CN100359340C - Production of optical thin-membrane with samarium sulfide holographic recording - Google Patents
Production of optical thin-membrane with samarium sulfide holographic recording Download PDFInfo
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- CN100359340C CN100359340C CNB2006100419078A CN200610041907A CN100359340C CN 100359340 C CN100359340 C CN 100359340C CN B2006100419078 A CNB2006100419078 A CN B2006100419078A CN 200610041907 A CN200610041907 A CN 200610041907A CN 100359340 C CN100359340 C CN 100359340C
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Abstract
The present invention relates to a method for preparing a samarium sulfide holographic recording optical thin film. The method comprises the following steps: removing O2 from water by introducing Ar gas into deionized water; then, dissolving analytically pure samarium chloride and sodium thiosulphate respectively into the deionized water introduced with the Ar gas to prepare a solution with the concentration of 0.05 to 0.1 mol/L; mixing the two solutions according to the volume ratio of 2: 1 to 1: 4; putting a platinum wire as an anode and a silicon chip as a cathode into the mixed solution; electrically depositing the mixed solution for 0.5 to 3 hours by adopting a DC voltage stabilizing and current stabilizing power source with the currents of 2 to 9 mA and the voltages of 10 to 20 V; at the same time, regulating the PH value of the mixed solution to be 2.5 to 5.5 with 3.6 % of a dilute hydrochloric acid solution; taking the silicon chip out of the solution; soaking the silicon chip in the deionized water twice; drying the silicon chip at the temperature of 20 to 40 DEG C in an oven after the silicon chip is taken out of the solution; then obtaining the samarium sulfide thin film. The present invention prepares the samarium sulfide thin film by controlling the PH value of the solution and regulating the ranges of the concentration ratio of SM and S. The surface of the prepared thin film which needs no heat treatment to be a crystal phase is relatively flat, and the samarium sulfide thin film with a single crystal phase is prepared.
Description
Technical field
The present invention relates to a kind of preparation method of optical thin film, particularly a kind of preparation method of optical thin-membrane with samarium sulfide holographic recording.
Background technology
Samaric sulfide is a kind of phase-change material, and normal temperature is the semiconductor phase of black down, can undergo phase transition under pressure to change the metal phase into and be accompanied by change in color.This phase transformation can also wait by thermal treatment, induced with laser and cause.Because the optical property of its two-phase has evident difference, so the samaric sulfide film can be used for holographic recording and storage, optical switch, making minimal stress meter and optical digital reservoir etc.
Preparation samaric sulfide film process mainly contains both at home and abroad at present: sputtering method, vapour deposition method, pulsed laser deposition method and metal-organic chemical vapor deposition equipment method etc.Sputtering method is one of modal method of preparation samaric sulfide film.People such as Huang Jianfeng adopt Sm target and Sm
2S
3The method of target dual-target sputtering, control Sm target power output is under the situation of 27.6W and n (S): n (Sm)=1.1～0.667, samaric sulfide film [the Huang Jianfeng that on the Si substrate, has prepared the semiconductor phase, Cao Liyun, Xiong Xinbai etc. sputtering method prepares the XRD research [J] of samaric sulfide film. Wuhan University of Technology's journal, 2003; 25 (5): 23-26.]; And people such as S.Tanemura also adopt Sm target and Sm
2S
3The method of target dual-target sputtering, the ratio of controlling the power of two targets has prepared metal phase and semiconductor samaric sulfide mutually on the silicon dioxide substrate, and be 5.97 [S.Tanemura by the lattice parameter that ED records semiconductor phase samaric sulfide, S.Koide, Y.Senzaki etal.Fabrication and characterization of metaland semiconductor samaric sulfide thin films by rf/dc dual magnetron sputtering[J] .Applied SurfaceScience, 2003; 212-213:279-286]; Sputter coating density height, pin hole is few, and the purity of rete is higher, and the tack between sputtered film and the substrate is good, controllable film thickness and good reproducibility.But adopt the required sputtering equipment complexity of the method, need high-tension unit, preparation cost is higher; The film forming speed of sputtering deposit is low, requires the substrate temperature rise higher, thereby is subject to the foreign gas influence.
The method of the reactive evaporations of employing such as C.F.Hickey obtains samaric sulfide by evaporation samarium in the atmosphere of sulfur-bearing on low temperature substrates.Evaporate samarium in vacuum chamber, the atmosphere of used sulfur-bearing is H
2S gas, substrate is not heated.Find also to exist simultaneously other compound such as oxysulfide, carbonide, Sm in the resulting film
2S
3Deng.Discover lower rate of sedimentation and high H
2S dividing potential drop (5 * 10
-4Torr) help to generate purer samaric sulfide film.The domestic bibliographical information for preparing samaric sulfide in this way that yet there are no, this kind method economy is convenient, material obtains easily, do not need very high temperature, very big practical value is arranged, but also need vacuum equipment and strict process condition [C.F.Hickey, U.J.Gibson.Optical response of switching samaric sulfide in thin films prepared by reactiveevaporation[J] .J.Appl.Phys., 1987,62 (9): 3912-3916.].P.Miodushevsky etc. adopt the pulsed laser deposition method, and light source adopts the XeCl laser instrument, when the control Wavelength of Laser is 308nm, have deposited the samaric sulfide optical thin film on glass substrate.The characteristics of this method maximum are to prepare the high-purity samaric sulfide film with good controllability, film surface is smooth, internal residual stress is little, but be difficult to obtain large-area polycrystalline samaric sulfide film, the deposition of aggregate particles and reverse sputtering also are the problem [P.Miodushevsky that is difficult to overcome, M.L.Protopapa, F.De Tomasi, M.R.Perrone, S.Tundo, L.Vasanelli.Fine trimming of samaric sulfide film resistance by XeCl laserablation[J] .Thin Solid Films, 2000; 359:251～54]; Volodin, employing metal-organic chemical vapor deposition equipment methods such as N.M have been feedstock production with dithiocar-bamate samaric sulfide film, and studied the mutual relationship of its growth growth kinetics and temperature, and the structure and the surface topography of film [Volodin, N.M. have been carried out characterizing; Zavyalova, L.V.; Kirillov, A.I.; Svechnikov, S.V.; Prokopenko, I.V.; Khanova, A.V.Investigation of growthconditions, crystal structure and surface morphology of samaric sulfide filmsfabricated by MOCVD technique[J] .SIE named after S.A.Lavochkin, Russia.Fizika Napivprovidnikiv, Kvantova ta Optoelektronika (1999), 2 (2): 78-83.].This method is had relatively high expectations to raw material, requires avirulence and better chemical stability will be arranged.Also must have suitable vapor pressure and suitable heat decomposition temperature simultaneously, process is wayward.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of preparation technology simple, do not need simply to obtain the preparation method of optical thin-membrane with samarium sulfide holographic recording of the samaric sulfide film of single thing phase, the smooth densification of film surface that obtains by preparation method of the present invention through bakingout process.
For achieving the above object, the technical solution used in the present invention is: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.05-0.1mol/L; Samarium trichloride solution and hypo solution are pressed 2: 1-1: 4 volume ratio is mixed, silicon chip is cleaned with acetone, ethanol in ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt dc current regulator power supply with the voltage electro-deposition of the electric current of 2-9mA and 10-20V 0.5-3 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 2.5-5.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 20-40 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
The chemicals that the present invention will contain Sm and S is dissolved in the water respectively and is mixed with solution, with the platinum filament is anode, with the silicon chip is negative electrode, under the effect of dc current regulator power supply, make Sm and S in cathodic deposition this forerunner's liquid solution energising a period of time, and by the pH value of control solution and the scope of regulating the concentration ratio of Sm and S, make Sm and S deposition, thereby prepare the samaric sulfide film.The film surface of preparation is more smooth, need not thermal treatment and is crystalline phase, can prepare the samaric sulfide film of single crystalline phase.
Description of drawings
Fig. 1 is the X-ray diffractometer analysis chart of the film of the embodiment of the invention 1 preparation, and horizontal ordinate is 2 θ angles among the figure, and unit is " degree ", and ordinate is a diffracted intensity, and unit is " cps ";
Fig. 2 is the X-ray diffractometer analysis chart of the film of the embodiment of the invention 3 preparations, and horizontal ordinate is 2 θ angles among the figure, and unit is " degree ", and ordinate is a diffracted intensity, and unit is " cps ".
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively and is mixed with concentration in the deionized water that feeds behind the Ar gas and is O.05mol/L samarium trichloride solution and hypo solution; Samarium trichloride solution and hypo solution are mixed by 1: 4 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 2mA and 10V 1 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 3.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 40 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.Referring to Fig. 1, with the thing phase of resulting film with Japanese D/max2000pc type X-ray diffractometer analytic sample of science, resulting principal crystalline phase is the samaric sulfide phase, and the result shows that film has the preferred orientation of (331) direction.
Embodiment 2: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.07mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 3 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 4mA and 20V 2 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 5.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 20 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
Embodiment 3: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.08mol/L; Samarium trichloride solution and hypo solution are mixed by 2: 1 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 6mA and 13V 3 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 4.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 30 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.Referring to Fig. 2, with the thing phase of resulting film with Japanese D/max2000pc type X-ray diffractometer analytic sample of science, resulting principal crystalline phase is the samaric sulfide phase.The result shows that film has the preferred orientation of (331) direction.
Embodiment 4: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.08mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 2 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 3mA and 15V 0.5 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 2.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 26 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
Embodiment 5: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.1mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 1 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 9mA and 18V 1.5 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 5.0 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 35 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
The property of thin film that the present invention prepares is stable, surfacing, purer; Technology controlling and process is simple, does not need to carry out later stage thermal treatment again, can reduce preparation cost.
Claims (6)
1, a kind of preparation method of optical thin-membrane with samarium sulfide holographic recording is characterized in that:
1) in deionized water, feeds Ar gas except that the O in anhydrating
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.05-0.1mol/L;
2) samarium trichloride solution and hypo solution are pressed 2: 1-1: 4 volume ratio is mixed, silicon chip is cleaned with acetone, ethanol in ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt dc current regulator power supply with the voltage electro-deposition of the electric current of 2-9mA and 10-20V 0.5-3 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 2.5-5.5 simultaneously;
3) silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 20-40 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
2, the preparation method of optical thin-membrane with samarium sulfide holographic recording according to claim 1 is characterized in that: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.05mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 4 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 2mA and 10V 1 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 3.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 40 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
3, the preparation method of optical thin-membrane with samarium sulfide holographic recording according to claim 1 is characterized in that: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.07mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 3 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 4mA and 20V 2 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 5.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 20 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
4, the preparation method of optical thin-membrane with samarium sulfide holographic recording according to claim 1 is characterized in that: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.08mol/L; Samarium trichloride solution and hypo solution are mixed by 2: 1 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 6mA and 13V 3 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 4.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 30 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
5, the preparation method of optical thin-membrane with samarium sulfide holographic recording according to claim 1 is characterized in that: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.08mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 2 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 3mA and 15V 0.5 hour, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 2.5 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 26 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
6, the preparation method of optical thin-membrane with samarium sulfide holographic recording according to claim 1 is characterized in that: feed Ar gas except that the O in anhydrating in deionized water
2, then, with analytically pure samarium trichloride crystal SmCl
36H
2O and thiosulfuric acid sodium crystal Na
2S
2O
35H
2O is dissolved in respectively in the deionized water that feeds behind the Ar gas and is mixed with samarium trichloride solution and the hypo solution that concentration is 0.1mol/L; Samarium trichloride solution and hypo solution are mixed by 1: 1 volume ratio, silicon chip is cleaned with acetone, ethanol in KQ-50E type ultrasonic cleaner, rinse well with deionized water again, with the platinum filament is anode, silicon chip is that negative electrode is inserted in the above-mentioned mixed solution, adopt WJJT15003D type dc current regulator power supply with the voltage electro-deposition of the electric current of 9mA and 18V 1.5 hours, the pH value of regulating mixed liquor with 3.6% dilute hydrochloric acid solution is 5.0 simultaneously; Silicon chip is taken out from solution, in deionized water, soak 2 times, take out back 35 ℃ of oven dry down in baking oven, promptly obtain the samaric sulfide film.
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| CN100359340C true CN100359340C (en) | 2008-01-02 |
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|---|---|---|---|---|
| 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 |
| 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 |
| CN102503552B (en) * | 2011-11-23 | 2013-04-10 | 陕西科技大学 | Preparation method of monocrystalline silicon surface aminosilane-samarium sulfide film |
| CN102503556B (en) * | 2011-11-23 | 2013-01-02 | 陕西科技大学 | Method for preparing patterned samaric sulfide film by utilizing mixed silane self-assembling method |
| CN102503558B (en) * | 2011-11-23 | 2013-08-07 | 陕西科技大学 | Method for preparing LiFePO4 nano-film by using biomimetic method |
| CN102503553B (en) * | 2011-11-23 | 2013-08-14 | 陕西科技大学 | Sm2S3 film preparation method integrating microwave hydrothermal method and auxiliary liquid-phase self-assembling method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258594A (en) * | 1998-12-30 | 2000-07-05 | 中国科学院感光化学研究所 | Preparation of fast responsive discoloring film |
| 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 |
| JP2004083933A (en) * | 2002-08-22 | 2004-03-18 | Japan Science & Technology Corp | Crystalline sulfide thin film and its manufacturing method |
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2006
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Patent Citations (3)
| 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 |
| CN1258594A (en) * | 1998-12-30 | 2000-07-05 | 中国科学院感光化学研究所 | Preparation of fast responsive discoloring film |
| JP2004083933A (en) * | 2002-08-22 | 2004-03-18 | Japan Science & Technology Corp | Crystalline sulfide thin film and its manufacturing method |
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