CN101949643B - High-temperature heat treatment device under magnetic field and method thereof for preparing bismuth ferrite film - Google Patents
High-temperature heat treatment device under magnetic field and method thereof for preparing bismuth ferrite film Download PDFInfo
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Abstract
The invention provides a high-temperature heat treatment device under a magnetic field and a method thereof for preparing a bismuth ferrite film. The device comprises a tube type heating furnace, wherein the tube type heating furnace is arranged between magnet pole heads of a direct current water-cooling magnet, the direct current water-cooling magnet is connected with a direct-current magnet power supply and a circulating water-cooling system, the heating cavity of the tube type heating furnace is communicated with a vacuumizing system and an atmosphere control system; the tube type heating furnace is also connected with a temperature controller; the water-cooling cavity is formed by adopting a double-layer nonmagnetic stainless steel material by the shell of the tube type heating furnace; heating bodies are connected in series by four silicon carbide rods; a high-temperature resistant aluminum oxide heat insulating fiber material is used as a heat insulating material; and a high-temperature aluminum oxide ceramic tube or a quartz glass tube is used as a furnace tube. The device has the characteristics of small volume, high magnetic field utilization ratio and heating efficiency, and the like, can be used for carrying out the synthesis and the heat treatment on materials below 2 Tesla of the magnetic field and under the condition of vacuum or atmosphere. The microstructure and the properties of the bismuth ferrite film prepared by the device are improved.
Description
Technical field:
The present invention relates to a kind of device that under magnetic field condition, carries out the synthetic and high-temperature heat treatment of material, the method that is specifically related to a kind of high-temperature tubular furnace apparatus of under direct current water-cooled magnet, working and prepares bismuth ferrite thin film.
Background technology:
In recent years, the preparation of the material under the magnetic field condition and heat treatment are subjected to people's great attention.Magnetic field can effectively change the formation of various defect states and ordered phase in the material crystallization process, magnetic field condition provides a new driving energy for material is synthetic simultaneously, can change electron spin and the nuclear spin of reactant, promote ions diffusion, increase the reactant activation, improve reaction selectivity, thereby bring out new physicochemical change, prepare the new material that is difficult to obtain with usual method and new material character.Therefore, magnetic field material synthetic with heat treatment in as a kind of important control measures, be widely used in material preparation and performance improvement.High temperature superconducting materia texture is improved and the raising of critical current density as being used for, the process of setting of metal or alloy and microstructure control etc.Usually the preparation of block materials and nonmagnetic substance need just can be played the effect of regulation and control than higher magnetic field condition, as several more than tesla.But in magnetic material and low-dimensional materials preparation process, lower magnetic field just can change the material growth pattern, obtains to have special micro-structural and material property.Therefore, the material under the middle downfield condition is synthetic significant in the preparation of magnetic material and low-dimensional nano structure material with annealing device.
Existing more about the synthetic publication with the annealing device aspect of material under the magnetic field condition.For example, Chinese patent CN2879162 discloses high-temperature heat treatment device under a kind of high-intensity magnetic field, utilize this device can carry out the processing such as smelting physical reaction, purification, refining of material fusion process, obtain the higher fused solution of cleanliness factor, also can carry out high-intensity magnetic field and retrain the unidirectional solidification of material down, directed, the uniform material of preparation tissue.Chinese patent CN101157125A discloses metal material high-temperature processing method and device under a kind of resultant field, and pulsed magnetic field treatment technology and high-intensity magnetic field treatment technology are effectively made up, and is used for the optimal control of metal material tissue structure.
In disclosed patent and the bibliographical information, annealing device under the most magnetic field, magnet adopts superconducting magnet usually, cost and operating cost are all than higher, what heating furnace usually adopted is similar well-type electric furnace, is mainly used in the control etc. of the institutional framework of the processing such as purification, refining of material fusion process and process of setting.Also do not see at present the relevant patent and the report that utilize high-temperature heat treatment device under direct current water-cooled magnet and the magnetic field that electric tube furnace constitutes.
Multi-ferroic material is with a wide range of applications at aspects such as magnetic, electric field induction device, memory and rectifying materials.For ferrous acid bismuth material, because it has very high antiferromagnetic Ne﹠1﹠el temperature and ferroelectrie Curie temperature and big electric polarization, be considered to a kind of one of single-phase multi-ferroic material of application prospect that has most.But the magnetic of this material and magneto-electric coupled effect usually a little less than, and its physical property and preparation technology's close association, be easy to generate bigger leakage current and influence iron electric polarization, these factors are its key in application problems of restriction, also are the hot issues of studying at present.
Summary of the invention:
The purpose of this invention is to provide high-temperature heat treatment device under a kind of magnetic field and prepare the method for bismuth ferrite thin film, can be lower than in magnetic field and carry out the synthetic and heat treatment of material under 2 teslas and vacuum or the atmospheric condition, rely on apparatus of the present invention, prepared the bismuth ferrite thin film sample.
Technical scheme of the present invention is as follows:
High-temperature heat treatment device under the magnetic field, comprise tubular heater, it is characterized in that described tubular heater is positioned between the magnet cartridge of direct current water-cooled magnet, described direct current water-cooled magnet is connected with direct current magnet power supply and circulating water cooling system, the heating chamber of described tubular heater is linked with pumped vacuum systems and atmosphere control system, and tubular heater also is connected with temperature controller.
High-temperature heat treatment device under the described magnetic field is characterized in that described pumped vacuum systems is to be made of oil-sealed rotary pump and vacuum valve, and the atmosphere control system is to be made of gas rotameter or mass-flow gas meter and control power supply thereof.
High-temperature heat treatment device under the described magnetic field is characterized in that described distance between two poles adjusting range: 60～150mm; When distance between two poles～60mm, the magnetic field size: 0～2 tesla is adjustable.
High-temperature heat treatment device under the described magnetic field, it is characterized in that described tubular heater structure is: the no magnetic material water cooling cavity that includes double layer jacket structure, described no magnetic material water cooling cavity two ends are equipped with the insulation material end cap, described no magnetic material water cooling cavity inner wall is provided with several layers of high-temperature-resistant thermal-insulation material and surrounds heating chamber, be provided with several Elema heaters in the described heating chamber, the two ends that are separately installed with Elema on the described insulation material end cap connect and draw, and cross in the middle of the described tubular heater and are provided with boiler tube.
High-temperature heat treatment device under the described magnetic field is characterized in that described end cap adopts high density high rigidity insulation material, and described high-temperature-resistant thermal-insulation material adopts high temperature alumina insulation fibre material, and described boiler tube adopts aluminium oxide ceramics or silica glass material; Described water cooling cavity adopts the magnetism-free stainless steel material.
The high-temperature heat treatment device prepares the method for bismuth ferrite thin film under the described magnetic field, it is characterized in that process is as follows:
(1), according to bismuth: iron is (1-1.05): 1 mol ratio, weighing bismuth nitrate, ferric nitrate, earlier bismuth nitrate, ferric nitrate are dissolved in the mono methoxy ether, under 50-60 ℃ of temperature, stir and dissolved fully to bismuth nitrate, ferric nitrate in 15-20 minute, wherein, the volume of mono methoxy ether: the molal quantity of ferric nitrate is that (5-6) rises: 1 mole; Afterwards, add anhydrous acetic acid, at room temperature stirred 20-30 minute, the volume of anhydrous acetic acid wherein: the volume of mono methoxy ether is 2: (2-3), add monoethanolamine at last, the volume of monoethanolamine wherein: the volume of anhydrous acetic acid is 1: (14-16), and under the room temperature agitating solution 3-4 hour and obtain forerunner's colloid of ferrous acid bismuth;
(2), adopt coating processes to be coated in ferrous acid bismuth forerunner colloid to form gel mould on the silicon chip, be placed on baking oven again, in air 330-350 ℃ dry, pyrolysis 8-10 minute down;
(3), repetitive process (2) is to required bismuth ferrite thin film thickness;
(4), will reach certain thickness ferrous acid bismuth pyrolysis film, be placed on 530-550 ℃ of annealing 40-60 minute down that is rapidly heated in the tubular heater of high-temperature heat treatment device under the described magnetic field, in annealing process, apply magnetic field, atmosphere is air, like this bismuth ferrite thin film that can obtain to prepare under the magnetic field.
Described method is characterized in that the process of more optimizing is as follows:
(1), according to bismuth: iron is 1.05: 1 mol ratio, weighing bismuth nitrate, ferric nitrate.Earlier bismuth nitrate, ferric nitrate are dissolved in the mono methoxy diethyl ether solution, stir at 60 ℃ and dissolved fully to bismuth nitrate, ferric nitrate in 20 minutes, wherein, the volume of mono methoxy ether: the molal quantity of ferric nitrate is 6 liters: 1 mole.Afterwards, add anhydrous acetic acid, at room temperature stirred 30 minutes, the volume of anhydrous acetic acid wherein: the volume of mono methoxy ether is 2: 3, add monoethanolamine at last, the volume of monoethanolamine wherein: the volume of anhydrous acetic acid is 1: 16, agitating solution 4 hours under the room temperature and obtain forerunner's colloid of ferrous acid bismuth;
(2), adopt coating processes to be coated in ferrous acid bismuth forerunner colloid to form gel mould on the silicon chip, be placed on cabinet-type electric furnace again 350 ℃ of dry, pyrolysis 10 minutes down in air;
(3), repetitive process (2) is to required bismuth ferrite thin film thickness;
(4), will reach certain thickness ferrous acid bismuth pyrolysis film, be placed on the 550 ℃ of annealing 60 minutes down that are rapidly heated in the tubular heater of high-temperature heat treatment device under the described magnetic field, apply magnetic field in annealing process, atmosphere is air, like this bismuth ferrite thin film that can obtain to prepare under the magnetic field.
The present invention adopts direct current water-cooled magnet as magnetic field generator, has to make and low, the simple to operate characteristics of operating cost; The high-temperature tubular oven enclosure adopts double-deck magnetism-free stainless steel material to constitute the water cooling cavity, and be connected with water inlet pipe and outlet pipe, heater is connected in series by several Elemas, heat-insulation and heat-preservation adopts the high-temperature resistant aluminium oxide insulation fibre, has that volume is little, characteristics such as the efficiency of heating surface and magnetic field utilization ratio height.Elema and heater thereof closely contact with high-temperature resistant aluminium oxide insulation fibre material, leave the space between Elema heater and the boiler tube.The tube furnace boiler tube atmosphere that can vacuumize and ventilate is handled, to adapt to the preparation requirement of different materials.This device is used for the synthetic and heat treatment of material, particularly to the synthetic and heat treatment of magnetic material and low-dimension nano material, might play regulating and controlling effect to micro-structural and the performance of material, thereby prepare the new material that is difficult to obtain with usual method and new material character.
Utilize (001) grain orientation of the bismuth ferrite thin film of the inventive method preparation to strengthen, and the compact structure of film, even; The dielectric properties of bismuth ferric film material, magnetic property and magneto-electric coupled performance are improved significantly, and its ferroelectricity and electric leakage performance also are improved.
Description of drawings:
Fig. 1 constitutes schematic diagram for apparatus of the present invention.
Fig. 2 is the tubular heater sectional structure chart.
Fig. 3 is that the bismuth ferrite thin film for preparing under the magnetic field of zero magnetic field and varying strength adopts the X-ray diffracting spectrum (XRD) that obtains after the test of Phillips X ' Pert type x-ray diffractometer;
Fig. 4 for adopt take the photograph behind the LEO 1530 type field emission scanning electron microscopes observation surface topography stereoscan photograph, number in the figure (a) is BF1, (b) is BF2, (c) is BF3.
The magnetic property result that Fig. 5 adopts MPMS XL type superconducting quantum interference device (SQUID) to measure for bismuth ferrite thin film.(a) figure is that the intensity of magnetization of sample concerns with variation of temperature, and (b) figure be sample in temperature is that 27 ℃ (300K) intensity of magnetization of measuring down is with the magnetic field variation relation of (being parallel to film surface).
The result that the dielectric constant that Fig. 6 adopts TH2828/A/S type LCR electric impedance analyzer to measure for bismuth ferrite thin film changes with measuring frequency, illustration is the result that the dielectric loss of sample changes with measuring frequency.
Fig. 7 is that the thin employing of ferrous acid bismuth LCR electric impedance analyzer is combined the magnetic dielectric properties result who measures with superconducting quantum interference device (SQUID), and wherein illustration is for hanging down the enlarged drawing of place.
Label among Fig. 1,2:
1, temperature controller, 2, direct current water-cooled magnet, 3 vacuum systems, 4, tubular heater, 5, direct current magnet power supply, 6, the atmosphere control system, 7, recirculating cooling water system, 8, outlet pipe; 9, non-magnetic rustproof outer steel shell; 10, cooling water cavity; 11, high temperature alumina insulation fibre material; 12, high density high rigidity insulation material; 13, Elema; 14, water inlet pipe; 15, aluminium oxide ceramics or quartz glass boiler tube; 16, Elema heater.
The specific embodiment
Below in conjunction with accompanying drawing apparatus of the present invention are elaborated.
The formation of apparatus of the present invention as shown in Figure 1, mainly by 1, temperature controller, 2, direct current water-cooled magnet, 3 vacuum systems, 4, tubular heater, 5, direct current magnet power supply, 6, the atmosphere control system, 7, recirculating cooling water system forms.Tubular heater 4 is positioned between the magnet cartridge of direct current water-cooled magnet 2, direct current water-cooled magnet 2 is connected with direct current magnet power supply 5 and circulating water cooling system 7, the heating chamber of described tubular heater 4 is linked with pumped vacuum systems 3 and atmosphere control system 6, and tubular heater 4 also is connected with temperature controller 1.
The pole of magnet area of bed of direct current water-cooled magnet 2: diameter 80～200mm, maximum adjusting range: the 60～150mm of distance between two poles, the magnetic field size: 0～2 tesla is adjustable when distance between two poles～60mm.The sectional structure chart of tubular heater 4 as shown in Figure 2, body of heater shell 9 adopts double-jacket formula magnetism-free stainless steel material to constitute water cooling cavity 10, cavity gap 1～8mm, the water cooling cavity is connected with water inlet pipe 14 and outlet pipe 8, the heating furnace heater is connected in series by four Elemas 13, Elema heater 16 contacts with high-temperature resistant aluminium oxide insulation fibre material 11, and water cooling cavity two ends are equipped with end cap structural thermal insulation material, and insulation material is selected high-density hard insulation material 12 for use.For ease of installing, insulation material 11 and 12 is made the form of splitting respectively and is fastened mutually, and presses the size and dimension hollow out grooving shape of Elema, and four Elemas 13 and heater 16 thereof are played mutual isolation and supporting role.Boiler tube adopts high temperature alumina earthenware or quartz glass tube 15, and diameter is less than 40mm.Elema and heater thereof closely contact with insulation material, leave the space between Elema heater and the boiler tube.Body of heater appearance and size: long 400～700mm, high 100～200mm, wide 60～120mm.1300 ℃ of maximum temperatures.Installing parameter designing such as used direct current water-cooled magnet 2 and direct current magnet power supply 5 power is complementary, by regulating the size in output power of power supply change magnetic field, direct current magnet power supply 5 links to each other with recirculating cooling water system 7 as required, temperature controller 1 adopts the temperature programmed control mode, pumped vacuum systems 3 is made of oil-sealed rotary pump and vacuum valve etc., and atmosphere control system 6 is made of gas rotameter or mass-flow gas meter and control power supply thereof.Tubular heater 4 is positioned between the two magnetic pole heads of direct current water-cooled magnet 2, and pending sample is positioned over the center of boiler tube usually, is in the homogeneity range of magnetic field.Parameters such as different magnetic field, temperature, vacuum or atmosphere flow are set according to the material heat treatment needs.
Among Fig. 3, abscissa is the angle of diffraction, and ordinate is the relative intensity of diffraction maximum, and number in the figure BF1, BF2 and BF3 represent zero magnetic field (being suitable for following all diagrams), the bismuth ferrite thin film for preparing under the magnetic field of 3000 gaussian sums, 6500 Gauss's sizes respectively.By the position of each diffraction maximum among the XRD figure and relative intensity as can be known, the film of preparation is bismuth ferrite thin film, and bismuth ferrite thin film has height (001) grain orientation.And (wherein, abscissa is by being added preparation magnetic field size, and left ordinate is crystallite dimension for the illustration from figure, right ordinate is the texture degree of film) in can find, with adding magnetic field increase, (001) orientation of ferrous acid bismuth strengthens, but crystallite dimension obviously changes.
Fig. 4 for adopt take the photograph behind the LEO 1530 type field emission scanning electron microscopes observation surface topography stereoscan photograph, number in the figure (a) is BF1, (b) is BF2, (c) is BF3.As can be seen from the figure (BF2, the BF3) bismuth ferrite thin film (BF1) for preparing under the no magnetic field have fine and close, pattern and bigger particle size uniformly to the bismuth ferrite thin film for preparing under the magnetic field.
The magnetic property result that Fig. 5 adopts MPMS XL type superconducting quantum interference device (SQUID) to measure for bismuth ferrite thin film.(a) figure is that the intensity of magnetization of sample concerns with variation of temperature, finds that the intensity of magnetization of the bismuth ferrite thin film for preparing under the bigger magnetic field is bigger in measured warm area.(b) figure is that sample is that the intensity of magnetization of 27 ℃ (300K) is with the variation relation in the magnetic field of measuring that is parallel to film surface in temperature.The intensity of magnetization of the bismuth ferrite thin film for preparing under the magnetic field that discovery is bigger is bigger in measured magnetic field range equally.
The dielectric properties result that Fig. 6 adopts TH2828/A/S type LCR electric impedance analyzer to measure for bismuth ferrite thin film.Be the result that dielectric constant changes with measuring frequency, illustration is the result that the dielectric loss of sample changes with measuring frequency, finds that the bismuth ferrite thin film for preparing under the magnetic field has bigger dielectric constant and less dielectric loss.
Fig. 7 is the magnetic dielectric properties result that ferrous acid bismuth thin employing LCR electric impedance analyzer and superconducting quantum interference device (SQUID) are measured, and wherein illustration is the enlarged drawing of low place.The bismuth ferrite thin film for preparing under the discovery magnetic field is compared the bismuth ferrite thin film for preparing under the null field and is had bigger magneto-electric coupled effect.
Claims (2)
1. the high-temperature heat treatment device prepares the method for bismuth ferrite thin film under the magnetic field, it is characterized in that, include high-temperature heat treatment device under the magnetic field, its structure is: tubular heater is positioned between the magnet cartridge of direct current water-cooled magnet, described direct current water-cooled magnet is connected with direct current magnet power supply and circulating water cooling system, the heating chamber of described tubular heater is linked with pumped vacuum systems and atmosphere control system, and tubular heater also is connected with temperature controller; Described pumped vacuum systems is to be made of oil-sealed rotary pump and vacuum valve, and the atmosphere control system is to be made of gas rotameter or mass-flow gas meter and control power supply thereof; Described magnet cartridge spacing adjustable range: 60～150mm; When distance between two poles 60mm, the magnetic field size: 0-2 tesla is adjustable; Described tubular heater structure is: the no magnetic material water cooling cavity that includes double layer jacket structure, described no magnetic material water cooling cavity two ends are equipped with the insulation material end cap, described no magnetic material water-cooled cavity inner wall is provided with several layers of high-temperature-resistant thermal-insulation material and surrounds heating chamber, be provided with several Elema heaters in the described heating chamber, the two ends that are separately installed with the Elema heater on the described insulation material end cap connect and draw, and cross in the middle of the described tubular heater and are provided with boiler tube; Described end cap adopts high density high rigidity insulation material, and described high-temperature-resistant thermal-insulation material adopts high temperature alumina insulation fibre material, and described boiler tube adopts aluminium oxide ceramics or silica glass material; Described water cooling cavity adopts the magnetism-free stainless steel material;
Process is as follows:
(1), according to bismuth: iron is (1-1.05): 1 mol ratio, weighing bismuth nitrate, ferric nitrate, earlier bismuth nitrate, ferric nitrate are dissolved in the mono methoxy ether, under 50-60 ℃ of temperature, stir and dissolved fully to bismuth nitrate, ferric nitrate in 15-20 minute, wherein, the volume of mono methoxy ether: the molal quantity of ferric nitrate is that (5-6) rises: 1 mole; Afterwards, add anhydrous acetic acid, at room temperature stirred 20-30 minute, the volume of anhydrous acetic acid wherein: the volume of mono methoxy ether is 2: (2-3), add monoethanolamine at last, the volume of monoethanolamine wherein: the volume of anhydrous acetic acid is 1: (14-16), and under the room temperature agitating solution 3-4 hour and obtain forerunner's colloid of ferrous acid bismuth;
(2), adopt coating processes to be coated in ferrous acid bismuth forerunner colloid to form gel mould on the silicon chip, be placed on baking oven again, in air 330-350 ℃ dry, pyrolysis 8-10 minute down;
(3), repetitive process (2) is to required bismuth ferrite thin film thickness;
To reach certain thickness ferrous acid bismuth pyrolysis film, be placed on 530-550 ℃ of annealing 40-60 minute down that is rapidly heated in the tubular heater of high-temperature heat treatment device under the described magnetic field, apply magnetic field in annealing process, atmosphere is air, like this bismuth ferrite thin film that can obtain to prepare under the magnetic field.
2. method according to claim 1 is characterized in that the process of more optimizing is as follows;
(1), according to bismuth: iron is 1.05: 1 mol ratio, weighing bismuth nitrate, ferric nitrate, earlier bismuth nitrate, ferric nitrate are dissolved in the mono methoxy diethyl ether solution, stir at 60 ℃ and to dissolve fully to bismuth nitrate, ferric nitrate in 20 minutes, wherein, the volume of mono methoxy ether: the molal quantity of ferric nitrate is 6 liters: 1 mole; Afterwards, add anhydrous acetic acid, at room temperature stirred 30 minutes, the volume of anhydrous acetic acid wherein: the volume of mono methoxy ether is 2: 3, add monoethanolamine at last, the volume of monoethanolamine wherein: the volume of anhydrous acetic acid is 1: 16, agitating solution 4 hours under the room temperature and obtain forerunner's colloid of ferrous acid bismuth;
(2), adopt coating processes to be coated in ferrous acid bismuth forerunner colloid to form gel mould on the silicon chip, be placed on cabinet-type electric furnace again 350 ℃ of dry, pyrolysis 10 minutes down in air;
(3), repetitive process (2) is to required bismuth ferrite thin film thickness;
(4), will reach certain thickness ferrous acid bismuth pyrolysis film, be placed on the 550 ℃ of annealing 60 minutes down that are rapidly heated in the tubular heater of high-temperature heat treatment device under the described magnetic field, apply magnetic field in annealing process, atmosphere is air, like this bismuth ferrite thin film that can obtain to prepare under the magnetic field.
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| CN105749827B (en) * | 2016-02-26 | 2019-04-26 | 东北大学 | A kind of device and method using high-intensity magnetic field liquid phase synthesis low-dimension nano material |
| CN106969634B (en) * | 2017-03-31 | 2019-02-19 | 西京学院 | A kind of more atmosphere calciner plants of use for laboratory nano particle |
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| CN1389879A (en) * | 2001-04-17 | 2003-01-08 | 日立金属株式会社 | Heat treatment furnace in magnetic field and heat treatment method thereof |
| WO2003093520A1 (en) * | 2002-04-27 | 2003-11-13 | Emerson Electric (China) Holdings Co. Ltd. | PROCESS FOR INCREASING MAGNETIC-FIELD-INDUCED STRAIN IN POLYCRYSTALLINE Ni2MnGa BY MAGNETIC HEAT TREATMENT |
| CN2879162Y (en) * | 2006-01-24 | 2007-03-14 | 东北大学 | High temperature processing device under strong magnetic field |
| CN101157125A (en) * | 2007-11-16 | 2008-04-09 | 中国科学院电工研究所 | A method and apparatus for processing metallic material within complex magnetic field |
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| CN1389879A (en) * | 2001-04-17 | 2003-01-08 | 日立金属株式会社 | Heat treatment furnace in magnetic field and heat treatment method thereof |
| WO2003093520A1 (en) * | 2002-04-27 | 2003-11-13 | Emerson Electric (China) Holdings Co. Ltd. | PROCESS FOR INCREASING MAGNETIC-FIELD-INDUCED STRAIN IN POLYCRYSTALLINE Ni2MnGa BY MAGNETIC HEAT TREATMENT |
| CN2879162Y (en) * | 2006-01-24 | 2007-03-14 | 东北大学 | High temperature processing device under strong magnetic field |
| CN101177775A (en) * | 2006-11-10 | 2008-05-14 | 中国科学院物理研究所 | Vacuum deposition film and film heat treating plant having applied magnetic field |
| CN101157125A (en) * | 2007-11-16 | 2008-04-09 | 中国科学院电工研究所 | A method and apparatus for processing metallic material within complex magnetic field |
| CN101186341A (en) * | 2007-12-03 | 2008-05-28 | 哈尔滨工业大学 | Method for preparing (100) preferred orientation bismuth ferrite thin film |
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