heat-up rate, soaking time 7 hours, after sintering completes, cooling naturally, finally obtains the vanadium dioxide film that about 50nm is thick.
Fig. 3 is the VO that embodiment 2 obtains 2the x ray diffraction spectra of film, 39.8 ° of diffraction angle correspondences VO 2(020) diffraction, in addition, do not find other obvious VO 2diffraction peak exists, and shows that film prepared by the present invention has good crystal property and high growth orientation.
Fig. 4 is the VO that embodiment 2 obtains 2before and after phase transformation, the change curve of resistivity, can find out, 100 Ω when 0.1M Ω when sheet resistance is from room temperature before and after phase transformation changes to 90 DEG C, and the variation of resistivity reaches 3 magnitudes, and transformation temperature is 57.6 DEG C, and phase Trapezoidal is 4.2 DEG C.
Embodiment 3
In the time of 590 DEG C of sintering temperatures, insulation 10 hours, vacuum tightness 8Pa, prepare vanadium dioxide film.
(1) precursor liquid preparation:
Get Triisopropoxyvanadium(V) oxide 4.5g, dissolve in 50ml Virahol, then drip 25g Glacial acetic acid formation mixing solutions, with glass stick stirring 10 minutes, obtain the precursor liquid of vanadium dioxide film.
(2) clean substrate:
Select sapphire wafer to do substrate, inserted respectively acetone, ethanol and deionized water for ultrasonic and clean 5 minutes, finally dry up with nitrogen, for subsequent use.
(3) precursor liquid plated film:
Choose the precursor liquid of above-mentioned steps (1) gained, with sol evenning machine spin coating plated film; Even glue process is: 200 revs/min of first low speed, keep 9 seconds; 2000 revolutions per seconds of high speeds, keep 20 seconds again; Then, the film obtaining is placed on to 90 DEG C of roasting Jiao Tai upper, dry 5 minutes, obtains vanadium dioxide precursor film.
(4) vanadium dioxide film sintering:
The precursor film that above-mentioned steps is obtained is put into vacuum oven, starts vacuum pump system vacuum degree is evacuated to below 3Pa, regulates the valve between vacuum pump and system, makes vacuum keep in 8Pa left and right; 590 DEG C of sintering temperatures are set, 6 DEG C/min of heat-up rate, soaking time 10 hours, after sintering completes, cooling naturally, finally obtains the vanadium dioxide film that about 65nm is thick.
Fig. 5 is the VO that embodiment 3 obtains 2the x ray diffraction spectra of film, 39.8 ° of diffraction angle correspondences VO 2(020) diffraction, in addition, do not find other obvious VO 2diffraction peak exists, and shows that film prepared by the present invention has good crystal property and high growth orientation.
Fig. 6 is the VO that embodiment 3 obtains 2before and after phase transformation, the change curve of resistivity, can find out, 500 Ω when 2M Ω when sheet resistance is from room temperature before and after phase transformation changes to 90 DEG C, and the variation of resistivity reaches 3 more than magnitude, and transformation temperature is 56.6 DEG C, and phase Trapezoidal is 5.1 DEG C.
The above is only the preferred embodiment of the present invention; it should be pointed out that the ordinary person for the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (8)

1. a liquid phase preparation process for high orientation vanadium dioxide film, its preparation method is the alkoxide preparation precursor liquid of first using vanadium, then precursor liquid is applied to substrate surface and prepares precursor film, finally precursor film is placed under vacuum condition and fires and form; Specific as follows:
(1), taking Triisopropoxyvanadium(V) oxide as solute, Virahol is solvent preparation precursor liquid;
(2) gained precursor liquid is applied to Sapphire Substrate, makes precursor film;
(3) gained precursor film is placed in to vacuum oven sintering, is incubated 0.5 ~ 20 hour, obtain vanadium dioxide film, wherein, sintering temperature is controlled at 400 DEG C ~ 600 DEG C, and sintering environment vacuum degree control is at 3 Pa ~ 15 Pa.
2. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: the soaking time optimization range described in step (3) is at 4h ~ 10h.
3. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: the sintering temperature optimization range described in step (3) is at 430 DEG C ~ 590 DEG C.
4. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: the sintering environment vacuum tightness optimization range described in step (3) is at 4Pa ~ 8Pa.
5. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: make after precursor film in step (2), it is carried out to drying and processing.
6. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 5, is characterized in that: described drying and processing, and its bake out temperature is no more than 300 DEG C, and drying time is no more than 15 minutes.
7. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: in the time that step (1) is prepared precursor liquid, add Glacial acetic acid as stablizer, the mass ratio of Glacial acetic acid and Triisopropoxyvanadium(V) oxide is 1:1 ~ 6:1.
8. the liquid phase preparation process of a kind of high orientation vanadium dioxide film according to claim 1, is characterized in that: in the precursor liquid of preparing in step (1), the mass volume ratio g:ml of Triisopropoxyvanadium(V) oxide and Virahol is 1-15:100.
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CN106012014A (en) * 2016-06-06 2016-10-12 电子科技大学 Vanadium dioxide film growing method
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CN112125337A (en) * 2020-10-16 2020-12-25 成都先进金属材料产业技术研究院有限公司 Method for preparing nano vanadium dioxide by using pentavalent vanadium alkoxide as raw material
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669248A (en) * 2016-01-04 2016-06-15 北京理工大学 Vanadium dioxide thin film having regular truss network structure and preparation method thereof
CN106012014A (en) * 2016-06-06 2016-10-12 电子科技大学 Vanadium dioxide film growing method
CN110306236A (en) * 2019-07-12 2019-10-08 暨南大学 Large scale V6O13Single-chip and preparation method thereof
CN110306236B (en) * 2019-07-12 2020-09-04 暨南大学 Large size V6O13Single chip and preparation method thereof
CN112125337A (en) * 2020-10-16 2020-12-25 成都先进金属材料产业技术研究院有限公司 Method for preparing nano vanadium dioxide by using pentavalent vanadium alkoxide as raw material
CN113880138A (en) * 2021-11-09 2022-01-04 成都先进金属材料产业技术研究院股份有限公司 VO (vanadium oxide) directly prepared by using triisopropoxide vanadium as vanadium source2Method (2)
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