CN102633443A - Method for preparing Tb-doped BiFeO3 ferroelectric film on surface of conductive glass substrate - Google Patents
Method for preparing Tb-doped BiFeO3 ferroelectric film on surface of conductive glass substrate Download PDFInfo
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- CN102633443A CN102633443A CN2012100459615A CN201210045961A CN102633443A CN 102633443 A CN102633443 A CN 102633443A CN 2012100459615 A CN2012100459615 A CN 2012100459615A CN 201210045961 A CN201210045961 A CN 201210045961A CN 102633443 A CN102633443 A CN 102633443A
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Abstract
The invention discloses a method for preparing a Tb-doped BiFeO3 ferroelectric film on the surface of a conductive glass substrate. The method comprises the following steps of: 1, cleaning the substrate; 2, irradiating the substrate by using ultraviolet so that the surface of the substrate reaches atomic cleanliness; 3, dissolving Fe(NO3)3.9H2O, Bi(NO3)3.5H2O and Tb(NO3)3.5H2O in a molar ratio of 1: (1-x): x (x=0-0.15) into a mixed solution of ethylene glycol monomethyl ether and glacial acetic acid; and 4, preparing the film by adopting a spin coating method, then pre-annealing, annealing, crystallizing, and thus obtaining the crystalline Tb-doped BiFeO3 ferroelectric film. By the method, the residual polarization value of the film can be greatly improved; and after Tb is doped, the residual polarization value can be improved to 55mu C/cm<2>.
Description
Technical field
The invention belongs to field of functional materials, relate to adulterated BiFeO at the conducting glass substrate surface preparation Tb of functionalization
3The method of film.
Background technology
In recent years, BiFeO
3As a kind of novel ferromagnetic electric material, caused the great interest of people.BiFeO
3Simple calcium titanium ore structure with tripartite distortion has ferroelectric (T in order simultaneously under the room temperature
C=810 ℃) and G type antiferromagnetic order (T
N=380 ℃), be one of a few single phase multi-iron material.BiFeO
3The magnetoelectricity coupling is aspect information storage, spin electric device, and all there is extremely important application prospect Magnetic Sensor and electric capacity-aspects such as inductor integrated device.
The problem that always limits the application of ferrous acid bismuth material is: the specific inductivity of ferrous acid bismuth material is lower, is difficult to observe big residual polarization value under the room temperature, especially polycrystalline ferrous acid bismuth material; The leakage conductance of ferrous acid bismuth material is bigger, is difficult to obtain saturated ferroelectric hysteresis loop.
Summary of the invention
The object of the present invention is to provide a kind of at conducting glass substrate surface preparation Tb doping BiFeO
3The method of ferroelectric membranc, this method obtains BiFeO
3Film has big residual polarization value, saturated ferroelectric hysteresis loop.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of at conducting glass substrate surface preparation Tb doping BiFeO
3The method of ferroelectric membranc may further comprise the steps:
Step 1: FTO conducting glass substrate surface cleaning is clean;
Step 2: place ultraviolet radiation instrument to shine the FTO conducting glass substrate, make substrate surface reach the atomic cleanliness degree;
Step 3: with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and Tb (NO
3)
35H
2O in molar ratio 1: (1-x): x is dissolved in the mixed solution of EGME and Glacial acetic acid min. 99.5, obtains stable BiFeO after stirring
3Presoma; The concentration of metals ion is 0.3～0.9mol/L; 0＜x≤0.15 wherein, the volume ratio 3: 1～2: 1 of EGME and Glacial acetic acid min. 99.5 in the mixed solution;
Step 4: adopt spin-coating method at FTO conductive glass substrate surface spin coating BiFeO
3Presoma prepares film, and behind the even glued bundle, preannealing, annealing crystallization obtain crystalline state Tb doping BiFeO then
3Ferroelectric membranc.
The present invention further improves and is: adopt washing composition, acetone, ethanol to carry out ultrasonic cleaning in the step 1, use distilled water flushing after each ultrasonic cleaning, dry up with nitrogen at last.
The present invention further improves and is: in the step 3 in the gained precursor liquid concentration of metals ion be 0.3～0.9mol/L.
The present invention further improves and is: even glue speed is 3000～6000r/min in the step 4, and the even glue time is 15s.
The present invention further improves and is: the temperature of preannealing is 350 ℃ in the step 4, and the time is 5min; The temperature of annealing crystallization is 500 ~ 600 ℃, and the time is 20～30min.
The present invention further improves and is: the step that repeats spin coating system film, preannealing, annealing crystallization in the step 4 is up to the Tb doping BiFeO that obtains expecting thickness
3Ferroelectric membranc.
The present invention further improves and is: place ultraviolet radiation instrument to shine 40min the FTO conducting glass substrate in the step 2, make substrate surface reach the atomic cleanliness degree.
The present invention further improves and is: precursor liquid magnetic agitation 0.5h obtains stable BiFeO in the step 3
3Presoma.
The present invention further improves and is: 0.05≤x≤0.15.
With respect to prior art, the present invention has the following advantages: the present invention utilizes Prepared by Sol Gel Method to mix the bismuth ferrite thin film of Tb; The invention has the beneficial effects as follows through simple technology, require lower experiment condition, obtain having the BiFeO of big residual polarization value, saturated ferroelectric hysteresis loop
3Film, residual polarization value can be promoted to 55 μ C/cm
2About and the variation through the controlled doping amount, can obtain the BiFeO of different performance
3Film.
The present invention is through the doped and substituted of Tb element for A position Bi element; Can make the lattice distortion that is distorted, make the aggravation of ferrous acid bismuth structural asymmetry, with obtaining bigger residual polarization value; And better Tb replaces Bi with chemicalstability, helps suppressing the volatilization of Bi.
Be used to prepare BiFeO at present
3The method of film has a lot, like chemical Vapor deposition process (CVD), magnetron sputtering method (rf magnetron sputtering), deposition of metal organic method (MOD), metal-organic chemical vapor deposition equipment method (MOCVD), liquid phase deposition (LPD), molecular beam epitaxy (MBE), pulsed laser deposition (PLD), sol-gel method (Sol-Gel) etc.Compare additive method, the Sol-gel method suits on big surface and surface in irregular shape, to prepare film owing to do not need expensive vacuum apparatus, and advantage such as chemical composition is accurately controlled and be widely used for preparing ferroelectric material.
The present invention utilizes sol-gel method on the FTO substrate, to prepare Tb doping BiFeO
3Film, this method can increase substantially the residual polarization value of film, polycrystalline BiFeO
3Film is at room temperature lower, about 0.4 μ C/cm
2, and after the Tb doping, the residual polarization value can be promoted to 55 μ C/cm
2About.
Description of drawings
Fig. 1 is the BiFeO that the present invention prepares
3And Bi
0.9Tb
0.1FeO
3The XRD figure of film;
Fig. 2 is the BiFeO that the present invention prepares
3And Bi
0.9Tb
0.1FeO
3The ferroelectric hysteresis loop figure of film.
Embodiment
Embodiment 1
Step 1: selecting FTO conductive glass substrate for use is substrate, and the FTO conductive glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning 10min respectively, removes the impurity such as grease of FTO conductive glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 40min the FTO conductive glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ", form wetting ability hydroxyl preferably, improve the wetting ability of substrate;
Step 3: with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and Tb (NO
3)
35H
2O is dissolved in the mixed solution of EGME and Glacial acetic acid min. 99.5 by 1: 0.95: 0.05 mol ratio, obtains the precursor liquid that concentration of metal ions is 0.3～0.9mol/L, and magnetic agitation 0.5h obtains stable BiFeO
3Presoma, wherein the volume ratio of EGME and Glacial acetic acid min. 99.5 is 3: 1.
Step 4: adopt spin-coating method to prepare film at FTO conductive glass substrate surface; Even glue speed is 3000～6000r/min; The even glue time is 15s; Behind the even glued bundle, under 350 ℃ high temperature, carry out pre-treatment 5min then so that organic decomposition, then at 500 ℃～600 ℃ annealing 20～30min.Repeat to obtain several times the adulterated BiFeO of certain thickness Tb
3Film.
Step 5: prepare 0.502mm in the film surface ion sputtering
2The Au electrode.
Step 1: selecting FTO conductive glass substrate for use is substrate, and the FTO conductive glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning 10min respectively, removes the impurity such as grease of FTO conductive glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 40min the FTO conductive glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ", form wetting ability hydroxyl preferably, improve the wetting ability of substrate;
Step 3: with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and Tb (NO
3)
35H
2O is dissolved in the mixed solution of EGME and Glacial acetic acid min. 99.5 by 1: 0.90: 0.10 mol ratio, obtains the precursor liquid that concentration of metal ions is 0.3～0.9mol/L, and magnetic agitation 0.5h obtains stable BiFeO
3Presoma, wherein the volume ratio of EGME and Glacial acetic acid min. 99.5 is 2: 1.
Step 4: adopt spin-coating method to prepare film at FTO conductive glass substrate surface; Even glue speed is 3000～6000r/min; The even glue time is 15s; Behind the even glued bundle, under 350 ℃ high temperature, carry out pre-treatment 5min then so that organic decomposition, then at 500 ℃～600 ℃ annealing 20～30min.Repeat to obtain several times certain thickness Tb doping BiFeO
3Film.
Step 5: prepare 0.502mm in the film surface ion sputtering
2The Au electrode.
Embodiment 3
Step 1: selecting FTO conductive glass substrate for use is substrate, and the FTO conductive glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning 10min respectively, removes the impurity such as grease of FTO conductive glass substrate surface.With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 40min the FTO conductive glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ", form wetting ability hydroxyl preferably, improve the wetting ability of substrate;
Step 3: with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and Tb (NO
3)
35H
2O is dissolved in the mixed solution of EGME and Glacial acetic acid min. 99.5 by 1: 0.85: 0.15 mol ratio, obtains the precursor liquid that concentration of metal ions is 0.3～0.9mol/L, and magnetic agitation 0.5h obtains stable BiFeO
3Presoma, wherein the volume ratio of EGME and Glacial acetic acid min. 99.5 is 3: 1.
Step 4: adopt spin-coating method to prepare film at FTO conductive glass substrate surface; Even glue speed is 3000～6000r/min; The even glue time is 15s; Behind the even glued bundle, under 350 ℃ high temperature, carry out pre-treatment 5min then so that organic decomposition, then at 500 ℃～600 ℃ annealing 20～30min.Repeat to obtain several times certain thickness Tb doping BiFeO
3Film.
Step 5: prepare 0.502mm in the film surface ion sputtering
2The Au electrode.
From Fig. 1, can know the Bi that embodiment 1 is prepared
0.9Tb
0.1FeO
3Film has the distortion calcium titanium ore structure, does not have the appearance of impurity.We can find out Bi from Fig. 2
0.9Tb
0.1FeO
3Film can obtain higher residual polarization and be worth 55 μ C/cm
2
Because the ionic radius and the Bi ionic radius of lanthanon are more or less the same, valence state is also identical, but because there is certain gap in electronegativity, so can form discontinuity sosoloid.After Tb mixed, Gu the molten lattice that gets into can make the ferrous acid bismuth that is calcium titanium ore structure originally basically be distorted, structural aberration aggravated, thereby improves the ferroelectricity of film, and the residual polarization value can be promoted to 55 μ C/cm
2About, and, help suppressing the volatilization of Bi with the better Tb replacement of chemicalstability Bi.
The present invention is a kind of at conducting glass substrate surface preparation Tb doping BiFeO
3The method of ferroelectric membranc; After the cleaning of FTO substrate, uv irradiating 40min is with Bismuth trinitrate (Bi (NO
3)
35H
2O), iron nitrate (Fe (NO
3)
39H
2O) and Terbium trinitrate (Tb (NO
3)
35H
2O) be raw material (five water Bismuth trinitrates excessive 5%); By 1-x: 1: x (x=0～0.15) mol ratio is dissolved in certainty ratio blended EGME and the Glacial acetic acid min. 99.5; Fully stir dissolving fully; Obtain precursor liquid and magnetic agitation 0.5h that concentration of metal ions is 0.3～0.9mol/L, obtain stable BiFeO
3Presoma.At the even glue 15s of 3000～6000r/min, behind the even glued bundle, then at 350 ℃ preannealing 5min so that organic decomposition.500 ℃～600 ℃ annealing crystallization, repeat technology then several times, obtain certain thickness Tb doping BiFeO
3Ferroelectric membranc.Present device requires simple, and experiment condition reaches easily, and the uniformity of film of preparation is better, and doping is controlled easily, and can increase substantially the ferroelectric properties of film through doping.
The above is merely one embodiment of the present invention; It or not whole or unique embodiment; The conversion of any equivalence that those of ordinary skills take technical scheme of the present invention through reading specification sheets of the present invention is claim of the present invention and contains.
Claims (8)
1. one kind at conducting glass substrate surface preparation Tb doping BiFeO
3The method of ferroelectric membranc is characterized in that, may further comprise the steps:
Step 1: FTO conducting glass substrate surface cleaning is clean;
Step 2: place ultraviolet radiation instrument to shine the FTO conducting glass substrate, make substrate surface reach the atomic cleanliness degree;
Step 3: with Fe (NO
3)
39H
2O, Bi (NO
3)
35H
2O and Tb (NO
3)
35H
2O in molar ratio 1: (1-x): x is dissolved in the mixed solution of EGME and Glacial acetic acid min. 99.5, obtains stable BiFeO after stirring
3Presoma; The concentration of metals ion is 0.3～0.9mol/L; 0＜x≤0.15 wherein, the volume ratio 3: 1～2: 1 of EGME and Glacial acetic acid min. 99.5 in the mixed solution;
Step 4: adopt spin-coating method at FTO conductive glass substrate surface spin coating BiFeO
3Precursor liquid prepares film, and behind the even glued bundle, preannealing, annealing crystallization obtain crystalline state Tb doping BiFeO then
3Ferroelectric membranc.
2. method according to claim 1 is characterized in that, adopts washing composition, acetone, ethanol to carry out ultrasonic cleaning in the step 1, uses distilled water flushing after each ultrasonic cleaning, dries up with nitrogen at last.
3. method according to claim 1 is characterized in that, in the step 3 in the gained precursor liquid concentration of metals ion be 0.3～0.9mol/L.
4. method according to claim 1 is characterized in that, even glue speed is 3000～6000r/min in the step 4, and the even glue time is 15s.
5. method according to claim 1 is characterized in that, the temperature of preannealing is 350 ℃ in the step 4, and the time is 5min; The temperature of annealing crystallization is 500 ~ 600 ℃, and the time is 20～30min.
6. method according to claim 1 is characterized in that, the step that repeats spin coating system film, preannealing, annealing crystallization in the step 4 is up to the Tb doping BiFeO that obtains expecting thickness
3Ferroelectric membranc.
7. method according to claim 1 is characterized in that, places ultraviolet radiation instrument to shine 40min the FTO conducting glass substrate in the step 2, makes substrate surface reach the atomic cleanliness degree.
8. method according to claim 1 is characterized in that, 0.05≤x≤0.15.
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Cited By (12)
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|---|---|---|---|---|
| CN103058646A (en) * | 2012-11-07 | 2013-04-24 | 陕西科技大学 | Method for preparing Tb/Cr-codoped high-remanent-polarization BiFeO3 film by sol-gel process |
| CN103145192A (en) * | 2013-03-28 | 2013-06-12 | 新疆大学 | Method for preparing manganese, nickel codoped bismuth ferrite film by sol-gel process |
| CN103601248A (en) * | 2013-11-04 | 2014-02-26 | 陕西科技大学 | Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof |
| CN103601250A (en) * | 2013-11-04 | 2014-02-26 | 陕西科技大学 | Layer-by-layer alternatively doped low-leakage-current BiFeO3 film and preparation method thereof |
| CN103613372A (en) * | 2013-11-04 | 2014-03-05 | 陕西科技大学 | Tb, Mn and Cu three-element codoped low leakage current BiFeO3 film and preparation method |
| CN103613144A (en) * | 2013-11-04 | 2014-03-05 | 陕西科技大学 | B-site Mn and Cu codoped high remanent polarization BiFeO3 film and preparation method |
| CN103626236A (en) * | 2013-11-04 | 2014-03-12 | 陕西科技大学 | B-site Mn and Ni co-doped high-remanent-polarization BiFeO3 film and preparation method thereof |
| CN103626237A (en) * | 2013-11-04 | 2014-03-12 | 陕西科技大学 | Tb, Cr and Mn ternary co-doped high-remanent-polarization BiFeO3 film and preparation method thereof |
| CN103708562A (en) * | 2013-12-20 | 2014-04-09 | 陕西科技大学 | Bi0.90Ho0.10Fe1-XMnXO3 ferroelectric film with high remanent polarization and preparation method thereof |
| CN103739019A (en) * | 2013-12-20 | 2014-04-23 | 陕西科技大学 | BiFe1-XMnXO3 ferroelectric film with high remnant polarization and preparation method thereof |
| CN103771528A (en) * | 2013-12-20 | 2014-05-07 | 陕西科技大学 | Bi[1-X]HoXFeO3 ferroelectric film with high dielectric constant and preparation method of film |
| CN110563048A (en) * | 2019-09-23 | 2019-12-13 | 济南大学 | Polymer-assisted epitaxial growth BiFeO3Method for producing multiferroic thin film |
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| CN103145192A (en) * | 2013-03-28 | 2013-06-12 | 新疆大学 | Method for preparing manganese, nickel codoped bismuth ferrite film by sol-gel process |
| CN103145192B (en) * | 2013-03-28 | 2016-04-27 | 新疆大学 | Sol-gel technology prepares the method for manganese, nickel co-doped bismuth ferrite thin film |
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| CN103613144A (en) * | 2013-11-04 | 2014-03-05 | 陕西科技大学 | B-site Mn and Cu codoped high remanent polarization BiFeO3 film and preparation method |
| CN103601248B (en) * | 2013-11-04 | 2015-06-24 | 陕西科技大学 | Tb, Mn and Ni ternary co-doped low leakage current BiFeO3 film and preparation method thereof |
| CN103708562B (en) * | 2013-12-20 | 2015-06-24 | 陕西科技大学 | Bi0.90Ho0.10Fe1-XMnXO3 ferroelectric film with high remanent polarization and preparation method thereof |
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| CN110563048A (en) * | 2019-09-23 | 2019-12-13 | 济南大学 | Polymer-assisted epitaxial growth BiFeO3Method for producing multiferroic thin film |
| CN110563048B (en) * | 2019-09-23 | 2022-02-01 | 济南大学 | Polymer-assisted epitaxial growth BiFeO3Method for producing multiferroic thin film |
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Application publication date: 20120815 |