CN1740389A - Hydrothermal Sm2O3 film preparing process - Google Patents

Hydrothermal Sm2O3 film preparing process Download PDF

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Publication number
CN1740389A
CN1740389A CN 200510096004 CN200510096004A CN1740389A CN 1740389 A CN1740389 A CN 1740389A CN 200510096004 CN200510096004 CN 200510096004 CN 200510096004 A CN200510096004 A CN 200510096004A CN 1740389 A CN1740389 A CN 1740389A
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water heating
heating kettle
coating liquid
solution
hours
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CN 200510096004
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CN100359044C (en
Inventor
黄剑锋
曹丽云
黄艳
吴建鹏
贺海燕
朱广燕
邓飞
马小波
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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 hydrothermal process of preparing Sm2O3 film includes the following steps: dissolving SmCl3.6H2O in distilled water to compound transparent solution; regulating the pH value of the solution with ammonia water solution to 5.6-5.9 to form the film plating liquid; pouring the film plating liquid into hydrothermal reactor, soaking substrate inside the film plating liquid, sealing the hydrothermal reactor, setting the hydrothermal reactor inside one thermotank at 160-300 deg.c, controlling hydrothermal pressure at 2-20 MPa and maintaining for 24-72 hr before cooling naturally to room temperature; opening the hydrothermal reactor, taking the substrate, drying the substrate in a stove at 60-100 deg.c for 3-24 hr to obtain photoelectronic Sm2O3 film on the surface of the substrate. The said process is simple, and the Sm2O3 film has high purity and controllable crystal grain growth.

Description

A kind of hydrothermal preparation Sm 2O 3The method of film
Technical field
The present invention relates to a kind of preparation Sm 2O 3The method of film, particularly a kind of hydrothermal preparation 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 mineral acid.Sm 2O 3Be the Conversion of energy material of a new generation, have wide development prospect should be arranged.Sm 2O 3Optical thin film is 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 in addition 2O 3Film also serves many purposes, and can be used for electronics body and magneticsubstance, can be used in the spectral filter of special glass; Nanometer Sm 2O 3Can also be used for ceramic condenser and catalyzer aspect.In a word, Sm 2O 3This novel material of film has broad application prospects.
The preparation Sm that is reported at present 2O 3The method of optical thin film is mainly vacuum evaporation [V.A.Rozhkov, A.Yu.Trusova, I.G.Berezhnoy.Silicon MIS structures using samariumoxide films.Thin Solid Films 325 (1998) 151-155] and the method [A.A.Dakhel.dielecyric and optical properties of samarium oxide thinfi lms, Journal of Alloys and Compounds 365 (2004) 233-239] of atmosphere evaporation.The method of vacuum evaporation is to heat Sm under vacuum condition 2O 3, deposition obtains Sm on low temperature base version 2O 3Film.The method of atmosphere evaporation is to heat Sm under oxygen atmosphere 2O 3, deposition obtains Sm on low temperature base version 2O 3Film.These two kinds of methods are all very high to equipment requirements, and equipment and instrument is relatively more expensive, owing to evaporation exists in entire container, to Sm 2O 3Utilization ratio of raw materials is very little.In order to reach the purpose of practicability, must the low Sm of Development and Production cost 2O 3Optoelectronic film preparation technology.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the hydrothermal preparation Sm that a kind of preparation technology is simple, cost is low is provided 2O 3The method of film.
For achieving the above object, the technical solution used in the present invention is: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.05-0.1mol/L; 45～55 ℃ of heated and stirred, and to adopt mass percent be the pH value of the ammonia soln regulator solution of 5-10% with this solution, and the pH value that makes solution is 5.6～5.9, stirs the even colloidal sol of formation after 1-3 hour, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 50-80%, and substrate is immersed in the coating liquid, seal water heating kettle then, water heating kettle is placed 160-300 ℃ of constant temperature oven, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 24～72 hours at 2-20MPa; Open water heating kettle, take out substrate and place 60-100 ℃ baking oven inner drying promptly can obtain Sm after 3-24 hour at substrate surface 2O 3Optoelectronic film.
Because the present invention prepares Sm 2O 3Film is reflected in the liquid phase and once finishes, and does not need subsequent crystallization heat treatment, thereby has avoided Sm 2O 3That film may cause in heat treatment process is curling, dry and cracked, grain coarsening and film and defectives such as substrate or atmosphere reaction, and processing unit is simple, and gained film purity is higher, and grain growing is controlled.
Description of drawings
Accompanying drawing is the Sm that makes according to preparation method of the present invention 2O 3Film SPA400-SPI3800N type afm scan figure.
Embodiment
Embodiment 1: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.05mol/L; 55 ℃ of heated and stirred, and to adopt mass percent be the pH value of 10% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.6, stirs the even colloidal sol of formation after 1 hour, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 80%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 160 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 24 hours at 20MPa; Open water heating kettle, take out substrate and place 80 ℃ baking oven inner drying promptly can obtain Sm after 18 hours at substrate surface 2O 3Optoelectronic film.
Embodiment 2: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.1mol/L; 49 ℃ of heated and stirred, and to adopt mass percent be the pH value of 8% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.9, stirs the even colloidal sol of formation after 3 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 50%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 300 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 72 hours at 8MPa; Open water heating kettle, take out substrate and place 60 ℃ baking oven inner drying promptly can obtain Sm after 24 hours at substrate surface 2O 3Optoelectronic film.
Embodiment 3: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.08mol/L; 45 ℃ of heated and stirred, and to adopt mass percent be the pH value of 5% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.8, stirs the even colloidal sol of formation after 2 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 60%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 250 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 36 hours at 15MPa; Open water heating kettle, take out substrate and place 100 ℃ baking oven inner drying promptly can obtain Sm after 3 hours at substrate surface 2O 3Optoelectronic film.
Embodiment 4: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.06mol/L; 52 ℃ of heated and stirred, and to adopt mass percent be the pH value of 7% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.7, stirs the even colloidal sol of formation after 2 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 70%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 180 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 48 hours at 2MPa; Open water heating kettle, take out substrate and place 70 ℃ baking oven inner drying promptly can obtain Sm after 12 hours at substrate surface 2O 3Optoelectronic film.
Embodiment 5: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.07mol/L; 50 ℃ of heated and stirred, and to adopt mass percent be the pH value of 9% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.9, stirs the even colloidal sol of formation after 3 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 65%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 200 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 56 hours at 10MPa; Open water heating kettle, take out substrate and place 90 ℃ baking oven inner drying promptly can obtain Sm after 20 hours at substrate surface 2O 3Optoelectronic film.
Embodiment 6: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.09mol/L; 47 ℃ of heated and stirred, and to adopt mass percent be the pH value of 6% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.6, stirs the even colloidal sol of formation after 1 hour, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 75%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 270 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 40 hours at 18MPa; Open water heating kettle, take out substrate and place 75 ℃ baking oven inner drying promptly can obtain Sm after 15 hours at substrate surface 2O 3Optoelectronic film.
The Sm that makes according to preparation method of the present invention 2O 3Film purity height, good uniformity, film combine with substrate firmly, not only are not subjected to substrate shape and limitation of size, and can control film crystallite dimension size by temperature of reaction and pressure; And the preparation film do not need subsequent crystallization heat treatment, thus curling, dry and cracked, the grain coarsening of having avoided that film may cause in heat treatment process and film and defectives such as substrate or atmosphere reaction.
Referring to accompanying drawing, with the Sm of the present invention's preparation 2O 3Film is found to be the Sm of crystallite with Japanese D/max2000PCX x ray diffractometer x analytic sample of science 2O 3Film.With this film with SPA400-SPI3800N type afm scan, from photo as can be seen gained film evenly, fine and close, do not have and curl and defectives such as cracking even particle size.

Claims (7)

1, a kind of hydrothermal preparation Sm 2O 3The method of film is characterized in that:
1) at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.05-0.1mol/L;
2) with this solution 45～55 ℃ of heated and stirred, and to adopt mass percent be the pH value of the ammonia soln regulator solution of 5-10%, the pH value that makes solution is 5.6～5.9, stirs the even colloidal sol of formation after 1-3 hour, and is standby as coating liquid;
3) above-mentioned coating liquid is poured in the water heating kettle, compactedness is controlled at 50-80%, and substrate is immersed in the coating liquid, seal water heating kettle then, water heating kettle is placed 160-300 ℃ of constant temperature oven, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 24～72 hours at 2-20MPa;
4) open water heating kettle, take out substrate and place 60-100 ℃ baking oven inner drying promptly can obtain Sm after 3-24 hour at substrate surface 2O 3Optoelectronic film.
2, hydrothermal preparation Sm according to claim 1 2O 3The method of film is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.05mol/L; 55 ℃ of heated and stirred, and to adopt mass percent be the pH value of 10% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.6, stirs the even colloidal sol of formation after 1 hour, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 80%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 160 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 24 hours at 20MPa; Open water heating kettle, take out substrate and place 80 ℃ baking oven inner drying promptly can obtain Sm after 18 hours at substrate surface 2O 3Optoelectronic film.
3, hydrothermal preparation Sm according to claim 1 2O 3The method of film is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.1mol/L; 49 ℃ of heated and stirred, and to adopt mass percent be the pH value of 8% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.9, stirs the even colloidal sol of formation after 3 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 50%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 300 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 72 hours at 8MPa; Open water heating kettle, take out substrate and place 60 ℃ baking oven inner drying promptly can obtain Sm after 24 hours at substrate surface 2O 3Optoelectronic film.
4, the method for hydrothermal preparation Sm2O3 film according to claim 1 is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.08mol/L; 45 ℃ of heated and stirred, and to adopt mass percent be the pH value of 5% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.8, stirs the even colloidal sol of formation after 2 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 60%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 250 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 36 hours at 15MPa; Open water heating kettle, take out substrate and place 100 ℃ baking oven inner drying promptly can obtain Sm after 3 hours at substrate surface 2O 3Optoelectronic film.
5, the method for hydrothermal preparation Sm2O3 film according to claim 1 is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.06mol/L; 52 ℃ of heated and stirred, and to adopt mass percent be the pH value of 7% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.7, stirs the even colloidal sol of formation after 2 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 70%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 180 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 48 hours at 2MPa; Open water heating kettle, take out substrate and place 70 ℃ baking oven inner drying promptly can obtain Sm after 12 hours at substrate surface 2O 3Optoelectronic film.
6, the method for hydrothermal preparation Sm2O3 film according to claim 1 is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.07mol/L; 50 ℃ of heated and stirred, and to adopt mass percent be the pH value of 9% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.9, stirs the even colloidal sol of formation after 3 hours, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 65%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 200 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 56 hours at 10MPa; Open water heating kettle, take out substrate and place 90 ℃ baking oven inner drying promptly can obtain Sm after 20 hours at substrate surface 2O 3Optoelectronic film.
7, the method for hydrothermal preparation Sm2O3 film according to claim 1 is characterized in that: at first with SmCl 36H 2O is dissolved in the distilled water, is mixed with Sm 3+Concentration is the clear solution of 0.09mol/L; 47 ℃ of heated and stirred, and to adopt mass percent be the pH value of 6% ammonia soln regulator solution with this solution, and the pH value that makes solution is 5.6, stirs the even colloidal sol of formation after 1 hour, and is standby as coating liquid; Above-mentioned coating liquid is poured in the water heating kettle, and compactedness is controlled at 75%, and substrate is immersed in the coating liquid, seals water heating kettle then, and water heating kettle is placed 270 ℃ of constant temperature ovens, and the hydro-thermal pressure-controlling is incubated and naturally cools to room temperature after 40 hours at 18MPa; Open water heating kettle, take out substrate and place 75 ℃ baking oven inner drying promptly can obtain Sm after 15 hours at substrate surface 2O 3Optoelectronic film.
CNB2005100960045A 2005-09-08 2005-09-08 Hydrothermal Sm2O3 film preparing process Expired - Fee Related CN100359044C (en)

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Cited By (2)

* 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
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

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1174578A (en) * 1997-08-29 1999-03-16 Ube Ind Ltd Piezoelectric element and its manufacture
CN1128894C (en) * 2001-02-13 2003-11-26 中国科学技术大学 Alkaline rare earth-carbonate crystical film and its hydrothermal preparing process
CN1493519A (en) * 2002-10-29 2004-05-05 北京有色金属研究总院 Preparation of cerium zirconium composite oxide using coprecipitation-high pressure water heat combining method
CN1216803C (en) * 2003-01-10 2005-08-31 清华大学 Rare earth hydroxide nano tubes and synthesis of serial rare earth compounds nano tubes
CN1258828C (en) * 2004-02-13 2006-06-07 清华大学 Process for preparing proton exchange film fuel cell multi component catalyst

Cited By (2)

* 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
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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Denomination of invention: Method for preparing Sm*O* film by hydrothermal method

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