CN103482691A - Doped Bi4Ti3O12 film and preparation method thereof - Google Patents

Doped Bi4Ti3O12 film and preparation method thereof Download PDF

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CN103482691A
CN103482691A CN201310398578.2A CN201310398578A CN103482691A CN 103482691 A CN103482691 A CN 103482691A CN 201310398578 A CN201310398578 A CN 201310398578A CN 103482691 A CN103482691 A CN 103482691A
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夏傲
谈国强
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a doped Bi4Ti3O12 film and a preparation method thereof. The chemical formula of the film is Bi4Ti3-xHfxO12, wherein x=0.01-0.15. The preparation method comprises the following steps: generating an OTS monomolecular film on the surface of a substrate, removing a residual solution on the surface of the substrate, and functionalizing the OTS surface under irradiation of ultraviolet light to obtain the substrate with an attached functionalized OTS monolayer film; preparing a Bi(NO3)3.5H2O solution by using ethylene glycol monomethyl ether as solvent, adding HfOCl2, dissolving by stirring, transferring the obtained mixed solution into a vessel filled with Ti(OC4H9)4 and citric acid, further uniformly dissolving by stirring, and regulating the pH value of the obtained solution to 2.0, thus preparing a precursor solution; horizontally putting the substrate with the attached functionalized OTS monolayer film in the precursor solution, and depositing to obtain an amorphous film; and heating to 540-570 DEG C in a muffle furnace at a rate of 20-25 DEG C/min, and keeping the temperature for 20-30 minutes, thus obtaining the doped Bi4Ti3O12 film. The method is simple in preparation process and friendly to environment; the thickness of the film is easy to control; the crystalline phase of the film completely grows and is high in purity; the surface of the film is smooth, level, uniform and compact; and the film is firmly combined with the substrate.

Description

A kind of doping type Bi 4ti 3o 12film and preparation method thereof
Technical field
The present invention relates to a kind of Bi 4ti 3o 12film and preparation method thereof, be specifically related to a kind of doping type Bi 4ti 3o 12film and preparation method thereof.
Background technology
Bismuth titanates (Bi 4ti 3o 12) ferroelectric material that is laminated perovskite structure as a kind of typical bismuth, there is the performances such as good piezoelectricity, ferroelectric, pyroelectricity and electricity.Bi 4ti 3o 12crystalline structure be anisotropic cubic structure, it is by (Bi 2o 2) 2+(Bi 2ti 3o 10) 2-the perovskite structure layer forms separately.At (Bi 2ti 3o 10) 2-in perovskite structure layer unit, the Ti ion is surrounded by oxygen octahedra, forms the O-Ti-O key, and the Bi ion is positioned at TiO 6in the space of octahedra grid, 2 (Bi 2o 2) 2+the height of layer is 6 Ti-O key lengths.Its ferroelectric-para-electric phase transformation belongs to first-order phase transition, due to the unit cell of monoclinic phase near orthogonal crystallographic system very, therefore lattice parameter available orthogonal crystallographic system is described: a=0.5450, b=0.5406, c=3.2832nm.Its spontaneous polarization vector is positioned at the a-c plane, becomes about 4.5 ° of angles with a axle, along a axle and c-axis spontaneous polarization component, differ greatly, and be respectively 50 μ C/cm 2with 4 μ C/cm 2.
In recent years, people are to Bi 4ti 3o 12the Bi of the A position of film and the Ti of B position have carried out multiple doping research.Film performance after doping is greatly improved at aspects such as residual polarization, fatigue resistances.According to doping for ionic radius, Curie temperature stable (Tc>400 ℃), be easy to generate the requirement of stable perovskite structure, can be at Bi 4ti 3o 12the rare earth element that adulterated of A position La, Nd, Pr, Sm, Eu, Gd etc. are arranged.And, in the B position, usually carry out the donor ion doping of high price, as Nb, V, W etc.Doping for A position rare earth element, the people such as Uong Chon think, doping can make in 3 oxygen octahedras in the middle of bismuth oxygen layer, the position of the Ti of upper and lower two oxygen octahedras has highly asymmetric pair potential well, cause spontaneous polarization to increase along the deflection of c-axis direction, thereby the residual polarization of the c-axis direction of BIT film is increased.And, for B position doping, the increase of residual polarization is mainly the cause that the c-axis orientation degree due to film reduces, with the attribute of dopant ion itself, have nothing to do.
At present, Bi 4ti 3o 12the preparation method of film mainly contains metal organic chemical vapor deposition, sol-gel method, magnetron sputtering method and pulsed laser deposition.The vacuum environment that the common equipment of these preparation technologies is comparatively complicated, needs are strict and process system, cost costliness, or need the high-temperature calcination art breading, preparation process pollutes, and all can not realize that technique is simple, save energy and eco-friendly target.
Summary of the invention
The object of the present invention is to provide a kind of doping type Bi 4ti 3o 12film and preparation method thereof, the method preparation technology is simple, film thickness is easy to control and environmental friendliness, the doping type Bi of preparation 4ti 3o 12film crystalline phase zoon, purity are high, and film surface is smooth, smooth, even compact, and film is combined firmly with substrate.
In order to achieve the above object, doping type Bi of the present invention 4ti 3o 12film, chemical formula is Bi 4ti 3-xhf xo 12, wherein, x=0.01～0.15.
A kind of doping type Bi 4ti 3o 12the preparation method of film comprises the following steps:
1) preparation of OTS unimolecular layer and functionalization:
The mixing solutions of clean substrate being put into to OTS and toluene deposits, make substrate surface generate OTS unit molecule rete, remove subsequently the substrate surface residual solution, then irradiate 35-50min under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds stirring and dissolving in ethylene glycol monomethyl ether, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, and stirring and dissolving, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the container of citric acid, continue stirring and dissolving even, then adjust the pH value to 2.0 of gained solution, be mixed with precursor liquid; Wherein, Bi in precursor liquid 3+, Ti 4+and Hf 4+total concn be 0.01～0.05mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be that ((3-x) ︰ x, the concentration of wherein x=0.01～0.15, and citric acid equals Bi to 10～30) ︰ 3+, Ti 4+and Hf 4+total concn;
3) thin film deposition:
The OTS unitary film substrate level of attached function is placed in to precursor liquid, under 45-55 ℃, deposits 15～20h, obtain noncrystalline membrane;
4) crystallization of film is processed:
Noncrystalline membrane is put into to retort furnace, be incubated 20-30min after being warming up to 540-570 ℃ with the speed of 20-25 ℃/min, obtain doping type Bi 4ti 3o 12film.
Described substrate adopts the FTO glass substrate.
Described step 1) is removed the substrate surface residual solution and is realized by baking under 120 ℃.
In OTS in described step 1) and the mixing solutions of toluene, the volume ratio of OTS and toluene is 1:(95-105).
Described step 2) the pH value in is regulated by dripping Glacial acetic acid.
In described step 3), the substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid.
Compared with prior art, beneficial effect of the present invention is:
The present invention adopts the self-assembled monolayer membrane technique, and the OTS unit molecule rete of take is template, has prepared doping type Bi on the FTO glass substrate 4ti 3o 12film, i.e. Hf doping Bi 4ti 3o 12film.Prepared doping type Bi 4ti 3o 12hf in film 4+replace part Ti 4+position, thereby generate Bi 4ti 3-xhf xo 12phase, Hf 4+doping adjusted Bi 4ti 3o 12crystalline structure, be expected to its ferroelectric properties is produced to material impact.Through evidence, the doping type Bi that the present invention makes 4ti 3o 12film crystalline phase zoon, purity is high, and film surface is smooth, smooth, even compact, and film is combined firmly with substrate.
In addition, the self-assembled monolayer membrane technique that the present invention adopts is on traditional liquid phase deposition basis, in conjunction with the formed a kind of new film-forming method of bionical blending theory.Adopting the self-assembled monolayer membrane technique to prepare thin-film material is to utilize its functionalized surface for template-mediated inorganics deposition, makes the inorganics presoma of solubility be attached to substrate surface, promotes the inorganics film in surface nucleation and growth.This method is a kind of environment amenable filming technology, it is without specific installation, there is low temperature preparation, but the characteristics such as inorganic film of tight difficult drop-off induction and deposition with the nano level micro-pattern are easily controlled, are combined with substrate to film thickness, therefore, simple, the film thickness of preparation technology of the present invention is easy to control and environmental friendliness.
The accompanying drawing explanation
The doping type Bi that Fig. 1 is the embodiment of the present invention 1 preparation 4ti 3o 12the XRD figure spectrum of film;
The doping type Bi that Fig. 2 is the embodiment of the present invention 1 preparation 4ti 3o 12the EDS collection of illustrative plates of film;
The doping type Bi that Fig. 3 is the embodiment of the present invention 1 preparation 4ti 3o 12the SEM photo of film.
Embodiment
Embodiment 1:
1) preparation of OTS unimolecular layer and functionalization:
Clean FTO glass substrate is put into to OTS that volume ratio is 1:100 and the mixing solutions of toluene deposits 20min, make substrate surface generate OTS unit molecule rete, subsequently substrate is toasted under 120 ℃ to 5 minutes to remove remained on surface solution, irradiate 40min again under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds in ethylene glycol monomethyl ether solution, stirs it is dissolved fully, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, be stirred to and be uniformly dissolved equally, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the beaker of citric acid, continue stirring and dissolving even, then drip the pH value to 2.0 that Glacial acetic acid is adjusted gained solution, be made into precursor liquid; Wherein, in precursor liquid, Bi 3+, Ti 4+and Hf 4+total concn be 0.02mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be 15 ︰ 2.97 ︰ 0.03, the concentration of citric acid is 0.02mol/L;
3) thin film deposition:
The FTO glass substrate level of the OTS unitary film of attached function is placed in to precursor liquid, under 50 ℃, deposits 15h, obtain noncrystalline membrane; Wherein, the FTO glass substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid;
4) crystallization of film is processed:
Dried noncrystalline membrane is put into to retort furnace, be incubated 30min after being warming up to 560 ℃ with the speed of 25 ℃/min, obtain doping type Bi 4ti 3o 12film.
The doping type Bi that the present embodiment makes 4ti 3o 12the chemical formula of film is Bi 4ti 2.97hf 0.03o 12; As seen from Figure 1, in collection of illustrative plates except the SnO from the FTO glass substrate 2diffraction peak, all the other diffraction peaks and Bi 4ti 3o 12diffraction peak fit like a glove, and the peak type of diffraction peak is sharp-pointed, this explanation film crystalline phase zoon, purity is high.The compound appearance that does not have in addition other to contain Hf in collection of illustrative plates, this explanation Hf has been incorporated into Bi 4ti 3o 12lattice in.As seen from Figure 2, the unit in collection of illustrative plates have F, O, Ti, Bi, Hf and Sn, and wherein element F and Sn are from the FTO glass substrate, and other elements are from bismuth titanate film.The atlas analysis result of comparison diagram 1 and Fig. 2, result shows that EDS and XRD test result combine, and further illustrate Hf and have mixed Bi 4ti 3o 12lattice in.
By Fig. 3, for finding out, film surface is smooth, smooth, even compact.
Embodiment 2:
1) preparation of OTS unimolecular layer and functionalization:
Clean FTO glass substrate is put into to OTS that volume ratio is 1:95 and the mixing solutions of toluene deposits 25min, make substrate surface generate OTS unit molecule rete, subsequently substrate is toasted under 120 ℃ to 5 minutes to remove remained on surface solution, irradiate 50min again under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds in ethylene glycol monomethyl ether solution, stirs it is dissolved fully, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, be stirred to and be uniformly dissolved equally, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the beaker of citric acid, continue stirring and dissolving even, then drip the pH value to 2.0 that Glacial acetic acid is adjusted gained solution, be made into precursor liquid; Wherein, in precursor liquid, Bi 3+, Ti 4+and Hf 4+total concn be 0.01mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be 10 ︰ 2.99 ︰ 0.01, the concentration of citric acid is 0.01mol/L;
3) thin film deposition:
The FTO glass substrate level of the OTS unitary film of attached function is placed in to precursor liquid, under 45 ℃, deposits 20h, obtain noncrystalline membrane; Wherein, the FTO glass substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid;
4) crystallization of film is processed:
Dried noncrystalline membrane is put into to retort furnace, be incubated 25min after being warming up to 540 ℃ with the speed of 20 ℃/min, obtain doping type Bi 4ti 3o 12film.
The doping type Bi of the present embodiment 4ti 3o 12the chemical formula of film is Bi 4ti 2.99hf 0.01o 12.
Embodiment 3:
1) preparation of OTS unimolecular layer and functionalization:
Clean FTO glass substrate is put into to OTS that volume ratio is 1:105 and the mixing solutions of toluene deposits 15min, make substrate surface generate OTS unit molecule rete, subsequently substrate is toasted under 120 ℃ to 5 minutes to remove remained on surface solution, irradiate 35min again under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds in ethylene glycol monomethyl ether solution, stirs it is dissolved fully, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, be stirred to and be uniformly dissolved equally, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the beaker of citric acid, continue stirring and dissolving even, then drip the pH value to 2.0 that Glacial acetic acid is adjusted gained solution, be made into precursor liquid; Wherein, in precursor liquid, Bi 3+, Ti 4+and Hf 4+total concn be 0.05mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be 30 ︰ 2.90 ︰ 0.1, the concentration of citric acid is 0.05mol/L;
3) thin film deposition:
The FTO glass substrate level of the OTS unitary film of attached function is placed in to precursor liquid, under 55 ℃, deposits 18h, obtain noncrystalline membrane; Wherein, the FTO glass substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid;
4) crystallization of film is processed:
Dried noncrystalline membrane is put into to retort furnace, be incubated 20min after being warming up to 570 ℃ with the speed of 23 ℃/min, obtain doping type Bi 4ti 3o 12film.
The doping type Bi of the present embodiment 4ti 3o 12the chemical formula of film is Bi 4ti 2.9hf 0.1o 12.
Embodiment 4:
1) preparation of OTS unimolecular layer and functionalization:
Clean FTO glass substrate is put into to OTS that volume ratio is 1:105 and the mixing solutions of toluene deposits 15min, make substrate surface generate OTS unit molecule rete, subsequently substrate is toasted under 120 ℃ to 5 minutes to remove remained on surface solution, irradiate 35min again under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds in ethylene glycol monomethyl ether solution, stirs it is dissolved fully, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, be stirred to and be uniformly dissolved equally, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the beaker of citric acid, continue stirring and dissolving even, then drip the pH value to 2.0 that Glacial acetic acid is adjusted gained solution, be made into precursor liquid; Wherein, in precursor liquid, Bi 3+, Ti 4+and Hf 4+total concn be 0.05mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be 15 ︰ 2.85 ︰ 0.15, the concentration of citric acid is 0.05mol/L;
3) thin film deposition:
The FTO glass substrate level of the OTS unitary film of attached function is placed in to precursor liquid, under 55 ℃, deposits 18h, obtain noncrystalline membrane; Wherein, the FTO glass substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid;
4) crystallization of film is processed:
Dried noncrystalline membrane is put into to retort furnace, be incubated 20min after being warming up to 570 ℃ with the speed of 23 ℃/min, obtain doping type Bi 4ti 3o 12film.
The doping type Bi of the present embodiment 4ti 3o 12the chemical formula of film is Bi 4ti 2.85hf 0.15o 12.

Claims (7)

1. a doping type Bi 4ti 3o 12film is characterized in that: chemical formula is Bi 4ti 3-xhf xo 12, wherein, x=0.01～0.15.
2. a doping type Bi 4ti 3o 12the preparation method of film, is characterized in that, comprises the following steps:
1) preparation of OTS unimolecular layer and functionalization:
The mixing solutions of clean substrate being put into to OTS and toluene deposits, make substrate surface generate OTS unit molecule rete, remove subsequently the substrate surface residual solution, then irradiate 35-50min under UV-light, thereby realize that OTS is surface-functionalized, obtain the OTS unitary film substrate of attached function;
2) preparation of precursor liquid:
By Bi (NO 3) 35H 2o adds stirring and dissolving in ethylene glycol monomethyl ether, obtains Bi (NO 3) 3solution, then to Bi (NO 3) 3add HfOCl in solution 2, and stirring and dissolving, obtain mixing solutions; Mixing solutions is transferred to and fills Ti (OC 4h 9) 4in the container of citric acid, continue stirring and dissolving even, then adjust the pH value to 2.0 of gained solution, be mixed with precursor liquid; Wherein, Bi in precursor liquid 3+, Ti 4+and Hf 4+total concn be 0.01～0.05mol/L, Bi 3+, Ti 4+and Hf 4+mol ratio be that ((3-x) ︰ x, the concentration of wherein x=0.01～0.15, and citric acid equals Bi to 10～30) ︰ 3+, Ti 4+and Hf 4+total concn;
3) thin film deposition:
The OTS unitary film substrate level of attached function is placed in to precursor liquid, under 45-55 ℃, deposits 15～20h, obtain noncrystalline membrane;
4) crystallization of film is processed:
Noncrystalline membrane is put into to retort furnace, be incubated 20-30min after being warming up to 540-570 ℃ with the speed of 20-25 ℃/min, obtain doping type Bi 4ti 3o 12film.
3. doping type Bi according to claim 2 4ti 3o 12the preparation method of film is characterized in that: described substrate adopts the FTO glass substrate.
4. according to the described doping type Bi of claim 2 or 3 4ti 3o 12the preparation method of film is characterized in that: described step 1) is removed the substrate surface residual solution and is realized by baking under 120 ℃.
5. according to the described doping type Bi of claim 2 or 3 4ti 3o 12the preparation method of film is characterized in that: in the OTS in described step 1) and the mixing solutions of toluene, the volume ratio of OTS and toluene is 1:(95-105).
6. according to claim 2 or 3 doping type Bi 4ti 3o 12the preparation method of film is characterized in that: the pH value described step 2) is regulated by dripping Glacial acetic acid.
7. doping type Bi according to claim 2 4ti 3o 12the preparation method of film is characterized in that: in described step 3), the substrate of the OTS unitary film of attached function is that a ventricumbent mode that is attached with the OTS unitary film of functionalization is placed in to precursor liquid.
CN201310398578.2A 2013-09-04 2013-09-04 Doped Bi4Ti3O12 film and preparation method thereof Pending CN103482691A (en)

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CN104743891A (en) * 2015-03-20 2015-07-01 陕西科技大学 Preparation method of Bi4Ti3-xFexO12 ferroelectric film with high dielectric constant
CN106431391A (en) * 2016-09-13 2017-02-22 陕西科技大学 Method for preparing Bi4Ti(3-x)VxO12 powder

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CN104743891B (en) * 2015-03-20 2017-08-01 陕西科技大学 A kind of Bi of high-k4Ti3‑xFexO12The preparation method of ferroelectric thin film
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Application publication date: 20140101