CN110422882A - A kind of novel ferroelectric material and preparation method thereof - Google Patents
A kind of novel ferroelectric material and preparation method thereof Download PDFInfo
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- CN110422882A CN110422882A CN201910643018.6A CN201910643018A CN110422882A CN 110422882 A CN110422882 A CN 110422882A CN 201910643018 A CN201910643018 A CN 201910643018A CN 110422882 A CN110422882 A CN 110422882A
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Abstract
The invention discloses a kind of novel ferroelectric material, the chemical molecular formula of the ferroelectric material is BaFe4O7.The sol gel preparation method of the hydrothermal preparing process of ferroelectric material BaFe4O7, the high-temperature solid phase preparation method of ferroelectric material BaFe4O7 and ferroelectric material BaFe4O7.In material structure, since FeO4 tetrahedron and FeO6 octahedron are distorted, promote Fe3+ ion deflection tetrahedron and octahedral center, ferroelectricity is showed so as to cause sample, the material has the ferroelectric transition temperature of room temperature or more, the light absorption of visible-range, and there is significant photoelectric respone under visible light photograph, this kind of ferroelectricity photovoltaic material may have broad application prospects in terms of photoelectric conversion, information storage and sensor.
Description
Technical field
The present invention relates to photoelectric conversion and photovoltaic technology field, especially a kind of novel ferroelectric photovoltaic material and its preparation side
Method.
Background technique
The fundamental way for solving energy crisis is the effective use of renewable energy, and solar energy is most abundant, most important
Green energy resource, and be not limited by regions, great exploitation potential.Currently, solar-energy photo-voltaic cell mainly have silicon-based photovoltaic cells,
Inorganic multivariate compound photovoltaic cell, dye-sensitized photovoltaic battery, polymer multi-layer modified electrode type photovoltaic cell, perovskite light
Battery etc. is lied prostrate, in silicon-based photovoltaic cells, single silicon is the most mature, large-scale production, and photoelectric conversion efficiency generally exists
16%-18%, highest transfer efficiency is 24.7% under lab, but the at high price and mono-crystalline silicon solar of monocrystalline silicon is electric
Pond preparation process is complicated, it is made to be difficult to large area production.Polysilicon solar cell can reduce cost well, its advantage is that
The large scale square silicon ingot suitable for large-scale production can be directly produced, equipment is fairly simple, thus manufacturing process is simple, saves
Electricity saves silicon materials, requires material relatively low.And although amorphous silicon cost of manufacture is relatively low, transfer efficiency also can achieve
17.4%, but its stability difference and easy initiation photoelectric efficiency attenuating effect, limit the practical application of amorphous silicon battery.Arsenic, sulphur
II-VI compounds of group such as III-V compounds of group, CdS, copper indium gallium selenide such as including GaAs being typically used in race's photoelectricity compound
(CIGS) etc., the advantages of battery that this kind of material is produced, is low cost of manufacture, high efficiency, simple process and is easy to industrialize
Production, but in view of the toxicity of the elements such as gallium, cadmium, arsenic is big and pollutes the scarcity of the elements such as environment and indium, gallium, tellurium, such
Photoelectricity compound and nonideal photovoltaic material.
It has been investigated that, ferroelectricity photovoltaic material has very big application potential in solar-energy photo-voltaic cell field in recent years.
Because ferroelectricity photovoltaic material is different from the p-n junction in semiconductor, the photovoltaic effect of ferroelectricity photovoltaic material depends on material internal electric field
Polarization induction, therefore photovoltage is not limited by material band gap, can efficiently separate photo-generated carrier.However, conventional iron
The band gap of electric material is typically larger than 3 eV, this also means that 80% or more sunlight can not be absorbed by these materials, greatly
Photovoltaic performance is reduced, the practical application of ferroelectricity photovoltaic material is limited.Up to the present, with the ferroelectric material pole of narrow band gap
To be rare, and traditional perovskite structure is belonged to greatly, such as: BiFeO3 and [KNbO3] 1-x [BaNi1/2Nb1/2O3- δ] x, and
Non-perovskite type narrow band gap ferroelectricity photovoltaic material only has KBiFe2O5 at present.Therefore, the Novel iron electric light of exploitation narrow band gap is needed
Material is lied prostrate, replaces conventional iron electricity photovoltaic material to be conducive to ferroelectricity solar battery to greatly improve photovoltaic effect and exist with expectation
Development in terms of practical application.
Summary of the invention
To solve the above problems, the object of the present invention is to provide a kind of single-phase trigonal crystal structure, ferroelectricity is originated from FeO4 tetra-
Face body and FeO6 octahedron are distorted and promote Fe3+ ion deflection tetrahedron and octahedral center, and sample is in room temperature
When have ferroelectricity, visible light photograph under with significant photoelectric respone novel ferroelectric material and preparation method thereof.
To achieve the above object, technical solution of the present invention:
A kind of novel ferroelectric material, the chemical molecular formula of the ferroelectric material are BaFe4O7.
Preferably, the ferroelectric material is non-perovskite type trigonal crystal structure, FeO6 octahedron connects structure by total side
At two-dimensional layer, a three-dimensional net structure is constituted by the FeO4 tetrahedron trigonal biyramid that total vertex connects between layer and layer,
Ba atom is interspersed between tetrahedron and octahedron in gap.
Preferably, the ferroelectricity of the ferroelectric material is originated from FeO4 tetrahedron and FeO6 octahedron is distorted and promotees
Make Fe3+ ion deflection tetrahedron and octahedral center.
The hydrothermal preparing process of ferroelectric material BaFe4O7, the specific steps are as follows:
(1) soluble-salt of reaction raw materials Ba and Fe are made into the clear solution of 0.2M, liquid is taken according to molar ratio 1:4, in magnetic
It is stirred evenly on power blender;
(2) addition KOH or NaOH solid in mixed solution is stated directly up, so that solution basicity is reached 8M or more, in lasting stirring
Under mix mixture uniformly;
(3) it after said mixture is cooled to room temperature, is transferred in reaction kettle, compactedness 70%-80%, in 180-240
Reaction kettle is cooled to room temperature after being reacted 1-3 days in DEG C baking oven, and release;
(4) synthetic sample is cleaned with deionized water and ethyl alcohol, and is ultrasonically treated in ultrasonic oscillator, obtain black small
Grain crystal prototype, finally dries sample in 60 DEG C of baking ovens.
The high-temperature solid phase preparation method of ferroelectric material BaFe4O7, the specific steps are as follows:
(1) uniform according to molar ratio 1:4 ratio ground and mixed by the oxide or carbonate of reaction raw materials Ba and Fe;
(2) it will be transferred in crucible after mixture tabletting, heated 6-12 hours within the temperature range of 600-900 DEG C;
(3) by after above-mentioned resulting product grinding, step (3) are repeated until obtaining BaFe4O7 pure phase;
(4) it is cleaned with deionized water after impregnating synthetic sample with dust technology, and is ultrasonically treated in ultrasonic oscillator again, obtained
To black powder sample, finally sample is dried in 60 DEG C of baking ovens.
The sol gel preparation method of ferroelectric material BaFe4O7, the specific steps are as follows:
(1) taking a certain amount of molar ratio is that Ba the and Fe soluble-salt of 1:4 is placed in beaker, and the aqueous solution of nitric acid of 1:5, In is added
Stirred evenly on magnetic stirring apparatus, backward mixed solution in citric acid is added as chelating agent, and 1-2 is stirred at room temperature
Hour;
(2) it takes a certain amount of above-mentioned mixed liquor to be placed in evaporating dish, is heated to mixture in 250 DEG C of water-bath and is changed into colloid
State;
(3) the above-mentioned evaporating dish for having colloid that multiplies is placed on 400-600 DEG C calcining 1 hour in Muffle furnace, tentatively obtained
BaFe4O7 black powder;
(4) the above-mentioned powder prepared is placed in 700-900 DEG C annealing 4-8 hours in Muffle furnace, obtains BaFe4O7 nanometers
Grain.
Preferably, the ferroelectric material constitutive material are as follows:
(1) source Ba can be one of soluble-salt, oxide, carbonate or multiple combinations;
(2) source Fe can be one of soluble-salt, oxide, carbonate or multiple combinations.
Beneficial conditions of the invention are:
1, the BaFe prepared by the present invention4O7With relatively narrow band gap, most of visible light can be absorbed;
2, preparation method of the invention is simple, very low to equipment requirement, cheap, can prepare more perfect crystalline material, and
It can obtain very pure product;
3, BaFe of the invention4O7Ferroelectricity transition temperature more than room temperature (556 DEG C), have FeO4Tetrahedral layer and FeO6Eight
The alternately arranged non-perovskite structure of face body layer, optical band gap are about 2.2 eV, with traditional ferroelectric material BiFeO32.7
EV is compared, and band gap is lower;
4, ferroelectric material of the present invention synthesizes ferroelectricity photovoltaic material (especially narrow band gap ferroelectricity photovoltaic material) more new systems
Discovery provide good reference.
Detailed description of the invention
Fig. 1 is BaFe prepared by embodiment 14O7The Powder XRD pattern and structural schematic diagram of material.
Fig. 2 is BaFe prepared by embodiment 14O7The crystal morphology SEM and EDS of material scheme.
Fig. 3 is BaFe prepared by embodiment 14O7The dielectric thermogram of material.
Fig. 4 is BaFe prepared by embodiment 14O7The UV Diffuse Reflectance Spectroscopy and optical band gap figure of material.
Fig. 5 is BaFe prepared by embodiment 14O7Material under visible light illumination, photogenerated current density when 0 V bias and
Its photoelectric respone time diagram.
Specific embodiment
As shown in Fig. 1,2,3,4,5, the present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The hydrothermal preparing process of above-mentioned novel ferroelectric material BaFe4O7 is prepared, specifically:
(1) a certain amount of Ba (NO3) 25H2O and Fe (NO3) 39H2O is taken to be made into the solution for standby of 0.2 M respectively;
(2) it takes above-mentioned Ba (NO3) 2 and 3 solution of Fe (NO3) to take liquid according to molar ratio 1:4, is placed in the beaker of 100 mL, In
KOH solid is added under conditions of magnetic agitation, solution basicity is made to reach 8M or more, and uniformly mixing under continuous stirring;
(3) it after said mixture is cooled to room temperature, is transferred in reaction kettle, compactedness 80%, is reacted in 240 DEG C of baking ovens
Reaction kettle is cooled to room temperature after 3 days, and release;
(4) synthetic sample is cleaned with deionized water and ethyl alcohol, and is ultrasonically treated in ultrasonic oscillator, obtain black small
Grain BaFe4O7 crystal prototype, finally dries sample in 60 DEG C of baking ovens.
Fig. 1 is BaFe4O7 material powder XRD spectrum and structural schematic diagram prepared by embodiment 1, as we know from the figure sample
Powder X-ray RD is consistent with simulated metrics result, illustrates there is very high purity, sample by BaFe4O7 sample prepared by hydro-thermal method
Product are trigonal crystal structure, space group P31c, and Sample crystals structure can be described as: the FeO6 octahedral layer of side connection passes through altogether altogether
Side constitutes two-dimensional layer, constitutes a three-dimensional network knot by the FeO4 tetrahedron trigonal biyramid that total vertex connects between layer and layer
Structure, Ba atom are interspersed between tetrahedron and octahedron in gap;Fig. 2 is the crystal of BaFe4O7 material prepared by embodiment 1
Pattern SEM and EDX figure, sample are six square blocks, and size is at 10-30 μm, and its component known to EDX analysis is
BaFe4O7 further proves that sample is pure phase;Fig. 3 is the dielectric temperature spectrum of BaFe4O7 material prepared by embodiment 1, and sample exists
An apparent abnormal Dielectric peak is shown at 556 DEG C, illustrates that ferroelectric phase has occurred to paraelectric phase in this temperature or so in sample
Transformation, sample show ferroelectricity when being lower than this temperature;Fig. 4 is BaFe4O7 UV Diffuse Reflectance Spectroscopy, as seen from the figure sample
Light absorption with visible-range, forbidden bandwidth are about 2.2 eV;Fig. 5 is BaFe4O7 material prepared by embodiment 1 can
Under light-exposed irradiation, photogenerated current densogram when 0 V bias is 4 nA/cm2 by the density of photocurrent of Fig. 5 derived sample
Left and right;Therefore, BaFe4O7 has visible absorption, and shows significant photoelectric response performance.
Embodiment 2
The high-temperature solid phase preparation method of above-mentioned novel ferroelectric material BaFe4O7 is prepared, specifically:
(1) taking a certain amount of molar ratio is the oxide or carbonate powder of the Ba and Fe of 1:4, and ground and mixed is uniform;
(2) said mixture is transferred in planetary ball mill tank, and the tungsten-carbide ball of suitable ethyl alcohol and 5 mm is added, in planet
It is ground in formula ball mill, parameter is set as 350 rpm/min, and 10 min of every operation suspend 5 min cooling, and rear setting reversion repeats
Above-mentioned parameter grinds duration 4 hours, obtains being sufficiently mixed uniform fine powder;
(3) will be transferred in crucible after above-mentioned fine powder tabletting, 900 DEG C at a temperature of heat 12 hours, obtain black block sample
Product;
(4) by after above-mentioned resulting product grinding, step (3) are repeated until obtaining BaFe4O7 pure phase;
(5) it is cleaned with deionized water after impregnating synthetic sample with dust technology, and is ultrasonically treated in ultrasonic oscillator again, obtained
To black powder sample, finally sample is dried in 60 DEG C of baking ovens.
Embodiment 3
The sol-gel process for preparing of above-mentioned novel ferroelectric material BaFe4O7 is prepared, specifically:
(1) taking a certain amount of molar ratio is that Ba (NO3) 25H2O and Fe (NO3) 39H2O of 1:4 is placed in beaker, is added 1:
It is molten to be added to the clarification using citric acid as chelating agent later for 5 aqueous solution of nitric acid, 30 minutes formation clear solutions of magnetic agitation
It in liquid, and is stirred at room temperature 2 hours, carries out complex reaction sufficiently;
(2) it takes a certain amount of above-mentioned mixed liquor to be placed in evaporating dish, is heated to mixture in 250 DEG C of water-bath and is changed into colloid
State, this process carry out in draught cupboard;
(3) the above-mentioned evaporating dish for having colloid that multiplies is placed on 500 DEG C calcining 1 hour in Muffle furnace, tentatively obtains BaFe4O7 black
Powder;
(4) the above-mentioned powder prepared is placed in Muffle furnace and is annealed 8 hours for 800 DEG C, obtain black BaFe4O7 nano particle.
It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, above-described embodiment and explanation
It is merely illustrated the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also has
Various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention
It is defined by the appending claims and its equivalent thereof.
Claims (7)
1. a kind of novel ferroelectric material, which is characterized in that the chemical molecular formula of the ferroelectric material is BaFe4O7.
2. a kind of novel ferroelectric material according to claim 1, which is characterized in that the ferroelectric material is non-perovskite
Type trigonal crystal structure, FeO6 octahedron connect and compose two-dimensional layer by total side, the FeO4 connected between layer and layer by total vertex
Tetrahedron trigonal biyramid constitutes a three-dimensional net structure, and Ba atom is interspersed between tetrahedron and octahedron in gap.
3. a kind of novel ferroelectric material according to claim 1, which is characterized in that the ferroelectricity source of the ferroelectric material
It is distorted from FeO4 tetrahedron and FeO6 octahedron and promotes Fe3+ ion deflection tetrahedron and octahedral center.
4. the hydrothermal preparing process of ferroelectric material BaFe4O7 according to claim 1 to 3, which is characterized in that specific steps
It is as follows:
(1) soluble-salt of reaction raw materials Ba and Fe are made into the clear solution of 0.2M, liquid is taken according to molar ratio 1:4, in magnetic
It is stirred evenly on power blender;
(2) addition KOH or NaOH solid in mixed solution is stated directly up, so that solution basicity is reached 8M or more, in lasting stirring
Under mix mixture uniformly;
(3) it after said mixture is cooled to room temperature, is transferred in reaction kettle, compactedness 70%-80%, in 180-240
Reaction kettle is cooled to room temperature after being reacted 1-3 days in DEG C baking oven, and release;
(4) synthetic sample is cleaned with deionized water and ethyl alcohol, and is ultrasonically treated in ultrasonic oscillator, obtain black small
Grain crystal prototype, finally dries sample in 60 DEG C of baking ovens.
5. the high-temperature solid phase preparation method of ferroelectric material BaFe4O7 according to claim 1 to 3, which is characterized in that specific
Steps are as follows:
(1) uniform according to molar ratio 1:4 ratio ground and mixed by the oxide or carbonate of reaction raw materials Ba and Fe;
(2) it will be transferred in crucible after mixture tabletting, heated 6-12 hours within the temperature range of 600-900 DEG C;
(3) by after above-mentioned resulting product grinding, step (3) are repeated until obtaining BaFe4O7 pure phase;
(4) it is cleaned with deionized water after impregnating synthetic sample with dust technology, and is ultrasonically treated in ultrasonic oscillator again, obtained
To black powder sample, finally sample is dried in 60 DEG C of baking ovens.
6. the sol gel preparation method of ferroelectric material BaFe4O7 according to claim 1 to 3, which is characterized in that specific
Steps are as follows:
(1) taking a certain amount of molar ratio is that Ba the and Fe soluble-salt of 1:4 is placed in beaker, and the aqueous solution of nitric acid of 1:5, In is added
Stirred evenly on magnetic stirring apparatus, backward mixed solution in citric acid is added as chelating agent, and 1-2 is stirred at room temperature
Hour;
(2) it takes a certain amount of above-mentioned mixed liquor to be placed in evaporating dish, is heated to mixture in 250 DEG C of water-bath and is changed into colloid
State;
(3) the above-mentioned evaporating dish for having colloid that multiplies is placed on 400-600 DEG C calcining 1 hour in Muffle furnace, tentatively obtained
BaFe4O7 black powder;
(4) the above-mentioned powder prepared is placed in 700-900 DEG C annealing 4-8 hours in Muffle furnace, obtains BaFe4O7 nanometers
Grain.
7. ferroelectric material BaFe4O7 described in -6 according to claim 1, which is characterized in that the ferroelectric material constitutive material
Are as follows:
(1) source Ba can be one of soluble-salt, oxide, carbonate or multiple combinations;
(2) source Fe can be one of soluble-salt, oxide, carbonate or multiple combinations.
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Cited By (1)
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CN110957381A (en) * | 2019-12-18 | 2020-04-03 | 上海材料研究所 | Narrow-band-gap ferroelectric photovoltaic material and preparation method and application thereof |
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