CN103951404A - Chemical preparation method of Bi4LaTi3FeO15 multiferroic film - Google Patents

Chemical preparation method of Bi4LaTi3FeO15 multiferroic film Download PDF

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CN103951404A
CN103951404A CN201410139124.8A CN201410139124A CN103951404A CN 103951404 A CN103951404 A CN 103951404A CN 201410139124 A CN201410139124 A CN 201410139124A CN 103951404 A CN103951404 A CN 103951404A
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lati
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CN103951404B (en
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宿杰
卢朝靖
王晓杰
李华兵
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Qingdao University
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Abstract

The invention belongs to the technical field of physico-chemical material preparation, and relates to a chemical preparation method of a Bi4LaTi3FeO15 multiferroic film. The method is characterized in that single-layer magnetic octahedral group LaFeO3 is inserted into three-layer of layered perovskite-type ferroelectric Bi4Ti3O12 to form a novel four-layer layered perovskite-type Bi4LaTi3FeO15 multiferroic film. According to the method of the invention, a Bi4LaTi3FeO15 precursor sol is firstly prepared by a chemical preparation method, and then is deposited on a clean substrate of (111)Pt/Ti/SiO2/Si(100) directly to form a wet film; and annealing treatment in O2 atmosphere is carried out in a rapid heat treatment furnace. The method is simple in required equipment, low in cost, compatible with microelectronic technology and process, and suitable for industrial production. The prepared Bi4LaTi3FeO15 multiferroic film is pure in phase, good in ferroelectric properties, and quite beneficial to application and popularization of Bi4LaTi3FeO15 multiferroic films.

Description

A kind of Bi 4laTi 3feO 15the chemical preparation process of many iron thin films
Technical field
The invention belongs to physical chemistry technical field of material, relate to a kind of Bi 4laTi 3feO 15the chemical preparation process of many iron thin films.
Background technology
Multi-ferroic material can show ferroelectricity and magnetic simultaneously, and between them, has magneto-electric coupled effect, thereby can realize mutual regulation and control (N.A.Spaldin and M.Fiebig, Science309,391 (2005) of ferroelectricity and magnetic; W.Eerenstein, N.D.Mathur, and J.F.Scott, Nature442,759 (2006); M.Bibes, and A.Barth é 1 é my, Nature Mater.7,425 (2008)).Therefore, multi-iron material, as a kind of Multifunction material, has broad application prospects at spintronics and other field.Wherein multiferroic film material can be compatible with microelectronic technique, makes many iron thin films can be widely used in the fields such as micro sensor and multiple-state storage.For example, magnetic recording reading speed writes slow soon, and ferroelectric record reads complexity and writes soon, if use many ferroelectric material films as recording medium, can realize the read-write process of two-forty.
Realize multiple-state storage and will obtain the good many iron thin films of ferroelectric properties, this target majority deposits epitaxial film by Physical and realizes, as: pulsed laser deposition, molecular beam epitaxy, (the J.Wang such as magnetron sputtering, J.B.Neaton, H.Zheng, V.Nagarajan, S.B.Ogale, B.Liu, D.Viehland, V. Vaithyanathan, D.G. Schlom, U.V.Waghmare, N.A.Spaldin, K.M.Rabe, M.Wutting, and R.Ramesh, Science299, 1719 (2003) .Y. H.Chu, Q.He, C.H.Yang, P. Yu, LW.Martin, P. Shafer, R.Ramesh, Nano Lett.9, 1762 (2009)), but these methods need expensive complicated equipment, and not too easily realize extensive generation.Chemical method is easy to control thin film composition by contrast, and preparation technology and equipment simply can be mass-produced, and is more suitable for preparation of industrialization film.
In recent years, utilize difference to excite unit (ferroelectric cell and magnet unit) combination on atomic scale, realize single-phase multiferroic and paid close attention to widely.Its typical structure is four layers of laminated perovskite multi-iron material Bi 5mTi 3o 15(BMTO, M=Mn, Fe, Co, Ni), this structure can be regarded BiMO as 3magnet unit is inserted into three layers of laminated perovskite ferroelectrics Bi 4ti 3o 12in (J.B.Li, Y.P.Huang, G.H.Rao, G.Y.Liuet al., Appl.Phys.Lett.96,222903 (2010)).This many ferroelectric material films of class chemical constitution relative complex, most is prepared from by being easy to control thin film composition wet chemistry method, although wet chemistry method is easily prepared many iron thin films of pure phase, and the problem such as ubiquity poor ferroelectric property, leakage current are large.Similarly, there is recently article to report at Bi 4ti 3o 12in ferroelectrics, insert LaFeO 3magnet unit successfully synthesizes novel four layers of laminated perovskite Bi 4laTi 3feO 15multi-iron material (F.X.Wu, Z.Chen, Y.B.Chen, S.T.Zhang et al., Appl.Phys.Lett.98,212501 (2011)).Although insert LaFeO 3rear magnetic can strengthen, but there are no article, its ferroelectric properties is reported, this is mainly that the insertion of magnetic group can make leakage current increase, and then makes ferroelectric properties variation, thereby cannot obtain normal ferroelectric loop line.This just makes the iron material that this system is many be difficult to be actually used in the association areas such as micro sensor and multi-state memory, therefore how to obtain the Bi with good ferrum property 4laTi 3feO 15many iron thin films are current problems urgently to be resolved hurrily.
Summary of the invention
The object of the present invention is to provide a kind of Bi 4laTi 3feO 15the preparation method of many iron thin films, this invention preparation technology and required equipment are simple, cost is low, can with microelectronics process compatible, be applicable to suitability for industrialized production.Concrete technical scheme is as follows:
1.Bi 4laTi 3feO1 5the preparation of precursor sol: with analytically pure Bismuth trinitrate (Bi (NO 3) 35H 2o), lanthanum trioxide (La 2o 3), ferric acetyl acetonade (C 15h 21feO 6) and butyl (tetra) titanate (Ti (C 4h 9o) 4) etc. be main raw material; Press Bi 4laTi 3feO 15taking the various raw materials that meet chemical dosage ratio is configured; Wherein in order to make up the volatilization of the Bi element in follow-up heat treatment process, during weighing by Bi (NO 3) 35H 2excessive 4～the 6mo1% of O, concrete steps are:
(1) La: HNO in molar ratio 3measure dense HNO at=1: 20 3, then by La 2o 3join dense HNO 3in, be placed in and on magnetic stirring apparatus, be stirred to solution clarification;
(2) Bi: CH in molar ratio 3cOOH=1: 20 measure CH 3cOOH, then by Bi (NO 3) 35H 2o joins CH 3in COOH, be placed in 55 ℃ of heated and stirred 1.5h in constant temperature blender with magnetic force, to remove Bi (NO 3) 35H 2crystal water in O adds wherein C after solution cool to room temperature 15h 21feO 6, relay and on magnetic stirring apparatus, be stirred to C 15h 21feO 6dissolve;
(3) solution step (1) being obtained joins in the solution that step (2) obtains and stirs 0.5h, then by stoichiometric ratio, drips Ti (C 4h 9o) 4and stir, after mixing, adding ethylene glycol monomethyl ether is 0.05mol/L～0.1mol/L by above-mentioned gained solution constant volume;
(4) in (3) gained solution, add the methyl ethyl diketone of its volume 1% and stir 4h, it is standby that filtration obtains uniform and stable sorrel precursor sol.
2. whirl coating on sol evenning machine, the rotating speed 3000～6000rpm of sol evenning machine, even glue 30s, directly at (111) of cleaning Pt/Ti/SiO 2on/Si (100) substrate, deposit Bi 4laTi 3feO 15wet film.
3.Bi 4laTi 3feO 15wet film is heat-treated in rapid heat-treatment furnace.By prepared Bi 4laTi 3feO 15wet film is put into rapid heat-treatment furnace, with the speed of 20 ℃/s, from room temperature, is raised to 200 ℃, insulation 300s; Speed with 25 ℃/s rises to 300 ℃～450 ℃ again, insulation 250s, and finally the speed with 20 ℃/s～80 ℃/s rises to 700 ℃～800 ℃ fast, insulation 300s.At mobile O 2annealing crystallization in atmosphere, O 2flow be 1～5L/min.
4. after furnace temperature naturally cools to room temperature, film is taken out, repeating step 2 and 3,5～10 times, finally obtain Bi 4laTi 3feO 15many iron thin films.
The present invention is that preparation technology is simple, and cost is low, can with the chemical masking method of microelectronics process compatible, by adjusting the concentration of precursor solution, the annealing temperature of wet film, the flow of oxygen etc. makes Bi 4laTi 3feO 15the ferroelectric properties of multiferroic film has obtained obvious improvement.Prepared Bi 4laTi 3feO 15multiferroic film crystallization completely and without dephasign, has good ferroelectric properties, and remnant polarization is up to 13.3 μ Ccm -2.The present invention is scale operation Bi 4laTi 3feO 15multiferroic film provides robust techniques route.
Accompanying drawing explanation
The Bi that Fig. 1: embodiment 1 is prepared 4laTi 3feO 15the X-ray diffraction spectrogram of film
The Bi that Fig. 2: embodiment 2 is prepared 4laTi 3feO 15the X-ray diffraction spectrogram of film
The Bi that Fig. 3: embodiment 3 is prepared 4laTi 3feO 15the X-ray diffraction spectrogram of film
The Bi that Fig. 4: embodiment 1 is prepared 4laTi 3feO 15the ferroelectric loop line figure of film
The Bi that Fig. 5: embodiment 2 is prepared 4laTi 3feO 15the ferroelectric loop line figure of film
The Bi that Fig. 6: embodiment 3 is prepared 4laTi 3feO 15the ferroelectric loop line figure of film
The Bi that Fig. 7: embodiment 1,2,3 is prepared 4laTi 3feO 15the electric leakage flow graph of film
The Bi that Fig. 8: embodiment 1,2,3 is prepared 4laTi 3feO 15the transmission electron microscope picture of film
Embodiment
Below by specific embodiment, also the present invention is described further by reference to the accompanying drawings.
Embodiment 1
1. the preparation of precursor sol: with analytically pure Bismuth trinitrate (Bi (NO 3) 35H 2o), lanthanum trioxide (La 2o 3), ferric acetyl acetonade (C 15h 21feO 6) and butyl (tetra) titanate (Ti (C 4h 9o) 4) etc. be main raw material; Press Bi 4laTi 3feO 15taking the various raw materials that meet chemical dosage ratio is configured; Wherein in order to make up the volatilization of the Bi element in follow-up heat treatment process, during weighing by Bi (NO 3) 35H 2the excessive 4mo1% of O, concrete steps are:
(1) La: HNO in molar ratio 3measure dense HNO at=1: 20 3, then by La 2o 3join dense HNO 3in, be placed in and on magnetic stirring apparatus, be stirred to solution clarification;
(2) Bi: CH in molar ratio 3cOOH=1: 20 measure CH 3cOOH, then by Bi (NO 3) 35H 2o joins CH 3in COOH, be placed in 55 ℃ of heated and stirred 1.5h in constant temperature blender with magnetic force, to remove Bi (NO 3) 35H 2crystal water in O adds wherein C after solution cool to room temperature 15h 21feO 6, relay and on magnetic stirring apparatus, be stirred to C 15h 21feO 6dissolve;
(3) solution (1) being obtained joins in the solution that (2) obtain and stirs 0.5h, then by stoichiometric ratio, drips Ti (C 4h 9o) 4and stir, after mixing, adding ethylene glycol monomethyl ether is 0.075mol/L by above-mentioned gained solution constant volume;
(4) in (3) gained solution, add the methyl ethyl diketone of its volume 1% and stir 4h, it is standby that filtration obtains uniform and stable sorrel precursor sol.
2. whirl coating on sol evenning machine, the rotating speed 3500rpm of sol evenning machine, even glue 30s, directly at (111) of cleaning Pt/Ti/SiO 2on/Si (100) substrate, deposit Bi 4laTi 3feO 15wet film.
3.Bi 4laTi 3feO 15wet film is heat-treated in rapid heat-treatment furnace.By prepared Bi 4laTi 3feO 15wet film is put into rapid heat-treatment furnace, with the speed of 20 ℃/s, from room temperature, is raised to 200 ℃, insulation 300s; Speed with 25 ℃/s rises to 450 ℃ again, insulation 250s, and finally the speed with 60 ℃/s rises to 780 ℃ fast, and insulation 300s, at mobile O 2annealing crystallization in atmosphere, O 2flow be 4L/min.
4. after furnace temperature naturally cools to room temperature, film is taken out, repeating step 2 and 3,6 times, finally obtain Bi 4laTi 3feO 15many iron thin films.
Bi prepared by the present embodiment 4laTi 3feO 15film is mutually pure, and crystal grain is random orientation (shown in accompanying drawing 1); Film remnant polarization is high, is 13.3 μ Ccm -2, the rectangular degree of ferroelectric loop line is good, is 0.83 (shown in accompanying drawing 4); Leakage current is little, is 8.5 * 10 during 80V -5a/cm 2(shown in accompanying drawing 7).
Embodiment 2
All the other are with embodiment 1, and it is 0.1mol/L by solution constant volume that step 1 (3) adds ethylene glycol monomethyl ether.
Bi prepared by the present embodiment 4laTi 3feO 15film is mutually pure, and crystal grain is c-axis orientation (shown in accompanying drawing 2); Film remnant polarization is 1.4 μ Ccm -2, the rectangular degree of ferroelectric loop line is 0.59 (shown in accompanying drawing 5); During 80V, leakage current is 1.2 * 10 -4a/cm 2(shown in accompanying drawing 7).
Embodiment 3
All the other are with embodiment 1, and step 3 rises to 700 ℃ fast with the speed of 60 ℃/s.
Bi prepared by the present embodiment 4laTi 3feO 15film has a small amount of dephasign, and crystal grain is random orientation (shown in accompanying drawing 1); Film remnant polarization is 11.4 μ Ccm -2, the rectangular degree of ferroelectric loop line is 0.73 (shown in accompanying drawing 6); During 80V, leakage current is 1.5 * 10 -4a/cm 2(shown in accompanying drawing 7).
Bi 4laTi 3feO 15many iron thin films, because the insertion of magnetic group increases its leakage current, cause its ferroelectric properties variation, thereby cannot meet application requiring.In addition, this film chemical forms relative complex, and preparation process easily produces dephasign.Therefore prepare pure phase and the good Bi of ferroelectric properties 4laTi 3feO 15many iron thin films are desired always.
Comparative example 1, embodiment 2 and embodiment 3 can find out: the Bi that embodiment 1 prepares 4laTi 3feO 15film is mutually pure, and degree of crystallinity is complete, and crystal grain is random orientation; The Bi that embodiment 1 is prepared 4laTi 3feO 15the remnant polarization of film is up to 13.3 μ Ccm -2, higher than embodiment 2 and 3 prepared film remnant polarizations, (be respectively 11.4 and 1.3 μ Ccm -2); The Bi that embodiment 1 is prepared 4laTi 3feO 15the rectangular degree of thin-film ferroelectric loop line (0.83) is obviously better than the rectangular degree (being respectively 0.59 and 0.73) of embodiment 2 and the prepared thin-film ferroelectric loop line of example 3; The Bi that embodiment 1 is prepared 4laTi 3feO 15the leakage current of film is minimum, and when impressed voltage is 80V, leakage current is 8.5 * 10 -5a/cm 2, than the leakage current of embodiment 2 and example 3 prepared films low nearly order of magnitude.The prepared Bi of embodiment 1 in a word 4laTi 3feO 15many iron thin films are mutually pure, and degree of crystallinity is complete, and crystal grain is random orientation, and leakage current is minimum, and ferroelectric properties is optimum.In addition from the high resolution picture (shown in accompanying drawing 8) of transmission electron microscope, can find out Bi 4laTi 3feO 15film really by the octahedra group L aFeO of one deck magnetic 3be inserted into three shape Ferroelectrics Bi layer by layer 4ti 3o 12middle formation novel four is shape perovskite typed multi-iron material layer by layer, rather than simple doping vario-property.

Claims (4)

1. a Bi 4laTi 3feO 15the chemical preparation process of many iron thin films, is characterized in that, comprises the steps:
(a) Bi 4laTi 3feO 15the preparation of precursor sol: with analytically pure Bismuth trinitrate (Bi (NO 3) 35H 2o), lanthanum trioxide (La 2o 3), ferric acetyl acetonade (C 15h 21feO 6) and butyl (tetra) titanate (Ti (C 4h 9o) 4) etc. be main raw material; Press Bi 4laTi 3feO 15taking the various raw materials that meet chemical dosage ratio is configured; In order to make up the volatilization of Bi element in follow-up heat treatment process, Bi (NO during weighing 3) 35H 2excessive 4～the 6mol% of O;
(b) whirl coating on sol evenning machine, directly at (111) of cleaning Pt/Ti/SiO 2on/Si (100) substrate, deposit Bi 4laTi 3feO 15wet film;
(c) Bi 4laTi 3feO 15wet film is heat-treated in rapid heat-treatment furnace;
(d) after rapid heat-treatment furnace furnace temperature naturally cools to room temperature, film is taken out, repeating step (b) and (c) 5～10 times, finally obtain Bi 4laTi 3feO 15many iron thin films.
2. a kind of Bi as claimed in claim 1 4laTi 3feO 15the chemical preparation process of many iron thin films, is characterized in that, the concrete steps in step (a) are:
(1) La: HNO in molar ratio 3measure dense HNO at=1: 20 3, then by La 2o 3join dense HNO 3, be placed in and on magnetic stirring apparatus, be stirred to solution clarification;
(2) Bi: CH in molar ratio 3cOOH=1: 20 measure CH 3cOOH, then by Bi (NO 3) 35H 2o joins CH 3in COOH, be placed in 55 ℃ of heated and stirred 1.5h in constant temperature blender with magnetic force, to remove Bi (NO 3) 35H 2crystal water in O adds wherein C after solution cool to room temperature 15h 21feO 6, relay and on magnetic stirring apparatus, be stirred to C 15h 21feO 6dissolve;
(3) solution (1) being obtained joins in the solution that (2) obtain and stirs 0.5h, then by stoichiometric ratio, drips Ti (C 4h 9o) 4and stir, after mixing, adding ethylene glycol monomethyl ether is 0.05mol/L～0.1mol/L by above-mentioned gained solution constant volume;
(4) in (3) gained solution, add the methyl ethyl diketone of its volume 1% and stir 4h, filtering and obtain uniform and stable sorrel precursor sol.
3. a kind of Bi as claimed in claim 1 4laTi 3feO 15the chemical preparation process of many iron thin films, is characterized in that, in step (b), the rotating speed of sol evenning machine is 3000～6000rpm, even glue 30s.
4. a kind of Bi as claimed in claim 1 4laTi 3feO 15the chemical preparation process of many iron thin films, is characterized in that, in step (c): the speed with 20 ℃/s is raised to 200 ℃ from room temperature, and insulation 300s; Speed with 25 ℃/s rises to 300 ℃～450 ℃ again, insulation 250s, and then the speed with 20 ℃/s～80 ℃/s rises to 700 ℃～800 ℃ fast, and insulation 300s, at mobile O 2annealing crystallization in atmosphere, O 2flow be 1～5L/min.
CN201410139124.8A 2014-04-09 2014-04-09 A kind of Bi 4laTi 3feO 15the chemical preparation process of many iron thin films Expired - Fee Related CN103951404B (en)

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CN104844183A (en) * 2015-03-27 2015-08-19 青岛大学 Chemical preparation method of Bi4YTi3FeO15 multiferroic film
CN104844161A (en) * 2015-03-27 2015-08-19 青岛大学 Method for improving multiferroic performance of Y2NiMnO6 ceramic
CN104941539A (en) * 2015-06-12 2015-09-30 南方科技大学 Preparation method for perovskite type composite oxide nanocrystalline colloid
CN108975397A (en) * 2018-09-03 2018-12-11 青岛大学 Bismuth titanates single crystal nanoplate of cadmium ferrite doping vario-property and preparation method thereof

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CN103646749A (en) * 2013-12-27 2014-03-19 青岛大学 Quasi-isotropy microwave ferromagnetic multilayer film and preparation method thereof

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN104844183A (en) * 2015-03-27 2015-08-19 青岛大学 Chemical preparation method of Bi4YTi3FeO15 multiferroic film
CN104844161A (en) * 2015-03-27 2015-08-19 青岛大学 Method for improving multiferroic performance of Y2NiMnO6 ceramic
CN104844161B (en) * 2015-03-27 2017-12-22 青岛大学 One kind improves Y2NiMnO6The method of ceramic multi-ferrum property
CN104941539A (en) * 2015-06-12 2015-09-30 南方科技大学 Preparation method for perovskite type composite oxide nanocrystalline colloid
CN104941539B (en) * 2015-06-12 2020-09-18 南方科技大学 Preparation method of perovskite type composite oxide nanocrystal adhesive
CN108975397A (en) * 2018-09-03 2018-12-11 青岛大学 Bismuth titanates single crystal nanoplate of cadmium ferrite doping vario-property and preparation method thereof
CN108975397B (en) * 2018-09-03 2021-01-22 青岛大学 Lanthanum ferrite doped and modified bismuth titanate monocrystal nanosheet and preparation method thereof

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