CN103044018A - Method for preparing Bi0.85Sm0.15Fe1-xCrxO3 ferroelectric film via sol-gel process - Google Patents
Method for preparing Bi0.85Sm0.15Fe1-xCrxO3 ferroelectric film via sol-gel process Download PDFInfo
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- CN103044018A CN103044018A CN2012104990270A CN201210499027A CN103044018A CN 103044018 A CN103044018 A CN 103044018A CN 2012104990270 A CN2012104990270 A CN 2012104990270A CN 201210499027 A CN201210499027 A CN 201210499027A CN 103044018 A CN103044018 A CN 103044018A
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Abstract
The invention discloses a method for preparing a Bi0.85Sm0.15Fe1-xCrxO3 ferroelectric film via a sol-gel process. The method is carried out by the following steps of: washing an FTO (Fluorinedoped Tin Oxide) substrate and subsequently irradiating via ultraviolet light; using bismuth nitrate, ferric nitrate, samarium nitrate and chromic nitrate as raw materials (the bismuth nitrate excesses by 5%), dissolving the above raw materials in mixed ethylene glycol monomethyl ether and acetic anhydride according to a mole ratio of 0.90: (1-x):0.15:x (x is 0.00, 0.01, 0.02 or 0.03), then adding ethanol amine to adjust a viscosity and obtain a stable BiFeO3 (bismuth ferrite) precursor solution with a metal ion concentration of 0.003-0.3mol/L; and homogenizing and subsequently obtaining a dry film, then using a layer-by-layer annealing process to obtain a crystal-state Bi0.85Sm0.15Fe1-xCrxO3 ferroelectric film. The method disclosed by the invention has the advantages of simple device requirement, easy achievement of experiment condition, good uniformity of the prepared films and easy control of the doping amount, so that the ferroelectric performance of the film is greatly enhanced.
Description
Technical field
The invention belongs to field of functional materials, relate at the FTO/glass of functionalization substrate surface and prepare Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc.
Background technology
In recent years, BiFeO
3As a kind of novel ferromagnetic electric material, have ferroelectricity and antiferromagnetism, and follow weak ferromegnetism to cause the great interest of people.BiFeO
3Having the simple perovskite structure of tripartite distortion, have simultaneously ferroelectric order (TC=810 ℃) and G type antiferromagnetic order (TN=380 ℃) under the room temperature, is one of a few single phase multi-iron material.BiFeO
3The magnetoelectricity coupling is in aspect widespread uses such as information storage, spin electric device, information storage, image demonstration, pyroelectric effect, uncooled infrared focal plane array.Yet, pure phase BiFeO
3Exist the problem of large leakage conductance, limited its practical application thereby cause him can't obtain saturated ferroelectric hysteresis loop.
Summary of the invention
The object of the present invention is to provide a kind of sol-gel method to prepare Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc, this kind method reduces its leakage current, improves remnant polarization.
To achieve these goals, the present invention adopts following technical scheme:
A kind of sol-gel method prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc may further comprise the steps:
Step 1: the FTO/glass substrate surface is cleaned up;
Step 2: the FTO/glass substrate is put into oven for drying, take out and leave standstill to room temperature;
Step 3: place ultraviolet radiation instrument to shine the FTO/glass substrate, make substrate surface reach the atomic cleanliness degree;
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O in molar ratio 0.90: 1-x: 0.15: x is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then adds thanomin in the mixed solution and carries out viscosity and regulate, and obtaining concentration of metal ions after the magnetic agitation is the stable Bi of 0.003～0.3mol/L
0.85Sm
0.15Fe
1-xCr
xO
3Precursor liquid, x=0～0.03 wherein, the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1;
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15Fe
1-xCr
xO
3Precursor liquid prepares film, behind the even cementing bundle, toasts to get dry film, and then adopts layer by layer annealing to obtain the BiFeO that crystalline state Sm and Cr mix altogether
3Film.
The present invention further improves and is: adopt ultrasonic cleaning in washing composition, acetone, the ethanol in the step 1, with a large amount of distilled water flushing substrates, dry up with nitrogen at last behind each ultrasonic cleaning 10min.
The present invention further improves and is: the baking oven storing temperature is 70 ℃ in the step 2, and the time is 5min.
The present invention further improves and is: irradiation time is 40min in the step 3 medium ultraviolet rayed instrument.
The present invention further improves and is: the time of magnetic agitation is 3h in the step 4
The present invention further improves and is: even glue speed is 3500～4500r/min in the step 5, and the even glue time is 15s.
The present invention further improves and is: the dry film temperature is 220 ℃ in the step 5, and the time is 5min.
The present invention further improves and is: in the step 5 layer by layer the temperature of anneal be 550 ℃, the time is 10min.
The present invention further improves and is: x=0.01-0.03 or x=0.02-0.03.
The present invention further improves and is: x=0.02.
The present invention further improves and is: spin coating prepares film in the step 5, toasts to get dry film, carries out anneal, and the step of the so layer by layer annealing of repeated using is until obtain expecting the film of thickness again.
With respect to prior art, the present invention has the following advantages:
1. the inventive method selects lanthanon Sm to carry out the doping of A position, selects Cr to carry out the B position and mixes, because Sm
3+Radius is less than Bi
3+, Cr
3+Radius is less than Fe
3+, after the doping, admittedly be melting into into lattice, can make the originally approximate bismuth ferrite crystal lattices distortion that is perovskite structure, the structural aberration aggravation, the solarization that goes of Sm is opened donor-acceptor defective pair simultaneously, the rollover number of electricdomain in the film is increased, thereby improve the ferroelectricity of film.
2. at present for the preparation of BiFeO
3The method of film has a lot, such as 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 is because equipment is simple, reaction is easily carried out, temperature of reaction is lower, easy to operate, suit to prepare film on large surface and surface in irregular shape, easily realize the Uniform Doped on the molecular level, and the accurate advantage such as controlled and be widely used for preparing ferroelectric material of chemical composition.
3. adopt sol-gel method to prepare BiFeO among the present invention
3Film, by Sm, Cr codoped, the BiFeO that mixes altogether at FTO substrate preparation Sm and Cr
3Film, this method can be prepared a kind of Bi
0.85Sm
0.15Fe
0.98Cr
0.02O
3Film, in the 1kHz frequency, the saturated polarization under the 1545kV/cm test electric field is 110.90 μ C/cm
2, remnant polarization is 95.61 μ C/cm
2, coercive field is 476.97kV/cm.
4. present device requires simply, and experiment condition easily reaches, and the uniformity of film of preparation is better, and doping is easily controlled, and can increase substantially by doping the ferroelectric properties of film.
Description of drawings
Fig. 1 is the Bi that the present invention prepares
0.85Sm
0.15Fe
0.98Cr
0.02O
3The XRD figure of film;
Fig. 2 is the Bi that the present invention prepares
0.85Sm
0.15Fe
0.98Cr
0.02O
3The SEM figure of film;
Fig. 3 is the Bi that the present invention prepares
0.85Sm
0.15Fe
0.98Cr
0.02O
3The ferroelectric hysteresis loop figure of film.
Embodiment
Embodiment 1
Step 1: selecting the FTO/glass substrate is substrate, and the FTO substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively, with a large amount of distilled water flushing substrates, dries up with nitrogen at last behind each ultrasonic cleaning 10min.
Step 2: the FTO/glass substrate is put into 60 ℃ of baking oven baking 5min, take out and leave standstill to room temperature.
Step 3: place ultraviolet radiation instrument to shine 40min the FTO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O 0.90: 1.00: 0.15 in molar ratio: 0.00 is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then adds thanomin in the mixed solution and carries out viscosity and regulate, and obtaining concentration of metal ions behind the magnetic agitation 3h is the stable Bi of 0.003mol/L
0.85Sm
0.15FeO
3Precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15FeO
3Precursor liquid prepares film, and even glue speed is the even glue 15s of 3500r/min, and behind the even cementing bundle, 220 ℃ of baking 5min get dry film, and then 550 ℃ of layer by layer anneal that are incubated 10min, obtain the Bi of crystalline state doping Sm
0.85Sm
0.15FeO
3Film.
Step 6: at crystalline state Bi
0.85Sm
0.15FeO
3The film surface ion sputtering prepares 0.502mm
2The Au electrode, then 300 ℃ the insulation 20min carry out the electrode anneal.
Adopt XRD determining Bi
0.85Sm
0.15FeO
3The phase of film forms structure, measures Bi with FE-SEM
0.85Sm
0.15FeO
3The microscopic appearance of film.With the ferroelectric test system and test Bi of TF2000
0.85Sm
0.15FeO
3The ferroelectric properties of film records under the test electric field of 1kHz frequency, 1181.8kV/cm, and its saturated polarization is 54.33 μ C/cm
2, remnant polarization is 43.17 μ C/cm
2, coercive field is 456.80kV/cm.
Embodiment 2
Step 1: selecting the FTO/glass substrate is substrate, and the FTO substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively, with a large amount of distilled water flushing substrates, dries up with nitrogen at last behind each ultrasonic cleaning 10min.
Step 2: the FTO/glass substrate is put into 60 ℃ of baking oven baking 5min, take out and leave standstill to room temperature.
Step 3: place ultraviolet radiation instrument to shine 40min the FTO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O 0.90: 0.99: 0.15 in molar ratio: 0.01 is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then adds thanomin in the mixed solution and carries out the viscosity adjusting, and obtaining concentration of metal ions behind the magnetic agitation 3h is the stable Bi of 0.3mol/L
0.85Sm
0.15Fe
0.99Cr
0.01O
3Precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15Fe
0.99Cr
0.01O
3Precursor liquid prepares film, and even glue speed is the even glue 15s of 4500r/min, behind the even cementing bundle, gets dry film at 220 ℃ of baking 5min, and then 550 ℃ of layer by layer anneal that are incubated 10min, obtains the Bi that crystalline state Sm and Cr mix altogether
0.85Sm
0.15Fe
0.99Cr
0.01O
3Film.
Step 6: at crystalline state Bi
0.85Sm
0.15Fe
0.99Cr
0.01O
3The film surface ion sputtering prepares 0.502mm
2The Au electrode, then 300 ℃ the insulation 20min carry out the electrode anneal.
Adopt XRD determining BiFeO
3The phase of film forms structure, measures Bi with FE-SEM
0.85Sm
0.15Fe
0.99Cr
0.01O
3The microscopic appearance of film is with the ferroelectric test system and test Bi of TF2000
0.85Sm
0.15Fe
0.99Cr
0.01O
3The ferroelectric properties of film records under the test electric field of 1kHz frequency, 1545kV/cm, and its saturated polarization is 93.89 μ C/cm
2, remnant polarization is 83.28 μ C/cm
2, coercive field is 500.06kV/cm.
Embodiment 3
Step 1: selecting the FTO/glass substrate is substrate, with the FTO substrate of well cutting place successively washing composition,
Ultrasonic cleaning in acetone, the ethanol with a large amount of distilled water flushing substrates, dries up with nitrogen behind each ultrasonic cleaning 10min at last.
Step 2: the FTO/glass substrate is put into 60 ℃ of baking oven baking 5min, take out and leave standstill to room temperature.
Step 3: place ultraviolet radiation instrument to shine 40min the FTO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O 0.90: 0.98: 0.15 in molar ratio: 0.02 is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then adds thanomin in the mixed solution and carries out viscosity and regulate, and obtaining concentration of metal ions behind the magnetic agitation 3h is the stable Bi of 0.01mol/L
0.85Sm
0.15Fe
0.98Cr
0.02O
3Precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15Fe
0.98Cr
0.02O
3Precursor liquid prepares film, and even glue speed is the even glue 15s of 3800r/min, behind the even cementing bundle, gets dry film at 220 ℃ of baking 5min, and then 550 ℃ of layer by layer anneal that are incubated 10min, obtains the Bi that crystalline state Sm and Cr mix altogether
0.85Sm
0.15Fe
0.98Cr
0.02O
3Film.
Step 6: at crystalline state Bi
0.85Sm
0.15Fe
0.98Cr
0.02O
3The film surface ion sputtering prepares 0.502mm
2The Au electrode, then 300 ℃ the insulation 20min carry out the electrode anneal.
Adopt XRD determining Bi
0.85Sm
0.15Fe
0.98Cr
0.02O
3The phase of film forms structure, measures Bi with FE-SEM
0.85Sm
0.15Fe
0.98Cr
0.02O
3The microscopic appearance of film.With the ferroelectric test system and test Bi of TF2000
0.85Sm
0.15Fe
0.98Cr
0.02O
3The ferroelectric properties of film records under the test electric field of 1kHz frequency, 1545kV/cm, and its saturated polarization is 110.90 μ C/cm
2, remnant polarization is 95.61 μ C/cm
2, coercive field is 476.97kV/cm.
Embodiment 4
Step 1: selecting the FTO/glass substrate is substrate, and the FTO substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively, with a large amount of distilled water flushing substrates, dries up with nitrogen at last behind each ultrasonic cleaning 10min.
Step 2: the FTO/glass substrate is put into 70 ℃ of baking oven baking 5min, take out and leave standstill to room temperature.
Step 3: place ultraviolet radiation instrument to shine 40min the FTO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O 0.90: 0.97: 0.15 in molar ratio: 0.03 is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then carries out viscosity with thanomin and regulates, and obtaining concentration of metal ions behind the magnetic agitation 3h is the stable Bi of 0.08mol/L
0.85Sm
0.15Fe
0.97Cr
0.03O
3Precursor liquid, wherein the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1.
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15Fe
0.97Cr
0.03O
3Precursor liquid prepares film, and even glue speed is the even glue 15s of 4000r/min, behind the even cementing bundle, gets dry film at 220 ℃ of baking 5min, and then 550 ℃ of layer by layer anneal that are incubated 10min, obtains the Bi that crystalline state Sm and Cr mix altogether
0.85Sm
0.15Fe
0.97Cr
0.03O
3Film.
Step 6: at crystalline state Bi
0.85Sm
0.15Fe
0.97Cr
0.03O
3The film surface ion sputtering prepares 0.502mm
2The Au electrode, then 300 ℃ the insulation 20min carry out the electrode anneal.
Adopt XRD determining Bi
0.85Sm
0.15Fe
0.97Cr
0.03O
3The phase of film forms structure, measures Bi with FE-SEM
0.85Sm
0.15Fe
0.97Cr
0.03O
3The microscopic appearance of film.With the ferroelectric test system and test Bi of TF2000
0.85Sm
0.15Fe
0.97Cr
0.03O
3The ferroelectric properties of film records under the test electric field of 1kHz frequency, 1545kV/cm, and its saturated polarization is 84.04 μ C/cm
2, remnant polarization is 66.62 μ C/cm
2, coercive field is 523.16kV/cm.
With XRD test b i
0.85Sm
0.15Fe
1-xCr
xO
3The phase of film forms structure, FE-SEM test b i
0.85Sm
0.15Fe
1-xCr
xO
3The pattern of film surface is with the ferroelectric test system and test Bi of TF2000
0.85Sm
0.15Fe
1-xCr
xO
3The ferroelectric properties of film carries out above test to embodiment 3, result such as Fig. 1, Fig. 2 and shown in Figure 3.Fig. 1 and PDF20-0169 standard card coincide, therefrom as can be known, and the Bi of sol-gel method preparation
0.85Sm
0.15Fe
0.98Cr
0.02O
3Film has distorted perovskite structure, does not have the appearance of impurity.Fig. 3 shows Bi
0.85Sm
0.15Fe
0.98Cr
0.02O
3Film is in the 1kHz frequency, and the saturated polarization under the 1545kV/cm test electric field is 110.90 μ C/cm
2, remnant polarization is 95.61 μ C/cm
2, coercive field is 476.97kV/cm.
The invention provides a kind of Bi for preparing Sm and Cr codoped at the FTO/glass substrate surface
0.85Sm
0.15Fe
1-xCr
xO
3The method of film; 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), samaric nitrate (Sm (NO
3)
36H
2O) and chromium nitrate (Cr (NO
3)
39H
2O) be raw material (Bismuth trinitrate excessive 5%), in molar ratio 0.90: 1-x: 0.15: x(x=0.00,0.01,0.02,0.03) be dissolved in the ethylene glycol monomethyl ether and acetic anhydride of mixing (volume ratio is 14: 5), thanomin carries out viscosity and regulates (volume ratio of acetic anhydride and thanomin is 5: 1), fully magnetic agitation is to fully dissolving, and obtaining concentration of metal ions is 0.003～0.3mol/LBi
0.85Sm
0.15Fe
1-xCr
xO
3Precursor solution.At the even glue 15s of 3500～4500r/min, then get dry film at 220 ℃ of baking 5min, 550 ℃ of layer by layer anneal that are incubated 10min, obtain crystalline state Bi again
0.85Sm
0.15Fe
1-xCr
xO
3Film.Present device requires simple, and experiment condition easily reaches, and the uniformity of film of preparation is better, and doping is easily controlled, and by the suitable selection of doping, increases substantially the ferroelectric properties of film.
Above said content is in conjunction with concrete preferred implementation further description made for the present invention, it or not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (10)
1. a sol-gel method prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, may further comprise the steps:
Step 1: the FTO/glass substrate surface is cleaned up;
Step 2: the FTO/glass substrate is put into oven for drying, take out and leave standstill to room temperature;
Step 3: place ultraviolet radiation instrument to shine the FTO/glass substrate, make substrate surface reach the atomic cleanliness degree;
Step 4: with Bi (NO
3)
35H
2O, Fe (NO
3)
39H
2O, Sm (NO
3)
36H
2O and Cr (NO
3)
39H
2O in molar ratio 0.90: 1-x: 0.15: x is dissolved in the mixed solution of ethylene glycol monomethyl ether and acetic anhydride, then adds thanomin in the mixed solution and carries out viscosity and regulate, and obtaining concentration of metal ions after the magnetic agitation is the stable Bi of 0.003～0.3mol/L
0.85Sm
0.15Fe
1-xCr
xO
3Precursor liquid, x=0～0.03 wherein, the volume ratio of ethylene glycol monomethyl ether, acetic anhydride and thanomin is 14: 5: 1;
Step 5: adopt spin-coating method spin coating Bi on the FTO/glass substrate
0.85Sm
0.15Fe
1-xCr
xO
3Precursor liquid prepares film, behind the even cementing bundle, toasts to get dry film, and then adopts layer by layer annealing to obtain the BiFeO that crystalline state Sm and Cr mix altogether
3Film.
2. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, adopts ultrasonic cleaning in washing composition, acetone, the ethanol in the step 1, with a large amount of distilled water flushing substrates, dries up with nitrogen at last behind each ultrasonic cleaning 10min.
3. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, the baking oven storing temperature is 70 ℃ in the step 2, and the time is 5min.
4. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, irradiation time is 40min in the step 3 medium ultraviolet rayed instrument.
5. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, the time of magnetic agitation is 3h in the step 4.
6. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, even glue speed is 3500～4500r/min in the step 5, and the even glue time is 15s.
7. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, the dry film temperature is 220 ℃ in the step 5, and the time is 5min.
8. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, in the step 5 layer by layer the temperature of anneal be 550 ℃, the time is 10min.
9. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, x=0.01-0.03 or x=0.02-0.03.
10. a kind of sol-gel method according to claim 1 prepares Bi
0.85Sm
0.15Fe
1-xCr
xO
3The method of ferroelectric membranc is characterized in that, spin coating prepares film in the step 5, toasts to get dry film, carries out anneal, and the step of the so layer by layer annealing of repeated using is until obtain expecting the film of thickness again.
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