CN102503552B - Preparation method of monocrystalline silicon surface aminosilane-samarium sulfide film - Google Patents
Preparation method of monocrystalline silicon surface aminosilane-samarium sulfide film Download PDFInfo
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Abstract
一种单晶硅表面氨基硅烷-硫化钐薄膜的制备方法，在二碘化钐的四氢呋喃溶液中加入EDTA得溶液B；向溶液B中加入硫脲得溶液C；用氨水调节溶液C的pH值至2.5～4.5得前驱液D；将前驱液D置于烧杯中，再将功能化后的硅基板置于前驱液D中，将烧杯放入真空干燥皿中，抽真空，然后将真空干燥皿置于干燥箱中沉积制备硫化钐薄膜，将制备好的薄膜置于真空干燥箱中干燥得硫化钐纳米薄膜。由于本发明采用液相自组装方法，制得的硫化钐纳米薄膜，均匀，致密，低缺陷，强度高，并且通过控制前驱液浓度、pH值以及沉积时间可以控制薄膜厚度和晶粒大小。这种方法制备的硫化钐纳米薄膜重复性高，易于大面积制膜。且操作方便，原料易得，制备成本较低。A preparation method of aminosilane-samarium sulfide thin film on the surface of single crystal silicon, adding EDTA to the tetrahydrofuran solution of samarium diiodide to obtain solution B; adding thiourea to solution B to obtain solution C; adjusting the pH value of solution C with ammonia water To 2.5-4.5 to get the precursor solution D; put the precursor solution D in a beaker, then place the functionalized silicon substrate in the precursor solution D, put the beaker into a vacuum drying dish, vacuumize, and then put the vacuum drying dish Deposit and prepare a samarium sulfide thin film in a drying oven, and dry the prepared thin film in a vacuum drying oven to obtain a samarium sulfide nano-film. Because the present invention adopts the liquid phase self-assembly method, the prepared samarium sulfide nano film is uniform, compact, low in defects and high in strength, and the film thickness and grain size can be controlled by controlling the concentration of the precursor liquid, the pH value and the deposition time. The samarium sulfide nano film prepared by this method has high repeatability and is easy to form a film in a large area. Moreover, the operation is convenient, the raw materials are easy to obtain, and the preparation cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of samarium sulfide film, be specifically related to a kind of preparation method of monocrystalline silicon surface amino silane-samarium sulfide film.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
The SmS crystal is cubic structure, is a kind of pressure off-color material.Be the semiconductor (S-SmS) of black at normal temperatures and pressures, its lattice parameter is 0.597nm, 6.5 * 10
8Under the static pressure of Pa, the SmS crystal can experience from the in opposite directions phase transformation of Metal Phase (M-SmS) of semiconductor.Grating constant reduces to about 0.570nm from 0.597nm; And, crystal color will become golden yellow from black, volumetric contraction is [Jayaraman A about about 16% greatly, Narayanamurti V, Bucher Eetal.Continuous and Discontinuous Semiconductor-metal Tran-sition inSamarium Monochalcogenides Under Pressure[J] .Phy Rev Lett.1970,25 (20): 1430.].The film of SmS sees through as green, reflection then is blue or partially blue black, after occuring to change mutually, it can become blue look and flavous reflected colour [the Hickey C F of seeing through, Gibson U J.Optical Response of Switching SmS in ThinFilms Prepared by Reactive Evaporation[J] .J Appl Phys.1987,62 (9): 3912～3916].Therefore, have and press the SmS of variable color character can be used for holographic recording and reservoir, optical switch and optical digital reservoir etc.Up to the present, responding property of method evaporation [Petrov M P.Holographics Storage in SmSThin Films[J] the .Optics Communications.1977 for preparing samarium sulfide film, [the Huang Jianfeng such as 22 (3): 293～296], vacuum moulding machine, electron beam evaporation plating, dual-target sputtering, the .SmS optical thin film New research progress [J] such as horse small echo. material Leader .2006,20 (9): 9～12].These preparation technologies are comparative maturity, but the comparison in equipment that needs is special, costliness; Complicated process of preparation, the factors such as condition harshness, so that the cost of preparation samarium sulfide film is too high, the good film of processability that can not Simple fast.Self assembly (Self-assembled monolayers) technology (being called for short the SAMs technology), be a kind of new technology for preparing film, by the chemisorption between surfactant and the substrate, on baseplate material, form marshalling from group, densification, orderly unimolecule rete.Inorganic precursor solution is at the bionical synthetic masking technique of substrate surface deposition film forming take self-assembled film as template-mediated, has the unrivaled advantage of conventional physical chemical method, that a kind of novel, efficient green masking technique that has application prospect [is talked Guoqiang, Liu Jian, He Zhongliang. self-assembled monolayer membrane technology and the application [J] in preparation function film field thereof. 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 adhesion is good, does not need the later stage crystallization to process.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of monocrystalline silicon surface amino silane-samarium sulfide film is provided.Preparation method's technique of the present invention is simple, with low cost, and the film of preparing is even, densification, and low defective, intensity is high, and adhesion is good, does not need the later stage crystallization to process, and is functional.
For achieving the above object, concrete grammar of the present invention is as follows:
1) getting 0.1～10.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 10-80mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 0.1-2.0g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 0.01-10.00g
4N
2S) solution C that stirs to get;
4) the pH value to 2.5 of usefulness ammoniacal liquor regulator solution C～4.5 get precursor liquid D;
5) hydroxylated silicon substrate being placed volumetric concentration is that the absolute methanol solution of 0.5～1.5% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 10～360min, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 210～230 ℃ of drying 10～30min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1～2cm, irradiation 60～120min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 30～60 ℃ of deposit 20～50h, place 50～90 ℃ of drying 15～30min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Described hydroxylated silicon substrate is first silicon substrate to be immersed in the chloroazotic acid, naturally cools off at room temperature behind use ultrasonic oscillation 30～360min, and then repeatedly cleans with deionized water, uses N
2Dry up, then in ultraviolet illuminating instrument, irradiation 30～50min gets hydroxylated silicon substrate.
Because the present invention adopts the liquid phase self-assembling method, the samaric sulfide nano thin-film that makes, evenly, and densification, low defective, intensity is high, and can control film thickness and grain size by control Concentration of precursor solution, pH value and sedimentation time.The samaric sulfide nano thin-film repeatability of this method preparation is high, is easy to the large tracts of land masking.And easy to operate, raw material is easy to get, and preparation cost is lower.
Description of drawings
Fig. 1 is the prepared samarium sulfide film XRD collection of illustrative plates of embodiment 1;
Fig. 2 is the FESEM figure of the prepared samarium sulfide film of embodiment 1.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:
1) getting 0.1ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 20mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 0.1g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 0.05g
4N
2S) solution C that stirs to get;
4) the pH value to 2.5 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 60min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 30min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 0.5% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 60min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 210 ℃ of dry 30min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1cm, irradiation 60min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 30 ℃ of deposit 50h, place 50 ℃ of dry 30min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
The samarium sulfide film of this embodiment preparation is measured with the automatic x-ray diffractometer of Rigaku D/max2200PC type, as shown in Figure 1, prepared samarium sulfide film under the JSM-6700F field emission scanning electron microscope (Fig. 2) is observed.The diffraction peak of obvious SmS as can be seen from Figure 1 occurs at crystal face (331), as can be seen from Figure 2 film surface is even and fine and close.
Embodiment 2:
1) getting 0.5ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 10mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 0.5g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 0.01g
4N
2S) solution C that stirs to get;
4) the pH value to 3 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 30min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 50min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 0.8% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 360min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 220 ℃ of dry 20min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 2cm, irradiation 80min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 50 ℃ of deposit 30h, place 70 ℃ of dry 20min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Embodiment 3:
1) getting 3.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 40mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 0.8g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 0.8g
4N
2S) solution C that stirs to get;
4) the pH value to 3.5 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 120min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 40min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 1.0% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 180min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 230 ℃ of dry 10min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1.5cm, irradiation 90min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 40 ℃ of deposit 40h, place 90 ℃ of dry 15min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Embodiment 4:
1) getting 5.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 50mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 1.5g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 3.00g
4N
2S) solution C that stirs to get;
4) the pH value to 4.0 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 180min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 35min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 1.2% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 240min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 215 ℃ of dry 25min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 2cm, irradiation 120min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 360 ℃ of deposit 20h, place 80 ℃ of dry 25min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Embodiment 5:
1) getting 8.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 80mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 1.3g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 7.00g
4N
2S) solution C that stirs to get;
4) the pH value to 4.5 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 260min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 45min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 1.3% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 120min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 225 ℃ of dry 15min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1.5cm, irradiation 100min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 45 ℃ of deposit 35h, place 60 ℃ of dry 30min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Embodiment 6:
1) getting 10.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 60mL in the beaker solution A that stirs to get;
2) add the EDTA (ethylenediamine tetraacetic acid) of 1.3g in the solution A, the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 10.00g
4N
2S) solution C that stirs to get;
4) the pH value to 4 with ammoniacal liquor regulator solution C gets precursor liquid D;
5) silicon substrate is immersed in the chloroazotic acid, naturally cools off at room temperature behind the use ultrasonic oscillation 360min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 40min gets hydroxylated silicon substrate;
It is that the absolute methanol solution of 1.5% APTS (3-aminopropyl methyl triethoxysilane) at room temperature soaks 10min that hydroxylated silicon substrate is placed volumetric concentration, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 210 ℃ of dry 30min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1cm, irradiation 70min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 55 ℃ of deposit 40h, place 85 ℃ of dry 25min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
Claims (2)
1. the monocrystalline silicon in the surface amino groups silane-functionalized prepares the method for samarium sulfide film, it is characterized in that:
1) getting 0.1 ~ 10.0ml concentration is that the tetrahydrofuran solution of the samarium diodide of 0.1mol/L places beaker, the tetrahydrofuran that adds again 10-80mL in the beaker solution A that stirs to get;
2) add the EDTA(ethylenediamine tetraacetic acid of 0.1-2.0g in the solution A), the normal temperature lower magnetic force solution B that stirs to get;
3) in solution B, add the analytically pure thiocarbamide (CH of 0.01-10.00g
4N
2S) solution C that stirs to get;
4) the pH value to 2.5 of usefulness ammoniacal liquor regulator solution C ~ 4.5 get precursor liquid D;
5) hydroxylated silicon substrate being placed volumetric concentration is that the absolute methanol solution of 0.5 ~ 1.5% APTS at room temperature soaks 10 ~ 360min, wash with acetone, phenixin respectively after the taking-up, then dry up with nitrogen, under nitrogen atmosphere protection in 210 ~ 230 ℃ of drying 10 ~ 30min;
6) silicon substrate after the drying is placed in the ultraviolet irradiation instrument, ultraviolet radiation wavelength 184.9nm is under an atmospheric pressure, the maintenance irradiation distance is 1 ~ 2cm, irradiation 60 ~ 120min makes the amino of APTS head base carry out the hydroxylation transformation under the irradiation of ultraviolet light, obtains the silicon substrate of APTS 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 drying box, prepare samarium sulfide film at 30 ~ 60 ℃ of deposit 20 ~ 50h, place 50 ~ 90 ℃ of drying 15 ~ 30min of vacuum drying chamber to get the samaric sulfide nano thin-film film for preparing.
2. the monocrystalline silicon in the surface amino groups silane-functionalized according to claim 1 prepares the method for samarium sulfide film, it is characterized in that: described hydroxylated silicon substrate is first silicon substrate to be immersed in the chloroazotic acid, naturally cool off at room temperature after using ultrasonic oscillation 30 ~ 360min, and then repeatedly clean with deionized water, use N
2Dry up, then in ultraviolet illuminating instrument, irradiation 30 ~ 50min gets hydroxylated silicon substrate.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818718A (en) * | 2006-03-09 | 2006-08-16 | 陕西科技大学 | Production of optical thin-membrane with samarium sulfide holographic recording |
| CN101486483A (en) * | 2009-02-19 | 2009-07-22 | 陕西科技大学 | Method for preparing SmS film by microwave-hydrothermal method |
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| JP2931973B1 (en) * | 1998-02-25 | 1999-08-09 | 工業技術院長 | Preparation of samarium monosulfide piezochromic thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1818718A (en) * | 2006-03-09 | 2006-08-16 | 陕西科技大学 | Production of optical thin-membrane with samarium sulfide holographic recording |
| CN101486483A (en) * | 2009-02-19 | 2009-07-22 | 陕西科技大学 | Method for preparing SmS film by microwave-hydrothermal method |
Non-Patent Citations (8)
| Title |
|---|
| JP特开平11-241161A 1999.09.07 |
| 吴建鹏.SmS全息记录光学薄膜研究进展.《稀有金属材料与工程 》.2006,(第S2期),全文. * |
| 吴建鹏.阴极恒电流法制备SmS光学薄膜.《功能材料与器件学报》.2007,(第02期),全文. * |
| 曹丽云 * |
| 罗宏杰 * |
| 贺海燕 * |
| 马小波 * |
| 黄剑锋 * |
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