CN102863209A - Preparation method for bismuth ferrite-lead titanate/FTO conducting glass-structure material - Google Patents
Preparation method for bismuth ferrite-lead titanate/FTO conducting glass-structure material Download PDFInfo
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- CN102863209A CN102863209A CN2012103494517A CN201210349451A CN102863209A CN 102863209 A CN102863209 A CN 102863209A CN 2012103494517 A CN2012103494517 A CN 2012103494517A CN 201210349451 A CN201210349451 A CN 201210349451A CN 102863209 A CN102863209 A CN 102863209A
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Abstract
The invention relates to a method for preparing a high-quality bismuth ferrite-lead titanate film on an FTO (Fluorinedoped Tin Oxide) conducting glass substrate, and belongs to the technical field of the preparation process of inorganic nonmetallic materials. According to the invention, FTO conducting glass is serves as a substrate, a bismuth ferrite-lead titanate (0.7BFO-0.3PT) film/FTO conducting glass-structure material with the functions of ferroelectric storage and photoelectric response for visible light is prepared by a sol-gel method, and electrical and optical performances of the bismuth ferrite-lead titanate film/FTO conducting glass-structure material are respectively characterized by preparing an electrode-on-Pt and an ITO (Indium Tin Oxide) transparent electrode.
Description
Technical field
What the present invention relates to is (to mix the SnO of fluorine at FTO
2) prepare high quality bismuth ferrite with good ferroelectric storage and visible light photoelectric response function-lead titanate film by sol-gel technology on the Conducting Glass, belong to ceramic fabricating technology field.
Background technology
Bismuth ferrite (BiFeO
3, BFO) be a kind of single-phase multi-ferroic material, namely integrate ferroelectric, ferromagnetic, ferroelasticity can.And has magnetoelectric effect.(674 ~ 441nm) are in the visible light wave range, can show in theory good visible light photoelectric response and the energy gap of BFO is about 1.84 ~ 2.81eV.Therefore BFO can be used for developing multifunctional light, the electron devices such as storer, sensor, detector of magnetic-electricity, light-electric multiple degree of freedom cross complaint, is on active service in technical fields such as space flight, automotive industry, biology, medical science, information.(ferroelectric transition temperature is 830 because the transformation temperature of BFO is higher than room temperature
oC, magnetic transition temperature is 370
oC), can utilize the visible light of sun power, and not leaded, so the suitable environmental protection of its Service Environment.
Yet because the Fe among the BFO
3+Ion is the easily impact of restricted standby environment and appraising at the current rate in the material preparation process, causes generating extra electronics and the reduction that causes the BFO material insulation property, affects the most at last performance of devices.Therefore except the preparation means and environment that promote BFO, also be a kind of desirable method with BFO and other perovskite material solid solutions to stablize its insulativity.The latter for the thin-film material in the microdevice, can greatly reduce the material preparation cost for Application and preparation.The BiFeO that wherein proposes the sixties in last century
3-PbTiO
3System solid solution has high-insulativity, and strong ferroelectricity can be used as the film candidate material of the miniature multi-function device of mentioning.When with PbTiO
3(PT) during content to 0.3, be that BFO content is 0.7, the 0.7BFO-0.3PT component film of this moment has ferroelectric, the dielectric properties of optimization, and the Tapes gap is 2.89eV, can utilize visible light, be applied to aspect the microoptoelectronic device very large development space is arranged.And the lead tolerance of 0.7BFO-0.3PT thin-film material is lower, belongs to mutually environment amenable material.
The exploitation of thin-film material on device application also need be selected suitable supporting substrate.0.7BFO-0.3PT film can be used for developing the optoelectronic function device that integrates ferroelectric storage, visible light photoelectric response aspect, therefore mixes the SnO of fluorine
2, namely the FTO conductive glass is well suited for as corresponding supporting substrate.
0.7BFO-0.3PT film of the present invention prepares gained with sol-gel spin-coating method.This method technique is simple, easily controls the stoichiometric ratio of film composition, easily forms large-area uniform films, is fit to the preparation multi-component film material.Film has conveniently, the cycle is short yet although sol-gel process prepares, be easy to the advantages such as control, for specific thin-film material, in the presoma layoutprocedure of colloidal sol, there is specific interpolation proportioning window, otherwise is difficult to prepare the thin-film material with estimated performance.
The present invention adopts FTO (to mix the SnO of fluorine
2) conductive glass is as substrate, prepares bismuth ferrite-lead titanate (0.7BFO-0.3PT) film of integrating ferroelectric storage and visible light photoelectric response function/FTO conductive glass structured material with sol-gel process.Prepared platinum Pt top electrode in the test of the present invention its electric property has been carried out testing research; In order to reduce as far as possible top electrode to the impact of its photoelectric response, the thin-film material for preparing has also been prepared ITO (mixed the In of Sn
2O
3) transparent upper electrode, to carry out the research of photoelectric response.
Summary of the invention
The objective of the invention is (to mix the SnO of fluorine at FTO
2) on the conductive glass, by in the sol gel process process to the adjustment of additive formula in the precursor sol liquid, in atmospheric environment, prepare good bismuth ferrite-lead titanate (0.7BFO-0.3PT) thin-film material with ferroelectric storage and visible light photoelectric response of crystallinity.
The present invention is a kind of bismuth ferrite-lead titanate with ferroelectric storage and visible light photoelectric response function/FTO glass structure material preparation method, it is characterized in that having following technological process and step:
A. the pre-treatment of FTO Conducting Glass:
Dab with acetone and to wash substrate surface, pass through again acetone, 3 sonic oscillations of dehydrated alcohol, at least 5 minutes at every turn, use at last washed with de-ionized water, dry for standby;
B. the preparation of bismuth ferrite-lead titanate (0.7BFO-0.3PT) colloidal sol:
(1) takes by weighing positive four butyl esters of a certain amount of metatitanic acid with analytical balance, add the proper amount of glycol methyl ether; Take by weighing a certain amount of plumbic acetate, 60
0The C oil bath stirs to clarify; Add afterwards a certain amount of mixed solution; Mixed solution consists of: water, and Glacial acetic acid and ethylene glycol monomethyl ether three are mixed by certain molar ratio 1:2:1; Configuration obtains the precursor solution of lead titanate;
(2) oil bath temperature is adjusted to 90
0C continues to stir precursor solution and takes off placement normal temperature after 2 hours; Add a certain amount of ethylene glycol monomethyl ether stirring at normal temperature dissolving under the room temperature; Then add the certain proportion methane amide, the add-on of methane amide is measured with the mol ratio 1:2 of itself and positive four butyl esters of metatitanic acid ~ 1:6; Take by weighing respectively a certain amount of five water Bismuth trinitrates and nine water iron nitrates according to the 0.7BFO-0.3PT ratio after stirring, successively add; Then stirring at normal temperature adds the certain proportion Glacial acetic acid with drop-burette at last to fully dissolving, stirs 24h, forms bismuth ferrite-lead titanate (0.7BFO-0.3PT) colloidal sol, leaves standstill behind the 12-48h stand-by;
C. apply bismuth ferrite-lead titanate (0.7BFO-0.3PT) film and anneal at the FTO conductive glass:
Use the desk-top sol evenning machine of SC-1B type with the precursor sol of preparation with 1000 rev/mins, 5 seconds; 3000 rev/mins, 25 seconds speed is spin-coated on the FTO Conducting Glass, and then on the BP-2B type drying glue platform 240
0Most volatile organic matter is removed in the C baking, follows in the quick photo-thermal stove of KG-2-ZE type 500
0Under the C pre-crystallized 5 minutes, obtain thin film.So repeat above-mentioned spin coating, crystallization processes 12 times, obtain certain thickness film, at last in retort furnace 600
0C annealing made its complete crystallization in 1 hour.
Finally obtain complete bismuth ferrite-lead titanate/FTO glass structure material.
Main thought of the present invention is when preparing the 0.7BFO-0.3PT thin-film material with sol-gel process, when precursor sol liquid configures, must obtain suitable additive formula window by the proportioning of adjusting the methane amide additive, just can prepare bismuth ferrite-lead titanate (0.7BFO-0.3PT) thin-film material that integrates ferroelectric storage and visible light photoelectric response function.
Description of drawings
Fig. 1 is the X-ray diffractogram of the 0.7BFO-0.3PT film sample that makes in the embodiment of the invention.
Fig. 2 is PUND pulse (just-on-negative-lower pulse wave) test pattern of the 0.7BFO-0.3PT film sample that makes in the embodiment of the invention.
Fig. 3 is the ferroelectric fatigue property test figure of the 0.7BFO-0.3PT film sample that makes in the embodiment of the invention.
Fig. 4 is the photoelectric response I-T figure of the 0.7BFO-0.3PT film sample that makes in the embodiment of the invention.
Fig. 5 is Pt/0.7BFO-0.3PT/FTO, the ITO/0.7BFO-0.3PT/FTO structural representation with electrode.
Embodiment
Below be process and the step of specific embodiments of the invention:
I. at first the FTO Conducting Glass is carried out pre-treatment: with acetone, alcohol respectively ultrasonic cleaning use again later on deionized water rinsing, dry up for subsequent use.
II. prepare the 0.7BiFeO of 0.1 mol/L
3-0.3PbTiO
3 Colloidal sol 30 ml:
1. claim positive four butyl esters of metatitanic acid 0.2073 gram with analytical balance, add ethylene glycol monomethyl ether 5 ml; Take by weighing plumbic acetate 0.2373 gram, 60
OCOil bath stirs to clarify; Add afterwards 0.1316ml mixed solution (mixed solution forms: water, Glacial acetic acid and ethylene glycol monomethyl ether three's mol ratio is about about 1:2:1), configure the precursor solution that obtains lead titanate;
2. regulate oil bath temperature to 90
0C continues to stir precursor solution and takes off placement normal temperature after 2 hours; Add the dissolving of 13.92ml ethylene glycol monomethyl ether stirring at normal temperature under the room temperature, then add methane amide (mol ratio of positive four butyl esters of methane amide and metatitanic acid is between 1:2 and the 1:6) 0.1614ml, rear 0.6894 gram five water Bismuth trinitrates and 0.5742 gram, the nine water iron nitrates of taking by weighing respectively stir, successively add, then stirring at normal temperature adds the 1.015ml Glacial acetic acid with drop-burette at last to fully dissolving, stirs 24h, obtain stable 0.7BFO-0.3PT precursor sol, leave standstill behind the 12-48h stand-by;
III. spin coating preparation and the anneal of 0.7BFO-0.3PT film on the FTO Conducting Glass:
Use the desk-top sol evenning machine of SC-1B type with the precursor sol of preparation with 1000 rev/mins, 5 seconds; 3000 rev/mins, 25 seconds speed is spin-coated on the FTO Conducting Glass, and then on the BP-2B type drying glue platform 240
0Most volatile organic matter is removed in the C baking, follows in the quick photo-thermal stove of KG-2-ZE type 500
0Under the C pre-crystallized 5 minutes, obtain thin film.So repeat above-mentioned spin coating, crystallization processes 12 times, obtain certain thickness film, at last in retort furnace 600
0C annealing made its complete crystallization in 1 hour.
Detection test to embodiment of the invention products therefrom
Test example one
Mask plate with the 0.4mm diameter covers above-mentioned 0.7BFO-0.3PT film surface, and sputtered platinum makes top electrode Pt electrode, last 300
oC annealing 30 minutes makes between electrode and film and forms good contacting, and finishes the making of electrode, the 0.7BFO-0.3PT/FTO structure is carried out the detection of ferroelectric memory property.
Test example two
Mask plate with the 0.4mm diameter covers above-mentioned 0.7BFO-0.3PT film surface, in 200
oSputtering ITO top electrode under the C working temperature is to carry out the detection of visible light photoelectric response to the 0.7BFO-0.3PT/FTO structure.
Detection and detected result to embodiment gained sample
1, embodiment gained sample is carried out the XRD detection, listed in the Fig. 1 in the accompanying drawing.
2, to test example one gained sample carried out PUND pulses (just-on-negative-lower pulse wave) test, ferroelectric fatigue property detects, and lists in respectively Fig. 2, Fig. 3 in the accompanying drawing.
3, test example two gained samples are carried out the detection of photoelectric response feature (photoelectric current ~ time, I ~ T response curve), listed in Fig. 4 in the accompanying drawing.
The results show, the BFO-PT film for preparing in the FTO Conducting Glass with the inventive method is water chestnut side's phase (Fig. 1), crystallinity is good, film sample can bear larger voltage, and show good ferroelectric properties, use PUND pulse test, after having removed the non-ferroelectric factor such as leakage current, obtain under 20v voltage, obtaining the residual polarization value and be about 2Pr ~ 28 μ C*cm
2Fatigue Test uses pulse wave in conjunction with PUND Pulse test, through 10
8After the upset, under the 10kHz frequency, surpassing 10
8After the inferior counter-rotating, the residual polarization value descends 70%, compares with present most widely used Pb-based lanthanumdoped zirconate titanates (PZT) film, and relevant pzt thin film surpasses 10 under higher 50kHz
8After the inferior counter-rotating, the residual polarization value also descends more than 80%, so this 0.7BFO-0.3PT/FTO structured material has the ferroelectric memory property (Fig. 2,3) that is better than PZT
Under the radiation environment of standard-and AM1.5 sun light intensity, the light and shade electric current has the difference (dark current: 5x10 that is about an order of magnitude when applying the little bias voltage of 2V
-6A, photoelectric current: 4x10
-6A) the photoresponse time is ~ 90s, and the photoelectric response feature is obvious.(Fig. 4)
About with the 0.7BFO-0.3PT/FTO structural representation of top electrode with reference to figure 5.
Of the present inventionly apply the 0.7BFO-0.3PT film with sol-gel process at the FTO conductive glass, by adjusting the additive formula in the precursor sol liquid, obtain the additive formula window of optimization, realized collecting bismuth ferrite-lead titanate (0.7BFO-0.3PT) thin film technology of ferroelectric storage and visible light photoelectric response.
Claims (1)
1. the preparation method of the bismuth ferrite-lead titanate with ferroelectric storage and visible light photoelectric response function/FTO conductive glass structured material is characterized in that having following technological process and step:
The pre-treatment of FTO Conducting Glass:
Dab with acetone and to wash substrate surface, pass through again acetone, 3 sonic oscillations of dehydrated alcohol, at least 5 minutes at every turn, use at last washed with de-ionized water, dry for standby;
The preparation of bismuth ferrite-lead titanate (being 0.7BFO-0.3PT) colloidal sol:
(1) takes by weighing positive four butyl esters of a certain amount of metatitanic acid with analytical balance, add the proper amount of glycol methyl ether; Take by weighing a certain amount of plumbic acetate, 60
0The C oil bath stirs to clarify; Add afterwards a certain amount of mixed solution; Mixed solution consists of: water, and Glacial acetic acid and ethylene glycol monomethyl ether three are mixed by certain molar ratio 1:2:1; Configuration obtains the precursor solution of lead titanate;
(2) oil bath temperature is adjusted to 90
0C continues to stir precursor solution and takes off placement normal temperature after 2 hours; Add a certain amount of ethylene glycol monomethyl ether stirring and dissolving under the room temperature; Then add the certain proportion methane amide, the add-on of methane amide is measured with the mol ratio 1:2 of itself and positive four butyl esters of metatitanic acid ~ 1:6; Ratio according to 0.7BFO-0.3PT after stirring takes by weighing respectively a certain amount of five water Bismuth trinitrates and nine water iron nitrates, successively add, then stirring at room is to fully dissolving, add the certain proportion Glacial acetic acid with drop-burette at last, stir 24h, form bismuth ferrite-lead titanate (0.7BFO-0.3PT) colloidal sol, leave standstill behind the 12-48h stand-by;
C. apply bismuth ferrite-lead titanate (0.7BFO-0.3PT) film and anneal at the FTO conductive glass:
Use the desk-top sol evenning machine of SC-1B type with the precursor sol of preparation with 1000 rev/mins, 5 seconds; 3000 rev/mins, 25 seconds speed is spin-coated on the FTO Conducting Glass, and then on the BP-2B type drying glue platform 240
0Most volatile organic matter is removed in the C baking, follows in the quick photo-thermal stove of KG-2-ZE type 500
0Under the C pre-crystallized 5 minutes, obtain thin film; So repeat above-mentioned spin coating, crystallization processes 12 times, obtain certain thickness film; At last in retort furnace 600
0C annealing made its complete crystallization in 1 hour;
Finally obtain complete bismuth ferrite-lead titanate/FTO glass structure material.
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| CN105399339A (en) * | 2015-12-18 | 2016-03-16 | 北京汽车股份有限公司 | Bismuth ferrite-based thin film containing doping elements, and preparation method thereof |
| CN106906517A (en) * | 2017-02-27 | 2017-06-30 | 西安交通大学 | A kind of bismuth ferrite lead titanates piezoelectric monocrystal and preparation method thereof |
| CN110656350A (en) * | 2019-11-13 | 2020-01-07 | 苏州大学 | Ferroelectric film ternary composite photoelectrode and preparation method thereof |
| CN112340787A (en) * | 2020-11-09 | 2021-02-09 | 东北大学秦皇岛分校 | Single-phase spinel type high-entropy oxide, preparation method and application |
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| CN103193395A (en) * | 2013-03-28 | 2013-07-10 | 上海大学 | Synthesis of bismuth-ferrum multiferroic film serving in high electric field |
| CN103193395B (en) * | 2013-03-28 | 2016-02-17 | 上海大学 | A kind ofly to be on active service in the synthesis of the bismuth iron system multiferroic film of high electric field |
| CN103736494A (en) * | 2014-01-02 | 2014-04-23 | 上海大学 | Preparation method of ternary oxide film structure with visible light photoelectric catalysis effect |
| CN105399339A (en) * | 2015-12-18 | 2016-03-16 | 北京汽车股份有限公司 | Bismuth ferrite-based thin film containing doping elements, and preparation method thereof |
| CN105399339B (en) * | 2015-12-18 | 2018-12-11 | 北京汽车股份有限公司 | A kind of ferrous acid bismuth-based thin films and preparation method thereof containing doped chemical |
| CN106906517A (en) * | 2017-02-27 | 2017-06-30 | 西安交通大学 | A kind of bismuth ferrite lead titanates piezoelectric monocrystal and preparation method thereof |
| CN110656350A (en) * | 2019-11-13 | 2020-01-07 | 苏州大学 | Ferroelectric film ternary composite photoelectrode and preparation method thereof |
| CN110656350B (en) * | 2019-11-13 | 2021-11-19 | 苏州大学 | Ferroelectric film ternary composite photoelectrode and preparation method thereof |
| CN112340787A (en) * | 2020-11-09 | 2021-02-09 | 东北大学秦皇岛分校 | Single-phase spinel type high-entropy oxide, preparation method and application |
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