CN114751460A - Sol-gel preparation method of rare earth ferrite lutetium ferrite film - Google Patents
Sol-gel preparation method of rare earth ferrite lutetium ferrite film Download PDFInfo
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Abstract
The invention discloses a sol-gel preparation method of a rare earth ferrite lutetium ferrite film. The method comprises sol-gel, spin coating film preparation and heat treatment processes, ensures that the film grows completely and compactly without cracks by regulating and controlling the reasonable matching of sol concentration and rotating speed and drying temperature and time, and ensures that the film grows directionally without impurities by regulating and controlling pre-annealing temperature and time, annealing temperature and time. The invention uses the spin coating of the spin coater to prepare the film, has low equipment cost, short film crystallization time and simple process, and is beneficial to industrialized large-scale production. The lutetium ferrite film prepared by the method has the advantages of good growth orientation, no impurities, compact and complete growth, no cracks, excellent resistance change property, nonlinear electrical transport property and photoelectric property, and huge application potential and wide application prospect in the aspects of microelectronic devices, detectors and the like.
Description
Technical Field
The invention belongs to the field of ferrite film preparation, and particularly relates to rare earth ferrite lutetium ferrite (LuFe)2O4) A sol-gel preparation method of a film.
Background
With the rapid development of electronic devices, electronic memory devices have become increasingly important in our lives. Nonvolatile random access memories are becoming more popular due to their easy operation, high speed, low power consumption, high density, and simple structure, so that the preparation and development of resistive materials are of great importance, and thin film materials with high on-off ratio and resistive properties are easier to realize device miniaturization and integration. With the continuous development of the photoelectric technology, the photoelectric detection sensor attracts much attention due to its wide application in the industrial, military, biological and environmental fields, and therefore, higher requirements are put on materials having photoelectric properties, faster optical response speed and higher on-off ratio.
The lutetium ferrite film can form a built-in electric field in the film due to factors such as special crystal structures and the like, so that the electrical property response of the film is enhanced, and the lutetium ferrite film has high resistance adjustability and photoelectric properties. In addition, the lutetium ferrite film is also a multiferroic material, has ferroelectricity and ferromagnetism at the same time, and can realize electric control magnetism or magnetic control electricity through magnetoelectric coupling. In 2012, molecular beam epitaxy was used by Brooks at cornell university, usa at 1 × 10 -6At the temperature of Torr and 850 ℃, MgAl is successfully generated2O4(111) Lutetium ferrite single crystal thin films (Charles m. brooks, Julia a. mundy. applied Physics Letters,2012,101(13):132907.) were grown on three substrates, MgO (111) and 6H-SiC (0001). In the same year, Dai et Al of hong Kong university of science and technology uses lutetium ferrite ceramic prepared by laser pulse deposition method as target material under certain pressure and temperature in Al2O3(001) The lutetium ferrite film (M.Zeng, J.Liu, Y.B.Qin, et al.thin Solid Films,2012,520(20): 6446-. The two preparation methods have the advantages that the crystal growth environment can be accurately regulated and controlled to control the thickness of the film, and the defects that the equipment and the production cost are expensive, the growth period of the film is long, and the film is not suitable for large-scale preparation. Therefore, a chemical method which has low production cost and is easy to realize large-scale preparation of the lutetium ferrite film is urgently needed to solve the application obstruction of the film material.
Disclosure of Invention
The invention aims to provide a sol-gel preparation method of a rare earth ferrite lutetium ferrite film. The method comprises sol-gel, spin coating film preparation and heat treatment processes, ensures that the film grows completely and compactly without cracks by regulating and controlling the reasonable matching of sol concentration and rotating speed and drying temperature and time, and ensures that the film grows directionally without impurities by regulating and controlling pre-annealing temperature and time and annealing temperature and time.
The sol-gel preparation method of the rare earth ferrite lutetium ferrite film comprises the following steps:
(1) mixing the molar ratio of l: 2 dissolving the lutetium source and the iron source in the organic solvent, magnetically stirring for 2-24h until the solution is completely clear, standing and aging for 24-72h to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on a substrate, spin-coating at 1000-5000r/min for 10-120s, and then drying at 100-150 ℃ in vacuum for 10min-1h to obtain a precursor;
(3) taking out the precursor obtained in the step (2) after preannealing for 5-30min at the temperature of 200-450 ℃, and naturally cooling; then placing the film in an annealing furnace, firstly vacuumizing to reduce the air pressure in the annealing furnace to below 5Pa, then introducing argon for 10-30min, raising the temperature to 800-1300 ℃ at the heating rate of 2-20 ℃/min, and preserving the temperature for 0.5-5h to obtain the lutetium ferrite film.
The lutetium source is lutetium nitrate and/or lutetium chloride. The iron source is ferric nitrate and/or ferric chloride.
The organic solvent is ethylene glycol and/or ethylene glycol methyl ether.
The concentration of lutetium element in the gel obtained in the step (1) is 0.25-1.5M.
The substrate is selected from MgO (111) and Al2O3(001)、YSZ(111)、MgAl2O4(111) 4H-SiC (0001), ZnO (0001), and Si (001).
The flow rate of the argon is 0.5-5dm3/s。
And (3) repeating the steps (2) and (3) for a plurality of times to obtain the lutetium ferrite films with different thicknesses.
The invention adopts a sol-gel method, uses a compound containing high chemical activity components as a precursor, realizes the uniform mixing of the raw materials at the molecular level in a liquid phase, and carries out hydrolysis and condensation reactions, thereby being beneficial to the growth of crystals. The preparation of the complete compact crack-free lutetium ferrite film is realized by regulating and controlling the reasonable matching of sol concentration and rotating speed and three heat treatments of drying, pre-annealing and high-temperature annealing; the oriented growth of the film is realized without impurities by regulating and controlling the pre-annealing temperature and time, the high-temperature annealing temperature and time and changing the flow of argon to control the oxygen partial pressure. The invention uses the spin coating of the spin coater to prepare the film, has low equipment cost, short film crystallization time and simple process, and is beneficial to industrialized large-scale production. The lutetium ferrite film prepared by the invention has the advantages of good growth orientation, no impurities, compact and complete growth, no cracks, excellent resistance change property, nonlinear electric transport property and photoelectric property, and huge application potential and wide application prospect in the aspects of microelectronic devices, detectors and the like.
Drawings
FIG. 1 is a photograph of a lutetium ferrite film prepared in accordance with an embodiment of the present invention;
FIG. 2 is an XRD pattern of lutetium ferrite films prepared in examples 1-3;
FIG. 3 is an SEM image of a lutetium ferrite thin film prepared in example 1;
FIG. 4 is an optical micrograph of a lutetium ferrite film prepared in example 1;
FIG. 5 is a graph of the electrical transport properties of the lutetium ferrite film prepared in example 1;
FIG. 6 is a graph of the optoelectronic properties of the lutetium ferrite film prepared in example 1.
Detailed Description
Example 1
(1) Mixing the components in a molar ratio of 1: 2, dissolving lutetium nitrate and ferric nitrate in ethylene glycol, wherein the concentration of lutetium is 0.75M, magnetically stirring for 24 hours until the solution is completely clear, standing and aging for 48 hours to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on a Si (001) substrate, spin-coating at 3000r/min for 30s, and then carrying out vacuum drying at 110 ℃ for 30min to obtain a precursor;
(3) and (3) putting the precursor obtained in the step (2) into a reaction boat, pre-annealing for 15min at 300 ℃ by using a tube furnace, taking out and naturally cooling. Then the reaction boat is placed in an annealing furnace, and the annealing furnace is firstly vacuumized to annealThe pressure in the furnace is reduced to below 5Pa, and then high-purity argon (99.999 percent with the volume flow rate of 3 dm) is introduced3And/s) after 10min, heating to 950 ℃ at the heating rate of 3 ℃/min, and preserving heat for 4h to obtain the lutetium ferrite film which has good growth orientation, no impurities, compact and complete growth and no cracks.
Example 2
(1) Mixing the components in a molar ratio of 1: 2, dissolving lutetium chloride and ferric chloride in ethylene glycol, wherein the concentration of lutetium element is 0.5M, magnetically stirring for 24 hours until the solution is completely clear, standing and aging for 48 hours to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on a ZnO (0001) substrate, spin-coating for 10s at 4000r/min, and then carrying out vacuum drying for 1h at 100 ℃ to obtain a precursor;
(3) and (3) putting the precursor obtained in the step (2) into a reaction boat, pre-annealing for 5min at 450 ℃ by using a tube furnace, taking out and naturally cooling. Then the reaction boat is placed in an annealing furnace, the annealing furnace is vacuumized to reduce the air pressure in the annealing furnace to below 5Pa, and then high-purity argon (99.999 percent with the volume flow rate of 0.5 dm) is added3And/s) 20min later, heating to 1300 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1h to obtain the lutetium ferrite film which has good growth orientation, no impurities, compact and complete growth and no cracks.
Example 3
(1) Mixing the components in a molar ratio of 1: 2, dissolving lutetium nitrate and ferric chloride in ethylene glycol monomethyl ether, wherein the concentration of lutetium is 0.25M, magnetically stirring for 16h until the solution is completely clear, standing and aging for 48h to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on an MgO (111) substrate, spin-coating at 2000r/min for 40s, and then drying in vacuum at 150 ℃ for 10min to obtain a precursor;
(3) And (3) putting the precursor obtained in the step (2) into a reaction boat, pre-annealing for 30min at 200 ℃ by using a tube furnace, taking out and naturally cooling. Then the reaction boat is placed in an annealing furnace, the annealing furnace is vacuumized to reduce the air pressure in the annealing furnace to be below 5Pa, and then high-purity argon (99.999 percent with the volume flow rate of 4 dm) is added3And/s) 30min later, raising the temperature to 1200 ℃ at the heating rate of 4 ℃/min, and preserving the temperature for 2h to obtain the lutetium ferrite film which has good growth orientation, no impurities, compact and complete growth and no cracks.
Example 4
(1) Mixing the components in a molar ratio of 1: 2, dissolving lutetium chloride and ferric nitrate in ethylene glycol monomethyl ether, wherein the concentration of lutetium is 1.25M, magnetically stirring for 24 hours until the solution is completely clear, standing and aging for 48 hours to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on a 4H-SiC (0001) substrate, carrying out spin coating at 3500r/min for 25s, and then carrying out vacuum drying at 120 ℃ for 30min to obtain a precursor;
(3) and (3) putting the precursor obtained in the step (2) into a reaction boat, pre-annealing for 10min at 350 ℃ by using a tube furnace, taking out and naturally cooling. Then the reaction boat is placed in an annealing furnace, the annealing furnace is vacuumized to reduce the air pressure in the annealing furnace to below 5Pa, and then high-purity argon (99.999 percent with the volume flow rate of 3 dm) is added3S)20min later, heating to 1100 ℃ at the heating rate of 4 ℃/min, and preserving heat for 3 h;
(4) And (4) repeating the steps (2) and (3) for 5 times to obtain the lutetium ferrite film with good growth orientation, no impurities, compact and complete growth and no cracks.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. A sol-gel preparation method of a rare earth ferrite lutetium ferrite film is characterized by comprising the following specific steps:
(1) mixing the molar ratio of l: 2 dissolving the lutetium source and the iron source in the organic solvent, magnetically stirring for 2-24h until the solution is completely clear, standing and aging for 24-72h to obtain gel;
(2) uniformly coating the gel obtained in the step (1) on a substrate, spin-coating at 1000-5000r/min for 10-120s, and then drying at 100-150 ℃ in vacuum for 10min-1h to obtain a precursor;
(3) taking out the precursor obtained in the step (2) after preannealing for 5-30min at the temperature of 200-450 ℃, and naturally cooling; then placing the film in an annealing furnace, firstly vacuumizing the annealing furnace to reduce the air pressure in the annealing furnace to below 5Pa, then introducing argon for 10-30min, raising the temperature to 800-1300 ℃ at the heating rate of 2-20 ℃/min, and preserving the temperature for 0.5-5h to obtain the lutetium ferrite film.
2. A method of manufacture as in claim 1, wherein the source of lutetium is lutetium nitrate and/or lutetium chloride.
3. The method according to claim 1, wherein the iron source is ferric nitrate and/or ferric chloride.
4. The production method according to claim 1, wherein the organic solvent is ethylene glycol and/or ethylene glycol methyl ether.
5. The method of claim 1, wherein the gel obtained in step (1) has a lutetium concentration of 0.25 to 1.5M.
6. The method according to claim 1, wherein the substrate is selected from MgO (111), Al2O3(001)、YSZ(111)、MgAl2O4(111) 4H-SiC (0001), ZnO (0001), and Si (001).
7. The method according to claim 1, wherein the argon is introduced at a flow rate of 0.5 to 5dm3/s。
8. The method of claim 1, wherein steps (2) and (3) are repeated several times to obtain lutetium ferrite films of different thicknesses.
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