CN101494170A - Method for preparing Sm2O3 film by microwave assisted hydrothermal process - Google Patents

Method for preparing Sm2O3 film by microwave assisted hydrothermal process Download PDF

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CN101494170A
CN101494170A CNA2009100211919A CN200910021191A CN101494170A CN 101494170 A CN101494170 A CN 101494170A CN A2009100211919 A CNA2009100211919 A CN A2009100211919A CN 200910021191 A CN200910021191 A CN 200910021191A CN 101494170 A CN101494170 A CN 101494170A
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hydrothermal
microwave
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CN101494170B (en
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殷立雄
黄剑锋
曹丽云
李娟莹
黄艳
马小波
朱佳
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention provides a microwave hydrothermal method which is used for preparing a Sm2O3 film. An analyzed pure SmC13 question mark 6H2O is added into deionized water and is stirred on a magnetic stirring apparatus so as to lead the analyzed pure SmC13 question mark 6H2O to dissolve and a solution A is obtained; the solution A is heated, stirred and mixed with hartshorn to adjust the pH value, and a solution B of which the pH value is 5.4 swung 6.0 is obtained; the solution B is poured into a microwave hydrothermal kettle, and a clean uropatagia is immersed into the solution B. Then the microwave hydrothermal kettle is sealed and put into a warm-pressing and double-control microwave hydrothermal reactor for hydro-thermal reaction; after the reaction, the kettle is naturally cooled to room temperature; and the hydrothermal kettle is opened, and the uropatagia is taken out, washed with absolute ethyl alcohol and placed in a vacuum drying chamber, and a Sm2O3 optical thin-film is obtained. As the preparation process of the invention is finished at a time in liquidoid and needs no crystallization heat treatment, thus avoiding the curling, season check and grain growth coarsening of the Sm2O3 film which can be caused in the heat treatment and the defects of film and underlay or atmosphere reaction and the like.

Description

A kind of microwave-hydrothermal method prepares Sm 2O 3The method of film
Technical field
The present invention relates to a kind of Sm 2O 3The thin film technology method, particularly a kind of microwave-hydrothermal method prepares Sm 2O 3The method of film.
Background technology
Sm 2O 3Be a kind of pale yellow powder, easily deliquescence is water insoluble, is soluble in inorganic acid.Sm 2O 3Conversion of Energy material and the optoelectronic thin film material of a new generation.Sm 2O 3Film can be used to prepare optical switch, data storage, photo-electric conversion element and electrical switch etc.; Sm 2O 3Film also can be used in the filter of electronics body, magnetic material and special glass; In addition nanometer Sm 2O 3Can also be used for ceramic capacitor and catalyst aspect, have wide development prospect should be arranged.
The preparation Sm that reports at present 2O 3The method of optical thin film is mainly vacuum evaporation [V.A.Rozhkov, A.Yu.Trusova, I.G.Berezhnoy.Silicon MIS structuresusing samarium oxide films.Thin Solid Films 325 (1998) 151-155] and the method [A.A.Dakhel.dielecyric and optical properties ofsamarium oxide thin films, Journal of Alloys and Compounds365 (2004) 233-239] of atmosphere evaporation.The method of vacuum evaporation is to heat Sm under vacuum condition 2O 3, obtain Sm in low temperature base version deposition 2O 3Film.The method of atmosphere evaporation is to heat Sm under oxygen atmosphere 2O 3, obtain Sm in low temperature base version deposition 2O 3Film.These two kinds of methods are all very high to equipment requirement, and equipment and instrument is relatively more expensive, owing to evaporation exists in whole container, to Sm 2O 3The utilization rate of raw material is very little.In order to reach practical purpose, must the low Sm of Development and Production cost 2O 3Optoelectronic film preparation technology.Other has the report standby Sm of hydro-thermal legal system 2O 3Optoelectronic film [Huang Jianfeng, Cao Liyun, Huang Yan etc. a kind of hydro-thermal prepares Sm 2O 3The method of film [P]. Chinese patent: 200510096004.5,2006-03-01.].
Summary of the invention
The object of the present invention is to provide a kind of microwave-hydrothermal method to prepare Sm 2O 3The method of film, this method equipment is simple, and preparation time is short, easily control, and synthesize cheaply Sm 2O 3Film.
For achieving the above object, the present invention adopts technical scheme to be:
1) at first, with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.05～0.4mol/L;
2) secondly, 45～55 ℃ of stirrings, and to adopt mass percent be that 5～10% ammonia spirit regulates that to make the pH value of solution be 5.4～6.0, stirs and form solution B after 3～5 hours with clear solution A;
3) then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 50～67%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 220～300 ℃, reaction time was controlled at 4～8 hours, and reaction naturally cools to room temperature after finishing;
4) last, open water heating kettle, take out substrate and wash 4 times with absolute ethyl alcohol, and place 80～120 ℃ vacuum drying chamber inner drying namely to obtain Sm at substrate surface 2O 3Optical thin film.
The present invention adopts microwave-hydrothermal method to prepare Sm 2O 3Optoelectronic film is because preparation Sm 2O 3The film reaction is once finished in liquid phase, does not need the crystallization and thermal treatment in later stage, thereby has avoided Sm 2O 3That film may cause in heat treatment process is curling, dry and cracked, grain coarsening and film and the defectives such as substrate or atmosphere reaction, and the Sm for preparing 2O 3Optoelectronic film purity is higher, controlled, even, fine and close, the no visible defects of grain growth, the film that presentation quality is higher, and apparatus and process is simple, and preparation time is short, has broad application prospects.
Embodiment
Embodiment 1: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.17mol/L; Secondly, 55 ℃ of stirrings, and to adopt mass percent be that 5% ammonia spirit regulates that to make the pH value of solution be 5.8, stirs and form solution B after 3 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 63%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 280 ℃, reacted 5 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 100 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Embodiment 2: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.25mol/L; Secondly, 48 ℃ of stirrings, and to adopt mass percent be that 8% ammonia spirit regulates that to make the pH value of solution be 5.6, stirs and form solution B after 5 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 58%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 250 ℃, reacted 6 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 80 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Embodiment 3: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.33mol/L; Secondly, 52 ℃ of stirrings, and to adopt mass percent be that 6% ammonia spirit regulates that to make the pH value of solution be 6.0, stirs and form solution B after 4 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 220 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 110 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Embodiment 4: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.05mol/L; Secondly, 45 ℃ of stirrings, and to adopt mass percent be that 9% ammonia spirit regulates that to make the pH value of solution be 5.5, stirs and form solution B after 5 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 55%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 260 ℃, reacted 7 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 90 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Embodiment 5: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.1mol/L; Secondly, 50 ℃ of stirrings, and to adopt mass percent be that 7% ammonia spirit regulates that to make the pH value of solution be 5.7, stirs and form solution B after 3 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 50%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 300 ℃, reacted 4 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 120 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Embodiment 6: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.4mol/L; Secondly, 53 ℃ of stirrings, and to adopt mass percent be that 10% ammonia spirit regulates that to make the pH value of solution be 5.4, stirs and form solution B after 4 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 60%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 240 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 105 ℃ vacuum drying chamber inner drying promptly can obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
Because the present invention prepares Sm 2O 3The film reaction is once finished in liquid phase, does not need the crystallization and thermal treatment in later stage, thereby has avoided Sm 2O 3That film may cause in heat treatment process is curling, dry and cracked, grain coarsening and film and the defectives such as substrate or atmosphere reaction, and process equipment is simple, and gained film purity is higher, and grain growth is controlled.Can prepare evenly, densification, no visible defects, the higher film of presentation quality, prepared film shows certain oriented growth trend, and film has the strong absorption effect and visible light is had strong anti-reflection effect ultraviolet ray.And utilize the microwave hydrothermal method can better improve the quality of film and shorten the reaction time than simple hydro thermal method.

Claims (7)

1, a kind of microwave-hydrothermal method prepares Sm 2O 3The method of film is characterized in that:
1) at first, with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.05～0.4mol/L;
2) secondly, 45～55 ℃ of stirrings, and to adopt mass percent be that 5～10% ammonia spirit regulates that to make the pH value of solution be 5.4～6.0, stirs and form solution B after 3～5 hours with clear solution A;
3) then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 50～67%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 220～300 ℃, reaction time was controlled at 4～8 hours, and reaction naturally cools to room temperature after finishing;
4) last, open water heating kettle, take out substrate and wash 4 times with absolute ethyl alcohol, and place 80～120 ℃ vacuum drying chamber inner drying namely to obtain Sm at substrate surface 2O 3Optical thin film.
2, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.17mol/L; Secondly, 55 ℃ of stirrings, and to adopt mass percent be that 5% ammonia spirit regulates that to make the pH value of solution be 5.8, stirs and form solution B after 3 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 63%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the MDS-8 type temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 280 ℃, reacted 5 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 100 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
3, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.25mol/L; Secondly, 48 ℃ of stirrings, and to adopt mass percent be that 8% ammonia spirit regulates that to make the pH value of solution be 5.6, stirs and form solution B after 5 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 58%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 250 ℃, reacted 6 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 80 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
4, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.33mol/L; Secondly, 52 ℃ of stirrings, and to adopt mass percent be that 6% ammonia spirit regulates that to make the pH value of solution be 6.0, stirs and form solution B after 4 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 67%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 220 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 110 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
5, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.05mol/L; Secondly, 45 ℃ of stirrings, and to adopt mass percent be that 9% ammonia spirit regulates that to make the pH value of solution be 5.5, stirs and form solution B after 5 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 55%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 260 ℃, reacted 7 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 90 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
6, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.1mol/L; Secondly, 50 ℃ of stirrings, and to adopt mass percent be that 7% ammonia spirit regulates that to make the pH value of solution be 5.7, stirs and form solution B after 3 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 50%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 300 ℃, reacted 4 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 120 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
7, microwave-hydrothermal method according to claim 1 prepares Sm 2O 3The method of film is characterized in that: at first, and with analytically pure SmCl 36H 2O adds in the deionized water, stirs on magnetic stirring apparatus and makes its dissolving, makes Sm 3+Concentration is the clear solution A of 0.4mol/L; Secondly, 53 ℃ of stirrings, and to adopt mass percent be that 10% ammonia spirit regulates that to make the pH value of solution be 5.4, stirs and form solution B after 4 hours with clear solution A; Then, solution B is poured in the microwave hydrothermal still, compactedness is controlled at 60%, the substrate that cleans up is immersed in the solution B, seal the microwave hydrothermal still then, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 240 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, take out substrate and wash 4 times, and place 105 ℃ vacuum drying chamber inner drying promptly to obtain Sm at substrate surface with absolute ethyl alcohol 2O 3Optical thin film.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102330081A (en) * 2011-10-13 2012-01-25 陕西科技大学 Method for preparing Sm2O3 film by solvent heat method
CN104071821A (en) * 2014-06-20 2014-10-01 陕西科技大学 Method for preparing Sm(OH)3/ZnO composite film by using homogeneous hydrothermal method
CN104556201A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm(OH3)3/CuO nano composite by microwave-hydrothermal process
CN105110653A (en) * 2015-07-27 2015-12-02 陕西科技大学 Sol-gel preparation method of Sm2O3 film from sol prepared by peptization method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102330081A (en) * 2011-10-13 2012-01-25 陕西科技大学 Method for preparing Sm2O3 film by solvent heat method
CN104071821A (en) * 2014-06-20 2014-10-01 陕西科技大学 Method for preparing Sm(OH)3/ZnO composite film by using homogeneous hydrothermal method
CN104071821B (en) * 2014-06-20 2015-11-04 陕西科技大学 A kind of homogeneous phase hydrothermal method that adopts prepares Sm (OH) 3the method of/ZnO laminated film
CN104556201A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm(OH3)3/CuO nano composite by microwave-hydrothermal process
CN104556201B (en) * 2015-01-19 2016-03-30 陕西科技大学 A kind of microwave-hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex
CN105110653A (en) * 2015-07-27 2015-12-02 陕西科技大学 Sol-gel preparation method of Sm2O3 film from sol prepared by peptization method

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