CN101985749A - Method for preparing lanthanum-strontium-manganese-oxygen film - Google Patents
Method for preparing lanthanum-strontium-manganese-oxygen film Download PDFInfo
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- CN101985749A CN101985749A CN 201010564681 CN201010564681A CN101985749A CN 101985749 A CN101985749 A CN 101985749A CN 201010564681 CN201010564681 CN 201010564681 CN 201010564681 A CN201010564681 A CN 201010564681A CN 101985749 A CN101985749 A CN 101985749A
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Abstract
The invention discloses a method for preparing a lanthanum-strontium-manganese-oxygen film material on a silicon substrate by adopting an acetate chemical solution method. The method comprises the step of preparing precursor solution, namely preparing uniform, stable and transparent precursor solution at certain temperature by adding solutes of lanthanum acetate, strontium acetate and manganese acetate into a mixed solvent consisting of acetic acid and deionized water; preparing a gel film by performing spin coating on the prepared precursor solution on a silicon substrate, and performing heat treatment in stages in a short annealing furnace. The preparation method has the advantages that: the raw materials are cheap and nontoxic; pollution is prevented basically; the preparation process is simple; special equipment is not required; large-scale production is convenient; and the like. Meanwhile, the prepared film has large area, high uniformity, low roughness, no microcrack, stable performance, good electrical property and ferromagnetic performance and potential application prospect in intelligent thermal control devices of ferromagnetic film devices, spin electronic devices and spacecrafts.
Description
Technical field
The present invention relates to a kind of preparation method of lanthanum strontium manganese oxygen film, specifically, relate to a kind of method that adopts chemical solution method on silicon substrate, to prepare semi-metal lanthanum strontium manganese oxygen ferromagnetic thin film, belong to the magneticthin film preparing technical field.
Background technology
Lanthanum strontium manganese oxygen (La
1-xSr
xMnO
3, LSMO) film is class purposes functional materials very widely, and is existing main as magneto-resistor.Magnetic resistance material has great application prospect, be made at present in the information storage system magnetic head, magnetoresistive memory, automobile is with transmitter and be used for multiple general magneto-resistance effect devices such as measurement, control position, angle, speed, rotating speed, electric current.Another Application is the application of magnetic refrigeration aspect, and this class material can be used as high temperature, especially room temperature magnetic hysteresis cold material and be applied to health care, aerospace, automobile and other industries.In addition, this class material has the Curie temperature that is higher than room temperature, and near its metal-insulator transition temperature, noticeable change takes place in its infrared signature thereupon, also have anti-strong acid, water-fast gas, chemical property such as high temperature resistant simultaneously, in R﹠D process from now on, probably become the preferred material of surveying the radiometer device.Therefore, how research prepares LSMO film with excellent electric property and magnetic performance the industrial application of thin-film material is had important Research Significance.
At present, preparation La
1-xSr
xMnO
3The method of film mainly contains: chemical solution method, pulsed laser deposition, radio-frequency magnetron sputter method and channel spark ablation.Wherein chemical solution method is compared with other preparation methods, and the preparation film has lot of advantages: technology is simple, and cost is low, and stoichiometric ratio is easy to control, can prepare the uniform film of big area.In order to make La
1-xSr
xMnO
3Film is used for ferroelectric integrated device, La
1-xSr
xMnO
3Film should prepare on the Si substrate.But up to the present, though the bibliographical information that adopts chemical solution method to prepare the lanthanum strontium manganese oxygen film on the Si substrate is arranged, but all adopting metal alkoxide (toxicity is bigger) or nitrate (thermal degradation can discharge nitrogen oxide) basically is solute, methyl alcohol, ethylene glycol, methyl ether toxic reagent are solvent, have the serious defective of environmental pollution, and the film surface that grows there is crackle.Therefore, study and a kind ofly on the Si substrate, prepare the method for the LSMO film of high electric property and magnetic performance with poisonous material, will be significant to this area.
Summary of the invention
The present invention is directed to above-mentioned existing in prior technology defective and problem, provide a kind of not only technology simple, environmental pollution is little, preparation cost is low, and the film size of preparation is big, evenly and not ftractures stable performance, be suitable for the preparation method of the lanthanum strontium manganese oxygen film of suitability for industrialized production, realized on the Si substrate, preparing the target of the LSMO film of high electric property and magnetic performance with poisonous material.
The preparation method of lanthanum strontium manganese oxygen film provided by the invention comprises following concrete steps:
The preparation of A, precursor solution
Lanthanum acetate, strontium acetate and three kinds of solutes of manganese acetate are added acetic acid (CH by proportioning
3COOH) and in the mixed solvent that forms of deionized water, be heated to 60～80 ℃ solute is dissolved fully, the concentration of solution is controlled to be 0.1～0.4mol/L; The yellow transparent solution that obtains was at room temperature left standstill 48～72 hours; With the filtering with microporous membrane of 0.2 μ m, promptly get stable lanthanum strontium manganese oxygen (LSMO) precursor solution;
The preparation of B, thin-film material
The precursor solution for preparing at the uniform velocity is added drop-wise on the silicon substrate of cleaning of high speed rotating, solvent volatilization rapidly obtains gel-film; Place annealing furnace to carry out heat treatment in sections gel-film, promptly obtain the lanthanum strontium manganese oxygen film.
The mol ratio of the lanthanum acetate in the steps A, strontium acetate and three kinds of solutes of manganese acetate is preferably (10-x): x: 10, and 2≤x≤4 wherein.
The acetic acid in the mixed solvent in the steps A and the volume ratio of deionized water be preferably 5: 1～and 2: 1.
The rotating speed of the silicon substrate among the step B is preferably 3000～6000 rev/mins, and the hold-time is preferably 20～50 seconds.
Thermal treatment process among the step B is preferably: under 150～200 ℃, be incubated 2～4 minutes earlier; Again under 340～440 ℃, pyrolysis 3～10 minutes; Under 700～900 ℃, annealed 3～60 minutes at last.
Compared with prior art, the present invention has following beneficial effect:
1) preparation method of the present invention is that to adopt lanthanum acetate, strontium acetate, manganese acetate be solute, and acetic acid and water are solvent, and raw material is inexpensive, nontoxic, and whole process has only acetic acid and Carbon emission, and environmental pollution is little.
2) big, the good uniformity of the film size of the present invention preparation, roughness are little, non-microcracked, stable performance, and have good electric property and ferromagnetic property.
3) preparation technology of the present invention is simple, need not specific installation, helps large-scale production.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the LSMO film that makes of embodiment 1;
Fig. 2 is the AFM surface topography map of the LSMO film that makes of embodiment 1;
Fig. 3 is the temperature variant graph of relation of resistivity of the LSMO film that makes of embodiment 1;
Fig. 4 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 1 at 300K;
Fig. 5 is the temperature variant graph of relation of the specific magnetising moment of LSMO film under stilling the theatre that embodiment 1 makes;
Fig. 6 is the AFM surface topography map of the LSMO film that makes of embodiment 2;
Fig. 7 is the temperature variant graph of relation of resistivity of the LSMO film that makes of embodiment 2;
Fig. 8 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 2 at 300K;
Fig. 9 is the temperature variant graph of relation of the specific magnetising moment of LSMO film under stilling the theatre that embodiment 2 makes;
Figure 10 is the AFM surface topography map of the LSMO film that makes of embodiment 3;
Figure 11 is the temperature variant graph of relation of resistivity of the LSMO film that makes of embodiment 3;
Figure 12 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 3 at 300K;
Figure 13 is the temperature variant graph of relation of the specific magnetising moment of LSMO film under stilling the theatre that embodiment 3 makes;
Figure 14 is the X-ray diffractogram of the LSMO film that makes of embodiment 4;
Figure 15 is the AFM surface topography map of the LSMO film that makes of embodiment 4;
Figure 16 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 4 at 300K;
Figure 17 is the X-ray diffractogram of the LSMO film that makes of embodiment 5;
Figure 18 is the temperature variant graph of relation of resistivity of the LSMO film that makes of embodiment 5;
Figure 19 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 5 at 300K;
Figure 20 is the temperature variant graph of relation of the specific magnetising moment of LSMO film under stilling the theatre that embodiment 5 makes;
Figure 21 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 6 at 300K;
Figure 22 is the temperature variant graph of relation of the specific magnetising moment of LSMO film under stilling the theatre that embodiment 6 makes;
Figure 23 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 7 at 300K;
Figure 24 is the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 8 at 300K.
Specific implementation method
The present invention is described in further detail and completely below in conjunction with embodiment, but do not limit content of the present invention.
The preparation of A, precursor solution
With mol ratio is that lanthanum acetate, strontium acetate and three kinds of solutes of manganese acetate of 7: 3: 10 are dissolved in acetic acid (CH3COOH) and deionized water is in the mixed solvent that forms at 4: 1 by volume, be heated to 60～80 ℃ solute is dissolved fully, the concentration of solution is 0.15mol/L; The yellow transparent solution that obtains was at room temperature left standstill 48～72 hours; With the filtering with microporous membrane of 0.2 μ m, promptly get stable lanthanum strontium manganese oxygen (LSMO) precursor solution;
The preparation of B, thin-film material
The precursor solution for preparing is added drop-wise on the silicon substrate of cleaning of high speed rotating, the substrate rotating speed is 5000 rev/mins, and keeps 30 seconds, and solvent volatilization rapidly obtains gel-film; Place annealing furnace to carry out heat treatment in sections gel-film, that is: earlier 180 ℃ of insulations 3 minutes, again 360 ℃ of pyrolysis 10 minutes, whirl coating 6 times is at last 700 ℃ of annealing 30 minutes; Promptly getting thickness is the lanthanum strontium manganese oxygen film of 130nm.
The difference of present embodiment and embodiment 1 is: last annealed temperature is 750 ℃ of high temperature, and is identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
The difference of present embodiment and embodiment 1 is: last annealed temperature is 750 ℃ of high temperature, and annealing time is 60 minutes, and is identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
The difference of present embodiment and embodiment 1 is: the volume ratio of acetic acid in the precursor liquid (CH3COOH) and deionized water is 5: 1, and the concentration of solution is 0.4mol/L; The substrate rotating speed is 6000 rev/mins, and keeps 50 seconds; The thermal treatment process of film is: earlier 180 ℃ of insulations 3 minutes, again 440 ℃ of pyrolysis 10 minutes, whirl coating 4 times is at last 850 ℃ of annealing 60 minutes.Identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is about 290nm.
Embodiment 5
The difference of present embodiment and embodiment 1 is: the volume ratio of acetic acid in the precursor liquid (CH3COOH) and deionized water is 3: 1, and the concentration of solution is 0.15mol/L; The substrate rotating speed is 4000 rev/mins, and keeps 30 seconds; The thermal treatment process of film is: earlier 200 ℃ of insulations 3 minutes, again 380 ℃ of pyrolysis 10 minutes, whirl coating 6 times is at last 750 ℃ of annealing 48 minutes.Identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
The difference of present embodiment and embodiment 1 is: the volume ratio of acetic acid in the precursor liquid (CH3COOH) and deionized water is 3: 1, and the concentration of solution is 0.2mol/L; The thermal treatment process of film is: earlier 180 ℃ of insulations 3 minutes, again 440 ℃ of pyrolysis 3 minutes, whirl coating 4 times is at last 700 ℃ of annealing 60 minutes.Identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
Embodiment 7
The difference of present embodiment and embodiment 1 is: the volume ratio of acetic acid in the precursor liquid (CH3COOH) and deionized water is 2: 1, and the concentration of solution is 0.2mol/L; The substrate rotating speed is 3000 rev/mins, and keeps 20 seconds; The thermal treatment process of film is: earlier 200 ℃ of insulations 4 minutes, again 400 ℃ of pyrolysis 10 minutes, whirl coating 4 times is at last 750 ℃ of annealing 3 minutes.Identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
The difference of present embodiment and embodiment 1 is: the volume ratio of acetic acid in the precursor liquid (CH3COOH) and deionized water is 5: 1, and the concentration of solution is 0.15mol/L; The thermal treatment process of film is: earlier 200 ℃ of insulations 3 minutes, again 400 ℃ of pyrolysis 3 minutes, whirl coating 6 times is at last 750 ℃ of annealing 3 minutes.Identical described in all the other contents and the embodiment 1.The thickness of gained lanthanum strontium manganese oxygen film is close with embodiment 1.
Fig. 1, Figure 14, Figure 17 are the X ray diffracting spectrums of the LSMO film that makes of embodiment 1,4,5, and as seen: the crystalline structure by the prepared LSMO film of preparation method of the present invention all is tangible calcium attitude ore deposit structure.
Fig. 2, Fig. 6, Figure 10, Figure 15 are the AFM surface topography maps of the LSMO film that makes of embodiment 1,2,3,4, wherein: the surfaceness RMS=2.0nm of the LSMO film that embodiment 1 makes; The surfaceness RMS=3.1nm of the LSMO film that embodiment 2 makes; The surfaceness RMS=2.1nm of the LSMO film that embodiment 3 makes; The surfaceness RMS=5.4nm of the LSMO film that embodiment 4 makes.As seen: have advantages such as surfacing, roughness are little, flawless by the prepared LSMO film of preparation method of the present invention.With the rising and the holding time prolonging of annealing temperature, crystal grain can be grown up.
Fig. 3, Fig. 7, Figure 11, Figure 19 are the temperature variant graph of relation of resistivity of the LSMO film that makes of embodiment 1,2,3,5, as seen: all show good resistivity by the prepared LSMO film of preparation method of the present invention, near 0～50K, along with the rising resistivity decreased of temperature; Near 50～200K, rise with temperature rising resistivity; From about 200K to 400K left and right sides resistivity decreased.
Fig. 4, Fig. 8, Figure 12, Figure 16, Figure 19, Figure 21, Figure 23, Figure 24 are the magnetic hysteresis loop figure of the LSMO film that makes of embodiment 1,2,3,4,5,6,7,8 at 300K.As seen: all show good magnetic hysteresis expansion performance by the prepared LSMO film of preparation method of the present invention, coercive field is very little.Along with the rising and the holding time prolonging of annealing temperature, residual magnetization has enhancing trend.
Fig. 5, Fig. 9, Figure 13, Figure 20, Figure 22 are that the specific magnetising moment of LSMO film under stilling the theatre that make of embodiment 1,2,3,5,6 is with the variation of temperature curve.As seen: under static magnetic field, its specific magnetising moment slowly descends earlier with the temperature rising specific magnetising moment by the prepared LSMO film of preparation method of the present invention, and near 200K-320K, polarizability sharply descends, and the specific magnetising moment gradually becomes zero near 320K-400K.Explanation by the Curie temperature of the prepared LSMO film of preparation method of the present invention near 320K-400K.
Should be noted that at last, above embodiment is unrestricted the present invention in order to technical scheme of the present invention to be described only, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (5)
1. the preparation method of a lanthanum strontium manganese oxygen film is characterized in that, comprises following concrete steps:
The preparation of A, precursor solution
Lanthanum acetate, strontium acetate and three kinds of solutes of manganese acetate are added acetic acid (CH by proportioning
3COOH) and in the mixed solvent that forms of deionized water, be heated to 60～80 ℃ solute is dissolved fully, the concentration of solution is controlled to be 0.1～0.4mol/L; The yellow transparent solution that obtains was at room temperature left standstill 48～72 hours; With the filtering with microporous membrane of 0.2 μ m, promptly get stable lanthanum strontium manganese oxygen (LSMO) precursor solution;
The preparation of B, thin-film material
The precursor solution for preparing at the uniform velocity is added drop-wise on the silicon substrate of cleaning of high speed rotating, solvent volatilization rapidly obtains gel-film; Place annealing furnace to carry out heat treatment in sections gel-film, promptly obtain the lanthanum strontium manganese oxygen film.
2. the preparation method of lanthanum strontium manganese oxygen film according to claim 1 is characterized in that, the mol ratio of the lanthanum acetate in the steps A, strontium acetate and three kinds of solutes of manganese acetate is (10-x): x: 10, and 2≤x≤4 wherein.
3. the preparation method of lanthanum strontium manganese oxygen film according to claim 1 is characterized in that, the mixed solvent in the steps A is to be to mix in 5: 1～2: 1 to form by volume by acetic acid and deionized water.
4. the preparation method of lanthanum strontium manganese oxygen film according to claim 1 is characterized in that, the rotating speed of the silicon substrate among the step B is 3000～6000 rev/mins, and the hold-time is 20～50 seconds.
5. the preparation method of lanthanum strontium manganese oxygen film according to claim 1 is characterized in that, the thermal treatment process among the step B is: under 150～200 ℃, be incubated 2～4 minutes earlier; Again under 340～440 ℃, pyrolysis 3～10 minutes; Under 700～900 ℃, annealed 3～60 minutes at last.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774227A (en) * | 2014-01-20 | 2014-05-07 | 华东师范大学 | Manganite epitaxial thin film and preparation method thereof |
| CN104193316A (en) * | 2014-08-21 | 2014-12-10 | 中国科学院上海硅酸盐研究所 | Yttrium iron garnet film and preparation method thereof |
| CN110736548A (en) * | 2019-10-21 | 2020-01-31 | 北京科易达知识产权服务有限公司 | method and device for up-converting infrared image into visible image and up-conversion film preparation method |
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2010
- 2010-11-29 CN CN2010105646816A patent/CN101985749B/en active Active
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| CN1327085A (en) * | 2001-04-25 | 2001-12-19 | 中国科学院上海技术物理研究所 | Process for preparing lanthanum-strontium-cobalt-oxygen conductive film material |
| JP2004087745A (en) * | 2002-08-27 | 2004-03-18 | Hitachi Ltd | Magnetic reluctance effect element, magnetic head using it, and magnetic record reproducing device |
| CN1757785A (en) * | 2005-10-27 | 2006-04-12 | 复旦大学 | Preparation method of calcium titanium ore structure lanthanum strontium manganese oxygen half metal film |
| US20090026441A1 (en) * | 2007-07-26 | 2009-01-29 | Unity Semiconductor Corporation | Continuous plane of thin-film materials for a two-terminal cross-point memory |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774227A (en) * | 2014-01-20 | 2014-05-07 | 华东师范大学 | Manganite epitaxial thin film and preparation method thereof |
| CN104193316A (en) * | 2014-08-21 | 2014-12-10 | 中国科学院上海硅酸盐研究所 | Yttrium iron garnet film and preparation method thereof |
| CN110736548A (en) * | 2019-10-21 | 2020-01-31 | 北京科易达知识产权服务有限公司 | method and device for up-converting infrared image into visible image and up-conversion film preparation method |
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| CN101985749B (en) | 2011-10-19 |
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