CN102424960A - Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process - Google Patents

Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process Download PDF

Info

Publication number
CN102424960A
CN102424960A CN2011103764441A CN201110376444A CN102424960A CN 102424960 A CN102424960 A CN 102424960A CN 2011103764441 A CN2011103764441 A CN 2011103764441A CN 201110376444 A CN201110376444 A CN 201110376444A CN 102424960 A CN102424960 A CN 102424960A
Authority
CN
China
Prior art keywords
silicon substrate
solution
film
ots
thin film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2011103764441A
Other languages
Chinese (zh)
Inventor
黄剑锋
侯艳超
张烨
曹丽云
殷立雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN2011103764441A priority Critical patent/CN102424960A/en
Publication of CN102424960A publication Critical patent/CN102424960A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Silicon Compounds (AREA)

Abstract

The invention discloses a method for preparing an (105) oriented-growth Sm2S3 thin film by a liquid phase self-assembly process, which comprises: adding SmCl3.6H2O into deionized water, uniformly stirring, adding citric acid and sodium thiosulfate, regulating the pH value to 2.0 to 6.0, and obtaining a precursor solution D; immersing a hydroxylated silicon substrate in octadecyltrichlorosilane (OTS), washing the substrate with acetone and carbon tetrachloride respectively, and drying by blowing nitrogen; placing the dried hydroxylated silicon substrate in an ultraviolet radiation meter for light excitation, and obtaining functionalized silicon substrate; and placing the functionalized silicon substrate in the precursor solution D and drying under vacuum to obtain Sm2S3 nano thin film. Because the method adopts the self-assembly process, the prepared Sm2S3 nano thin film is uniform, compact and dense and has fewer drawbacks and high strength; and by controlling the concentration and pH value of the precursor solution and the deposition time, the thickness of the thin film and grain size can be controlled.

Description

A kind of liquid phase self-assembly method preparation (105) oriented growth Sm 2S 3The method of film
Technical field
The present invention relates to a kind of Sm 2S 3The preparation method of film is specifically related to a kind of liquid phase self-assembly method preparation (105) oriented growth Sm 2S 3The method of film.Be a kind of can preparing evenly, densification, low defective, intensity is high, does not need the preparation method of the nano thin-film of later stage crystallization processing.
Background technology
Sm 2S 3Two kinds of forms are arranged, and are respectively α-Sm 2S 3Type and γ-Sm 2S 3Type.α-Sm 2S 3Be Th 3P 4Structure, irreversible conversion takes place when 1573 ± 50k, become γ-Sm 2S 3γ-Sm 2S 3Bright-colored, often be used as plastics and paint pigment.γ-Sm in addition 2S 3Being semi-conductor, is good thermo-electric converting material [Michihiro Ohta, Haibin Yuan, Shinji Hirai, Yoichiro Uemura, Kazuyoshi Shimakage.Preparation ofR 2S 3(R:La, Pr, Nd, Sm) powders by sulfurization of oxide powders usingCS 2Gas [J] .Journal of Alloys and Compounds.2004,374:112～115].Up to the present, about Sm 2S 3Research also seldom.
And self-assembly (Self-assembled monolayers) technology (being called for short the SAMs technology); Be a kind of new technology for preparing film,, on baseplate material, form marshalling from group through the chemisorption between tensio-active agent and the substrate; Densification, orderly unit molecule rete.With the self-assembled film is that the inorganic precursor solution of template-mediated deposits film forming bionical synthetic masking technique at substrate surface; Has the unrivaled advantage of conventional physical chemical process; Be a kind of have application prospect novel, green masking technique [is talked Guoqiang efficiently; Liu Jian, He Zhongliang. the self-assembled monolayer membrane technique and the preparation function film Application for Field [J]. ceramic .2009,7:9～13].This film-forming method is easy and simple to handle, and cost is low, does not need specific installation, and even, fine and close, the low defective of the film of preparing, and intensity is high, and bonding force is good, does not need the later stage crystallization to handle.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, liquid phase self-assembly method preparation (105) oriented growth Sm with low cost 2S 3The method of film.The prepared film that goes out is even, densification, and low defective, intensity is high, and bonding force is good, does not need the later stage crystallization to handle, and is functional.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gets the analytically pure (SmCl of 0.3-1.5g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 10-50mL;
2) in solution A, add the Hydrocerol A of 0.01-1.00g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 0.01-10.00g 2S 2O 3) stir solution C;
4) use the pH value of ammoniacal liquor regulator solution C to get precursor liquid D as 2.0-6.0;
5) hydroxylated silicon substrate being placed volumetric concentration is that the toluene solution of 1～2% OTS (octadecyl trichlorosilane) at room temperature soaks 10～40min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 100～120 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 1～4cm, irradiation 5～60min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 40～90 ℃ of deposit 1-50h 2S 3Film places 50～90 ℃ of drying 5～20min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
Described hydroxylated silicon substrate is that silicon substrate is immersed in the chloroazotic acid, uses behind ultrasonic oscillation 30min～3h naturally cooling at room temperature, and then cleans repeatedly with deionized water, uses N 2Dry up, in the uviolizing appearance, irradiation 20～80min gets hydroxylated silicon substrate then.
Because the present invention adopts the liquid phase self-assembling method, the Sm that makes 2S 3Nano thin-film, evenly, densification, low defective, intensity is high, and can control film thickness and grain size through control precursor liquid concentration, pH value and depositing time.The Sm of this method preparation 2S 3Nano thin-film repeatability is high, is easy to big area system film.And easy to operate, raw material is easy to get, and preparation cost is lower.
Description of drawings
Fig. 1 is the prepared Sm of the embodiment of the invention 1 2S 3Film XRD figure spectrum;
Fig. 2 is the prepared Sm of the embodiment of the invention 1 2S 3The AFM figure of film.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) gets the analytically pure (SmCl of 0.3g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 10mL;
2) in solution A, add the Hydrocerol A of 0.01g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 0.2g 2S 2O 3) stir solution C;
4) using the pH value of ammoniacal liquor regulator solution C is 2.0 must precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, uses behind the ultrasonic oscillation 30min naturally cooling at room temperature, and then clean repeatedly, use N with deionized water 2Dry up; Then in the uviolizing appearance, irradiation 60min gets hydroxylated silicon substrate, is placed on volumetric concentration again and is in the toluene solution of 1% OTS (octadecyl trichlorosilane) at room temperature to soak 20min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 100 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 1cm, irradiation 40min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 90 ℃ of deposit 10h 2S 3Film places 50 ℃ of dry 20min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
Sm with this embodiment preparation 2S 3Film (Fig. 1) is measured with the Japanese automatic x-ray diffractometer of D/max2200PC type of science (XRD), uses the SPA400-SPI3800N type AFM (AFM) of NSK (Fig. 2) its surface topography to be analyzed simultaneously.Can find out prepared Sm from picture 2S 3Nano thin-film percent crystallinity is better, is the mutually purified Sm of thing 2S 3, and grow along (105) high preferred orientation.
Embodiment 2:
1) gets the analytically pure (SmCl of 0.8g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 30mL;
2) in solution A, add the Hydrocerol A of 0.05g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 0.01g 2S 2O 3) stir solution C;
4) using the pH value of ammoniacal liquor regulator solution C is 5.0 must precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, uses behind the ultrasonic oscillation 3h naturally cooling at room temperature, and then clean repeatedly, use N with deionized water 2Dry up; Then in the uviolizing appearance, irradiation 20min gets hydroxylated silicon substrate, is placed on volumetric concentration again and is in the toluene solution of 2% OTS (octadecyl trichlorosilane) at room temperature to soak 10min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 115 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 3cm, irradiation 20min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 80 ℃ of deposit 1h 2S 3Film places 60 ℃ of dry 16min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
Embodiment 3:
1) gets the analytically pure (SmCl of 1.0g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 40mL;
2) in solution A, add the Hydrocerol A of 0.3g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 3.00g 2S 2O 3) stir solution C;
4) using the pH value of ammoniacal liquor regulator solution C is 6.0 must precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, uses behind the ultrasonic oscillation 1h naturally cooling at room temperature, and then clean repeatedly, use N with deionized water 2Dry up; Then in the uviolizing appearance, irradiation 80min gets hydroxylated silicon substrate, is placed on volumetric concentration again and is in the toluene solution of 1.5% OTS (octadecyl trichlorosilane) at room temperature to soak 25min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 120 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 4cm, irradiation 5min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 50 ℃ of deposit 40h 2S 3Film places 70 ℃ of dry 13min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
Embodiment 4:
1) gets the analytically pure (SmCl of 1.5g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 50mL;
2) in solution A, add the Hydrocerol A of 0.8g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 5.00g 2S 2O 3) stir solution C;
4) using the pH value of ammoniacal liquor regulator solution C is 4.0 must precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, uses behind the ultrasonic oscillation 2h naturally cooling at room temperature, and then clean repeatedly, use N with deionized water 2Dry up; Then in the uviolizing appearance, irradiation 40min gets hydroxylated silicon substrate, is placed on volumetric concentration again and is in the toluene solution of 1.8% OTS (octadecyl trichlorosilane) at room temperature to soak 15min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 105 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 2cm, irradiation 30min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 40 ℃ of deposit 50h 2S 3Film places 80 ℃ of dry 10min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
Embodiment 5:
1) gets the analytically pure (SmCl of 1.2g 36H 2O) place beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 20mL;
2) in solution A, add the Hydrocerol A of 1.00g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 10.00g 2S 2O 3) stir solution C;
4) using the pH value of ammoniacal liquor regulator solution C is 3.0 must precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, uses behind the ultrasonic oscillation 2h naturally cooling at room temperature, and then clean repeatedly, use N with deionized water 2Dry up; Then in the uviolizing appearance, irradiation 30min gets hydroxylated silicon substrate, is placed on volumetric concentration again and is in the toluene solution of 1.3% OTS (octadecyl trichlorosilane) at room temperature to soak 40min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 110 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 1cm, irradiation 60min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 60 ℃ of deposit 30h 2S 3Film places 90 ℃ of dry 25min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.

Claims (2)

1. a liquid phase self-assembly method prepares (105) oriented growth Sm 2S 3The method of film is characterized in that:
1) gets the analytically pure SmCl of 0.3-1.5g 36H 2O places beaker, the even solution A that gets of the deionized water and stirring that in beaker, adds 10-50mL;
2) in solution A, add the Hydrocerol A of 0.01-1.00g, the normal temperature lower magnetic force stir solution B;
3) in solution B, add the analytically pure Sulfothiorine (Na of 0.01-10.00g 2S 2O 3) stir solution C;
4) use the pH value of ammoniacal liquor regulator solution C to get precursor liquid D as 2.0-6.0;
5) hydroxylated silicon substrate being placed volumetric concentration is that the toluene solution of 1～2% OTS (octadecyl trichlorosilane) at room temperature soaks 10～40min; Wash with acetone, tetracol phenixin respectively after the taking-up; Dry up with nitrogen then, in nitrogen atmosphere, in 100～120 ℃ of dryings;
6) exsiccant OTS silicon substrate is placed in the uviolizing appearance; The long 184.9nm of ultraviolet radiation wave-wave; Under a normal atmosphere, keeping irradiation distance is under the situation of 1～4cm, irradiation 5～60min; Make the alkyl of OTS head base under the optical excitation of UV-light, carry out hydroxylation and change, obtain the substrate after the OTS functionalization;
7) silicon substrate after the functionalization is placed precursor liquid D, beaker is put into the vacuum-drying ware, vacuumize, then the vacuum-drying ware is placed loft drier, prepare Sm at 40～90 ℃ of deposit 1-50h 2S 3Film places 50～90 ℃ of drying 5～20min of vacuum drying oven to get Sm the film for preparing 2S 3Nano thin-film.
2. liquid phase self-assembly method preparation (105) oriented growth Sm according to claim 1 2S 3The method of film is characterized in that: described hydroxylated silicon substrate is that silicon substrate is immersed in the chloroazotic acid, uses behind ultrasonic oscillation 30min～3h naturally cooling at room temperature, and then cleans repeatedly with deionized water, uses N 2Dry up, in the uviolizing appearance, irradiation 20～80min gets hydroxylated silicon substrate then.
CN2011103764441A 2011-11-23 2011-11-23 Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process Pending CN102424960A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011103764441A CN102424960A (en) 2011-11-23 2011-11-23 Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011103764441A CN102424960A (en) 2011-11-23 2011-11-23 Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process

Publications (1)

Publication Number Publication Date
CN102424960A true CN102424960A (en) 2012-04-25

Family

ID=45958987

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011103764441A Pending CN102424960A (en) 2011-11-23 2011-11-23 Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process

Country Status (1)

Country Link
CN (1) CN102424960A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6132568A (en) * 1998-02-25 2000-10-17 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Manufacturing method of samarium sulfide thin films
CN101486483A (en) * 2009-02-19 2009-07-22 陕西科技大学 Method for preparing SmS film by microwave-hydrothermal method
CN101659520A (en) * 2009-09-17 2010-03-03 陕西科技大学 Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6132568A (en) * 1998-02-25 2000-10-17 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Manufacturing method of samarium sulfide thin films
CN101486483A (en) * 2009-02-19 2009-07-22 陕西科技大学 Method for preparing SmS film by microwave-hydrothermal method
CN101659520A (en) * 2009-09-17 2010-03-03 陕西科技大学 Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
侯艳超等: "n(Sm3+)/n(S2O32-)对液相自组装法制备Sm2S3薄膜的影响", 《人工晶体学报》 *
谈国强等: "液相自组装法制备铁酸铋薄膜的研究", 《人工晶体学报》 *

Similar Documents

Publication Publication Date Title
Tang et al. A template-free aqueous route to ZnO nanorod arrays with high optical property
Han et al. Controlled growth of well-aligned ZnO nanowire arrays using the improved hydrothermal method
CN106381481A (en) Preparation method of metal doping molybdenum disulfide thin film
CN110642240B (en) Method for synthesizing high-purity carbon nanocoil by using composite catalyst formed on basis of multiple small-size catalysts
Yu et al. Enhanced photocatalytic activity and charge transfer of a TiO 2/BiVO 4 nanostructured composite
CN102153288A (en) Method for preparing copper disulfide thin film with preferred orientation
CN110767811A (en) Photoelectric detector of methylamine lead iodoperovskite single crystal nanowire and preparation method
Juhnevica et al. Synthesis and properties of ZnO/Al thin films prepared by dip-coating process
CN102010001A (en) Preparation method of titanium dioxide cubic cone crystal
CN102424960A (en) Method for preparing (105) oriented-growth Sm2S3 thin film by liquid phase self-assembly process
Ragina et al. Wet chemical synthesis and characterization of tin sulphide thin films from different host solutions
CN103400894A (en) Method for preparing zinc sulfide optoelectronic film
CN102503553B (en) Sm2S3 film preparation method integrating microwave hydrothermal method and auxiliary liquid-phase self-assembling method
Haque et al. Effect of annealing on structure and morphology of cadmium sulphide thin film prepared by chemical bath deposition
CN106830072B (en) A kind of preparation method of titanium dioxide nanowire array
CN112593205B (en) Method for preparing large-area single-layer molybdenum disulfide with assistance of ammonia water
CN102418139B (en) Method for preparing oriented grown samarium sulfide film (311) by hydrothermal assisted liquid-phase self-assembly
CN111816770B (en) Perovskite thin film preparation method, perovskite thin film and solar cell device
CN103880062A (en) Zinc oxide nano-column thin film and preparation method thereof
CN102515239B (en) Method for preparing samarium sulphide film by microwave-assisted liquid phase reduction process
CN101853901B (en) Method for preparing cadmium sulfide nanometer membrane by self assembly
CN102394224B (en) Preparation method of chloro silane-samaric sulfide film on single crystal silicon surface
Wang et al. Degradation of co-evaporated perovskite thin films
CN102503552B (en) Preparation method of monocrystalline silicon surface aminosilane-samarium sulfide film
CN102503557A (en) Method for preparing samarium sulfide film by adopting elementary substance sulfur as sulfur source

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20120425