CN101486483B - Method for preparing SmS film by microwave-hydrothermal method - Google Patents

Method for preparing SmS film by microwave-hydrothermal method Download PDF

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CN101486483B
CN101486483B CN2009100211938A CN200910021193A CN101486483B CN 101486483 B CN101486483 B CN 101486483B CN 2009100211938 A CN2009100211938 A CN 2009100211938A CN 200910021193 A CN200910021193 A CN 200910021193A CN 101486483 B CN101486483 B CN 101486483B
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smcl
deionized water
gas
hydrothermal
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CN101486483A (en
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殷立雄
黄剑锋
曹丽云
马小波
黄艳
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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 discloses a method for preparing SmS film by a microwave hydro-thermal method, wherein, Ar gas is led into de-ionized water for removing O2 in the water; and then analytically pure SmCl3 question mark 6H2 and Na2S2O3 question mark 5H2O are respectively dissolved in the de-ionized water with the Ar gas to prepare an SmCl3 solution and an Na2S2O3 solution; the SmCl3 solution and the Na2S2O3 solution are mixed and poured into a microwave hydro-thermal kettle, and then a cleaned basal piece is arranged in the microwave hydro-thermal kettle which is sealed and then put into a warm-pressing dual-control microwave hydro-thermal reactor for carrying out hydro-thermal reaction and is then naturally cooled to the room temperature; and the hydro-thermal kettle is opened, and the basal piece is washed by absolute ethyl alcohol or isopropyl alcohol and then arranged in an electric vacuum drying oven for drying. The method for preparing the SmS film is completed by one-time operation in the liquid phase, without post crystallization heat treatment, thus avoiding possible defects such as curl, dry cracking, grain growth coarsening and reaction between the film and a substrate or air, and the like, which are caused in the heat treatment of the SmS film.

Description

A kind of method of preparing SmS film by microwave-hydrothermal method
Technical field
The present invention relates to a kind of preparation method of SmS film, particularly a kind of microwave hydrothermal prepares the method for SmS film.
Background technology
The SmS crystal can experience one its color is by the black-and-blue golden yellow that becomes after the phase transformation from the semiconductor phase transformation of metal phase in opposite directions under the stress of 6.5 * 108Pa, and crystal structure does not change.And this phase transformation is reversible, and after stress was eliminated, the SmS crystal can change the semiconductor phase into again.Because it has the cause that optical property between two-phase and the two-phase has notable difference, is considered to one of the most promising holographic recording storage medium.
Because optics, electricity and the magnetic performance of significant difference before and after the special phase transformation of SmS and the phase transformation thereof, it can be used in many aspects.Development along with hi-tech, the purposes of SmS film will be more and more widely, [M.P.Petrov.Holographics Storage in SmSThin Films[J] .Optics Communications except that can be used for holographic recording and storing, 1977,22 (3): 293.], also can be used for optical switch, minimal stress meter and pressure-active element etc.After undergoing phase transition, the optical property of SmS film can be from visible light to region of ultra-red generation significant change, by certain information short time is added on the light wave, light path is changed, make to be in and connect or block state, therefore can be used for making optical switch [Charles B, reenberg.Optically switchable thin films:a review.ThinSolid Films, 1994,251:81.], can pass through laser or its on off state of pressure control.Under certain pressure, the resistivity and the reflectivity of SmS film also change along with pressure, therefore can also be used to making the minimal stress meter [Vasil ' ev, L.N.; Kaminskii, V.V.; Kurapov, Yu.M.Conductivity of SmS thin films[J] .Fizika Tverdogo Tela, 1996,38 (3): 779-785.] and pressure-active element [Matsubayashi Kazuyuki, Mukai Hitoshi, Tsuzuki Takashi, et al.Insulator-metal transition studied by heatcapacity measurements on SmS[J] .Physica B:Condensed Matter (Amsterdam, Netherlands), 2003, (329-333): 484.].Control temperature cycles or laser and/write, can in the SmS film, wipe and write data, thereby with SmS film making optical digital reservoir [Tanemura S, Miao L, Koide S.Optical propertiesof metal and semiconductor SmS thin films fabricated by rf/dc dualmagnetron sputtering.Applied Surface Science, 2004,238 (1-4): 360.].In addition, also can consider the SmS film is applied to holographic security technology.
At present, the preparation method of SmS film mainly contains sputtering method [Huang Jianfeng, Cao Liyun. the dual-target sputtering legal system is made the SmS optical thin film. Rare Metals Materials and engineering, 2004,33 (3): 333.], reactive vapour deposition method [C F Hickey, U J Gibson.SmS phase transition in thinfilms prepared by reactive evaporation[J] .Phase Transitions, 1989,14:187.], pulsed laser deposition [P Miodushevsky, M L Protopapa, F De Tomasi.Fine trimming of SmS film resistance by XeCl laserablation[J] .Thin Solid Films, 2000,359:251.] and mocvd method [VolodinN M, Zavyalova L V, Kirillov AI, et al.Investigation of growthconditions crystal structure and surface morphology of SmS filmsfabricated by MOCVD technique[J] .Kvantova ta Optoelektronika, 1999,2 (2): 78.] etc.It is relatively more expensive that these methods prepare SmS film equipment needed thereby, and cost is higher, and technology is difficult to control.Report in addition favourable with electrochemical process prepare the SmS film [Huang Jianfeng, horse small echo, Cao Liyun, Wu Jianpeng. a kind of preparation method of optical thin-membrane with samarium sulfide holographic recording [P]. Chinese patent: 200610041907.8,2008-01-02.].
Summary of the invention
The object of the present invention is to provide a kind of equipment simple, preparation time is short, easily control, the method of the preparing SmS film by microwave-hydrothermal method that synthetic cost is low, the SmS optoelectronic film purity of making by preparation method of the present invention is higher, grain growth is controlled, evenly, densification, no visible defects, presentation quality be higher.
For achieving the above object, the technical solution used in the present invention is:
1) at first, in deionized water, passes into Ar gas except the O in anhydrating 2
2) then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.05～0.4mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.05～0.4mol/L 2S 2O 3Solution;
3) secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 2: 1～1: 6 volume ratio, stirs, and be 3～3.5 with the HCl regulator solution pH value of 0.05mol/L;
4) above-mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 50～67%, the substrate that has cleaned is placed in one, sealing microwave hydrothermal still, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 160～300 ℃, reacts 4～8 hours, and reaction naturally cools to room temperature after finishing;
5) last, open water heating kettle, substrate with absolute ethyl alcohol or washed with isopropyl alcohol 4 times, and is promptly obtained the SmS optical thin film at substrate surface after placing 40～60 ℃ electric vacunm drying case inner drying.
Because the present invention prepares the SmS film and is reflected in the liquid phase and once finishes, do not need subsequent crystallization heat treatment, thereby curling, dry and cracked, the grain coarsening of having avoided that the SmS film may cause in heat treatment process and film and defectives such as substrate or atmosphere reaction, and process equipment is simple, gained film purity is higher, and grain growth is controlled.The film of preparing evenly, densification, no visible defects, the higher film of presentation quality, measured its optical property by ultraviolet spectrophotometer, the prepared SmS film of ultraviolet spectrum test shows has the ultraviolet absorption characteristic of 290-300nm.And utilize the microwave hydrothermal method can better improve quality and the Reaction time shorten of film than simple hydro-thermal method and the electrochemistry precipitation method.
Embodiment
Embodiment 1: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.1mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.1mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 2: 1 volume ratio, stirs, and be 3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 60%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 200 ℃, reacts 7 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 50 ℃ electric vacunm drying case inner drying.
Embodiment 2: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.3mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.2mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 1 volume ratio, stirs, and be 3.2 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 55%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 230 ℃, reacts 6 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 48 ℃ electric vacunm drying case inner drying.
Embodiment 3: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.05mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.3mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution according to 1: 3, volume ratio mix, stir, be 3.4 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 58%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 270 ℃, reacts 5 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 57 ℃ electric vacunm drying case inner drying.
Embodiment 4: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.2mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.05mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 5 volume ratio, stirs, and be 3.1 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 63%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 180 ℃, reacts 8 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 45 ℃ electric vacunm drying case inner drying.
Embodiment 5: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.4mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.4mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution according to 1: 2, volume ratio mix, stir, be 3.5 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 52%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 300 ℃, reacts 4 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 60 ℃ electric vacunm drying case inner drying.
Embodiment 6: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.15mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.35mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 6 volume ratio, stirs, and be 3.3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 67%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 250 ℃, reacts 6 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 55 ℃ electric vacunm drying case inner drying.
Embodiment 7: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.35mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.15mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1.5: 1 volume ratio, stirs, and be 3.5 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 50%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 160 ℃, reacts 8 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 40 ℃ electric vacunm drying case inner drying.
Embodiment 8: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.25mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.25mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 4 volume ratio, stirs, and be 3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 65%, clean substrate is placed in one, sealing microwave hydrothermal still, put it in the MDS-8 type warm-pressing double-control microwave hydrothermal reaction, hydrothermal temperature is controlled at 280 ℃, reacts 4 hours, and reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 53 ℃ electric vacunm drying case inner drying.

Claims (9)

1. the method for a preparing SmS film by microwave-hydrothermal method is characterized in that:
1) at first, in deionized water, passes into Ar gas except the O in anhydrating 2
2) then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.05～0.4mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.05～0.4mol/L 2S 2O 3Solution;
3) secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 2: 1～1: 6 volume ratio, stirs, and be 3～3.5 with the HCl regulator solution pH value of 0.05mol/L;
4) above-mentioned solution is poured in the microwave hydrothermal still, compactedness is controlled at 50～67%, the substrate that has cleaned is placed in one, sealing microwave hydrothermal still, put it in the two control of the temperature and pressure microwave hydrothermal reaction, hydrothermal temperature is controlled at 160～300 ℃, reacts 4～8 hours, and reaction naturally cools to room temperature after finishing;
5) last, open water heating kettle, substrate with absolute ethyl alcohol or washed with isopropyl alcohol 4 times, and is promptly obtained the SmS optical thin film at substrate surface after placing 40～60 ℃ electric vacunm drying case inner drying.
2. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.1mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.1mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 2: 1 volume ratio, stirs, and be 3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 60%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 200 ℃, reacted 7 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 50 ℃ electric vacunm drying case inner drying.
3. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.3mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.2mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 1 volume ratio, stirs, and be 3.2 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 55%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 230 ℃, reacted 6 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 48 ℃ electric vacunm drying case inner drying.
4. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.05mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.3mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution according to 1: 3, volume ratio mix, stir, be 3.4 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 58%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 270 ℃, reacted 5 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 57 ℃ electric vacunm drying case inner drying.
5. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.2mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.05mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 5 volume ratio, stirs, and be 3.1 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 63%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 180 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 45 ℃ electric vacunm drying case inner drying.
6. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.4mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.4mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution according to 1: 2, volume ratio mix, stir, be 3.5 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 52%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 300 ℃, reacted 4 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 60 ℃ electric vacunm drying case inner drying.
7. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.15mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.35mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 6 volume ratio, stirs, and be 3.3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 67%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 250 ℃, reacted 6 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 55 ℃ electric vacunm drying case inner drying.
8. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.35mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.15mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1.5: 1 volume ratio, stirs, and be 3.5 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 50%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 160 ℃, reacted 8 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with absolute ethanol washing 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 40 ℃ electric vacunm drying case inner drying.
9. the method for preparing SmS film by microwave-hydrothermal method according to claim 1 is characterized in that: at first, pass into Ar gas except the O in anhydrating in deionized water 2Then, with analytically pure SmCl 36H 2O dissolves in the deionized water that passes into Ar gas, is configured to the SmCl that concentration is 0.25mol/L 3Solution is with analytically pure Na 2S 2O 35H 2O dissolves in the deionized water that passes into Ar gas, is configured to the Na of 0.25mol/L 2S 2O 3Solution; Secondly, with SmCl 3Solution and Na 2S 2O 3Solution mixes according to 1: 4 volume ratio, stirs, and be 3 with the HCl regulator solution pH value of 0.05mol/L; Mentioned solution is poured in the microwave hydrothermal still, and compactedness is controlled at 65%, and clean substrate is placed in one, sealing microwave hydrothermal still puts it in the warm-pressing double-control microwave hydrothermal reaction, and hydrothermal temperature is controlled at 280 ℃, reacted 4 hours, reaction naturally cools to room temperature after finishing; At last, open water heating kettle, substrate with washed with isopropyl alcohol 4 times, and is namely obtained the SmS optical thin film at substrate surface after placing 53 ℃ electric vacunm drying case inner drying.
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CN102394224B (en) * 2011-11-23 2013-05-15 陕西科技大学 Preparation method of chloro silane-samaric sulfide film on single crystal silicon surface
CN102503552B (en) * 2011-11-23 2013-04-10 陕西科技大学 Preparation method of monocrystalline silicon surface aminosilane-samarium sulfide film
CN102424997A (en) * 2011-11-23 2012-04-25 陕西科技大学 Method for preparing SmS film through electrodeposition-liquid phase self assembly
CN102418139B (en) * 2011-11-23 2014-08-27 陕西科技大学 Method for preparing oriented grown samarium sulfide film (311) by hydrothermal assisted liquid-phase self-assembly
CN102515239B (en) * 2011-11-23 2014-03-12 陕西科技大学 Method for preparing samarium sulphide film by microwave-assisted liquid phase reduction process
CN104193183A (en) * 2014-08-01 2014-12-10 浙江大学 Method for preparing thick film based on microcrystalline glass substrate
CN106277054B (en) * 2016-07-26 2017-10-13 陕西科技大学 One kind prepares tubulose SmS CrS2The method that interlayer mismatches compound

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