CN101955323A - Method for preparing bismuth titanate functional membrane on glass substrate - Google Patents

Method for preparing bismuth titanate functional membrane on glass substrate Download PDF

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CN101955323A
CN101955323A CN 201010287622 CN201010287622A CN101955323A CN 101955323 A CN101955323 A CN 101955323A CN 201010287622 CN201010287622 CN 201010287622 CN 201010287622 A CN201010287622 A CN 201010287622A CN 101955323 A CN101955323 A CN 101955323A
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夏傲
谈国强
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a method for preparing a bismuth titanate functional membrane on a glass substrate. The method comprises the following steps of: (1) preprocessing a substrate; (2) depositing an OTS self-assembly membranous layer, namely performing depositing preparation of the OTS self-assembly membranous layer on the cleaned substrate in the step (1); (3) preparing reaction solution; (4) depositing a membrane by a liquid phase method; and (5) post-processing the membrane, namely performing heat preservation on the membrane at the temperature of between 550 and 650 DEG C for 30 minutes for annealing to obtain the bismuth titanate functional membrane. The method has the characteristics of in-situ and spontaneous formation, ordered arrangement of bonding height, a few defects, strong bonding force, crystalline state of the bismuth titanate membrane and the like.

Description

A kind of method that on glass substrate, prepares the bismuth titanates function film
Technical field:
The invention belongs to field of functional materials, the preparation method who relates to a kind of bismuth titanate film, especially a kind of method for preparing the bismuth titanates function film on glass substrate can be prepared by present method and to have the spontaneous formation of original position, become the bismuth ferrite thin film that the key high-sequential is arranged, defective is few, bonding force is strong.
Background technology:
Ferroelectric ceramic(s) has obtained in fields such as ultrasonic transduction, transmitter, nondestructive testing and mechanicss of communication to use widely as sensitive materials such as electricity, power, light.Along with the raising of miniaturization of devices, functionalization, stability and reliability, require the performance of material further to improve.Traditional ferroelectric ceramic(s) how leaded (as Pb-based lanthanumdoped zirconate titanates (PZT), lead lanthanum zirconate titanate (PLZT)), they bring very big infringement all can for environment and human health in preparation and use.In recent years, along with the demand of environment protection and social sustainable development, that world developed country begins to be devoted to research and develop is novel, with eco-friendly ferroelectric ceramic material, bismuth titanates (Bi 4Ti 3O 12One of) present hot subject that has become ferroelectric membranc preparation in the world and applied research.
As far back as the seventies in 20th century, U.S.'s Westing House electric corporation utilizes Bi 4Ti 3O 12Made first and be used for the FEFED ferro-electric field effect device of data storage, states such as Japan, Korea S, Europe also drop into a large amount of human and material resources and carry out Bi 4Ti 3O 12Research and development, thereby started people to Bi 4Ti 3O 12The upsurge of ferroelectric membranc research.Along with Bi 4Ti 3O 12Theory and experimental study sophisticated has higher residual polarization and height-oriented Bi 4Ti 3O 12Film and doping type Bi 4Ti 3O 12Film is produced out.People such as J.S.Kim adopt the method for adding tensio-active agent in preparation process, have obtained the Bi that is orientated along the c axle fully 4Ti 3O 12Film.It is 70 μ C/cm that people such as Ji Cheul Bae use the sol-gel method to make Pr 2Bi 4Ti 3O 12Film.People such as Hirofumi Matsuda are at Ir (111)/Ti/SiO 2The Bi that mixes praseodymium of a axle orientation of having grown on/the Si 4Ti 3O 12Film, its residual polarization Pr is up to 46 μ C/cm 2Human chemical solution depositions (CSD) such as Li Wei are at (111) Pt/Ti/SiO 2Prepared the polycrystalline Bi that mixes neodymium and tungsten simultaneously in/the Si substrate 4Ti 3O 12Film, its Pr and coercive field Ec are respectively 59.27 μ C/cm 2, 203.2kV/cm.
And domestic Bi 4Ti 3O 12Research start late, usefulness femtosecond pulse deposition techniques such as the Zhou Youhua of the Central China University of Science and Technology are prepared the Bi of a axle preferrel orientation on the Si substrate 4Ti 3O 12Ferroelectric membranc, the remnant polarization Pr of film are 15 μ C/cm 2, coercive field Ec is 48kV/cm, experiment shows that depositing temperature has material impact to the growth for Thin Film orientation.Usefulness sol-gel methodes such as the Guo Dongyun of the Central China University of Science and Technology have been prepared the Bi of random orientation on the p-Si substrate 4Ti 3O 12Film, its Pr and Ec are respectively 12 μ C/cm 2And 130kV/cm.Employing sol-gel methodes such as the Wang Xiuzhang of Hubei Normal University have prepared Bi on glass substrate 4Ti 3O 12With the adulterated Bi of neodymium 3.35Nd 0.65Ti 3O 12(BNT) film, ferroelectric test shows, neodymium mixes and makes the dielectricity of film and ferroelectricity obtain enhancing, and Pr is by 57.2 μ C/cm 2Be increased to 68.4 μ C/cm 2The Bi of these research preparations 4Ti 3O 12The residual polarization of film is all little, and coercive field is higher.To push ferroelectric material to industrial application, just must solve the low and coercive field problem of higher of above-mentioned residual polarization, therefore explore new preparation technology, thereby the ferroelectric properties of test material just become research Bi 4Ti 3O 12One step of thin-film material key.
Bi 4Ti 3O 12Thereby in some ionic mix and can change its structure and change its ferroelectric properties to a great extent.Prior theory and experimental study show: at Bi 4Ti 3O 12In mix a certain amount of rare earth ion and reduced the deformation of its structure with the Bi ion that replaces the A position, strengthened TiO 6Octahedral symmetry, its fatigue resistance and polarizability have obtained tangible improvement.But the increase of mixing and brought coercive field when residual polarization is improved in the A position.Guarantee to reduce coercive field when residual polarization increases, the doping of material being carried out the B position is feasible, but the degree of this reduction does not still also reach practical requirement.Therefore, by new approach to Bi 4Ti 3O 12A position or B position mix adjusting its lattice parameter, and the kind of definite dopant ion and quantity, thus improve Bi 4Ti 3O 12Ferroelectric properties is present Bi 4Ti 3O 12Application even commercialization problem demanding prompt solution.
Explore novel Bi 4Ti 3O 12The preparation technology of film is preparation Bi 4Ti 3O 12The basis of material, is the technique direction that have development potentiality with the self-assembly preparation that self-growing form is carried out nano material and device by the liquid phase reaction method under mild conditions, material in process of growth, its key is the growth position of accurate control material, obtains the nanostructure of high-sequential.Implement the self-assembly preparation and at first need to select suitable masterplate.In recent years, self-assembled monolayer is owing to receiving increasing concern in the shown great potential of the self-assembly preparation field of nano material and nanostructure.Tensio-active agent such as alkyl sulfur compounds, lipid acid, organosilane etc., mode that can be by self-assembly forms the unimolecular film (SAMs) of high-sequential at substrate surface, prepares with the micro-pattern that carries out nano material and nanostructure as masterplate.
Summary of the invention:
The present invention has reported employing liquid phase self-assembled monolayer membrane technique, utilizes (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, according to certain proportioning raw materials, under certain mode of deposition, has prepared film, obtains the bismuth titanate film of crystallization then through certain anneal.The advantage of this method is to have the spontaneous formation of original position, become that the key high-sequential is arranged, defective is few, bonding force is strong, be the preparation method of the bismuth titanate film of characteristics such as " crystal forms ".
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of method for preparing the bismuth titanates function film on glass substrate is provided, according to following steps:
(1) pre-treatment substrate: at first glass substrate is placed deionized water for ultrasonic ripple washing 10-15min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15-20min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain;
(2) deposition OTS self-assembly rete: substrate cleaned in the step (1) is carried out the deposition preparation of OTS self-assembly rete; At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution; After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s～20min, and this process is carried out in homemade atmosphere protection reactor, passes to nitrogen protection, prevents airborne moisture contamination and oxygenizement; Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then; Toast 5-10min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate;
(3) preparation reaction solution: with (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid of 0.0050-0.03mol/l, and wherein the mol ratio of Bi and Ti is 4: 3, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10;
(4) liquid phase method deposit film: the substrate after the OTS functionalization vertically is positioned in the precursor liquid that has configured, under different condition, carries out the depositing of thin film preparation respectively;
(5) post-processed of film: film is incubated 0.5-1h down at 550-650 ℃ carries out anneal, obtain the bismuth titanates function film.
Described step (1) is meant: at first glass substrate is placed deionized water for ultrasonic ripple washing 10min, 12.5min or 15min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15min, 17.5min or 20min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain.
Described step (2) is meant: deposition OTS self-assembly rete: substrate cleaned in the step (1) is carried out the deposition preparation of OTS self-assembly rete; At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution; After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s, 1min, 5min, 10min or 20min, and this process is carried out in homemade atmosphere protection reactor, pass to nitrogen protection, prevent airborne moisture contamination and oxygenizement; Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then; Toast 5min, 7.5min or 10min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate.
Described step (3) is meant: with (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid of 0.0050mol/l, 0.01mol/l or 0.03mol/l, and wherein the mol ratio of Bi and Ti is 4: 3, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10.Prepare Bi with liquid phase deposition 4Ti 3O 12Film is often wanted post-processed such as annealed further to improve the microtexture of film and is improved the performance of film.In the experiment, annealing schedule is that film is incubated 30min down at 550,600 and 650 ℃ respectively, to analyze annealing temperature to Bi 4Ti 3O 12The influence of film crystallization degree.
The present invention adopts liquid phase self-assembled monolayer membrane technique, down glass substrate is carried out sensitization ultraviolet equipment auxiliary and handles, and on the glass substrate of sensitization induced growth Bi 4Ti 3O 12Film is for Bi 4Ti 3O 12The preparation technology of film is a kind of brand-new trial, and this novel technology of preparing is a kind of innovation to synthesis technique itself not only, and can be to product B i 4Ti 3O 12The performance of film produces the influence of matter.The advantage of this method is to have the spontaneous formation of original position, become that the key high-sequential is arranged, defective is few, bonding force is strong, be the preparation method of the bismuth titanate film of characteristics such as " crystal forms ".
Description of drawings:
Fig. 1 is the Bi of preparation under the different precursor liquid pH values 4Ti 3O 12The X-Ray diffractogram of film.(a)1.20；(b)1.25；(c)1.30；(d)1.35；
The Bi of Fig. 2 for preparing under the different mode of deposition 4Ti 3O 12The X-Ray diffractogram of film.(a) 50 ℃ of deposition 4h; (b) 50 ℃ of deposition 6h; (c) 60 ℃ of deposition 4h; (d) 60 ℃ of deposition 6h;
The Bi of Fig. 3 for preparing under the different annealing temperature 4Ti 3O 12The X-Ray diffractogram of film.(a)550℃；(b)600℃；(c)650℃；
The Bi of preparation when Fig. 4 is different precursor liquid pH value 4Ti 3O 12The stereoscan photograph of film.(a)1.20；(b)1.25；(c)1.30；(d)1.35；
The Bi of Fig. 5 for preparing under the different mode of deposition 4Ti 3O 12The stereoscan photograph of film.(a) 50 ℃ of deposition 4h; (b) 50 ℃ of deposition 6h; (c) 60 ℃ of deposition 4h; (d) 60 ℃ of deposition 6h;
The Bi of Fig. 6 for preparing under the different annealing temperature 4Ti 3O 12The stereoscan photograph of film.(a)550℃；(b)600℃；(c)650℃。
Embodiment:
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail:
Embodiment 1:
1, Bi 4Ti 3O 12The preparation of film
1.1 with (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid (wherein the mol ratio of Bi and Ti is 4: 3) of 0.01mol/l, uses rare nitric acid titration precursor liquid again, obtains the pH value and is respectively 1.35,1.30,1.25 and 1.20 precursor liquid.
1.2 the substrate after the OTS functionalization vertically is positioned in the precursor liquid that has configured, under different conditions, carries out the depositing of thin film preparation respectively.
1.3 sample is placed 550,600 and 650 ℃ of insulation 30min down respectively.To improve Bi 4Ti 3O 12The crystallization degree of film.
Fig. 1 deposits the back and obtains through 600 ℃ of calcining 30min for substrate in different pH value precursor liquids Bi 4Ti 3O 12The film XRD figure.As can be seen from Figure 1, the pH value is 1.30 o'clock, and the bismuth titanate film of preparation is purer, and diffraction peak intensity is bigger.
The film of Fig. 2 for preparing under the different mode of deposition is as can be seen from the figure at 60 ℃ of deposit 6h gained Bi 4Ti 3O 12Main characteristic peak intensity higher, peak shape is comparatively sharp-pointed.
The film of Fig. 3 for preparing under the different annealing temperature, as can be seen from the figure along with the film annealing temperature raises, Bi 4Ti 3O 12The diffraction peak of each crystal face strengthens, the crystal grain zoon.。
The film morphology photo of preparation when Fig. 4 is different pH value, as can be seen from the figure the pH value is that 1.30 o'clock gained film compactness is higher, more even, and film surface grain size, shape basically identical.
Fig. 5 is the film morphology photo under the different mode of deposition, as can be seen from the figure when 60 ℃ of deposit 6h, has formed Bi fine and close, homogeneous at substrate surface 4Ti 3O 12Film, grain growing is obvious, and it is big that particle diameter becomes, and film quality obviously improves.
Fig. 6 is the film morphology photo under the different annealing temperature, as can be seen from the figure through 600 ℃ of annealed Bi 4Ti 3O 12Film is more even, does not have unusual oarse-grained deposition.
Comprehensive above-mentioned scanning electron microscope, X-Ray diffraction analysis show: when the pH of precursor liquid value is 1.30, mode of deposition is 60 ℃/6h, the film of preparing when annealing temperature is 600 ℃ is comparatively pure, and pattern is comparatively fine and close, even, and the growth of bismuth titanate film is more intact.
Embodiment 2:
1, patterning Bi 4Ti 3O 12The preparation of film
1.1, the pre-treatment of substrate
At first glass substrate is placed deionized water for ultrasonic ripple washing 10min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain.
1.2, the deposition of OTS self-assembly rete
After substrate is cleaned, carry out the deposition preparation of OTS self-assembly rete.At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution.After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s～20min, and this process is carried out in homemade atmosphere protection reactor, passes to nitrogen protection, prevents airborne moisture contamination and oxygenizement.Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then.Toast 5min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate.
The substrate surface that deposits OTS is covered photomask, and level is put into the uviolizing instrument, and the ultraviolet radiation ripple is 184.9nm, at 1 normal atmosphere, keeping irradiation distance is under the situation of 1cm, shines the different time respectively, obtains the OTS self-assembled monolayer of patterning; UV-irradiation makes the alkyl of OTS head base carry out the hydroxylation transformation under the optical excitation of UV-light simultaneously.
1.3, the preparation of reaction solution
With (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid (wherein the mol ratio of Bi and Ti is 4: 3) of 0.01mol/l, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10.
1.4, liquid phase method deposit film process
Substrate after the OTS functionalization vertically is positioned in the precursor liquid that has configured, under different condition, carries out the depositing of thin film preparation respectively.
1.5, the post-processed of film
Prepare Bi with liquid phase deposition 4Ti 3O 12Film is often wanted post-processed such as annealed further to improve the microtexture of film and is improved the performance of film.In the experiment, annealing schedule is that film is incubated 30min down at 550-650 ℃, to analyze annealing temperature to patterning Bi 4Ti 3O 12The influence of film crystallization degree.
Embodiment 3:
1, Bi 4Ti 3O 12The preparation of film (crystal pulling method)
1.1, the pre-treatment of substrate
At first glass substrate is placed deionized water for ultrasonic ripple washing 10min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain.
1.2, the deposition of OTS self-assembly rete
After substrate is cleaned, carry out the deposition preparation of OTS self-assembly rete.At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution.After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s～20min, and this process is carried out in homemade atmosphere protection reactor, passes to nitrogen protection, prevents airborne moisture contamination and oxygenizement.Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then.Toast 5min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate.
The substrate surface that deposits OTS is covered photomask, and level is put into the uviolizing instrument, and the ultraviolet radiation ripple is 184.9nm, at 1 normal atmosphere, keeping irradiation distance is under the situation of 1cm, shines the different time respectively, obtains the OTS self-assembled monolayer of patterning; UV-irradiation makes the alkyl of OTS head base carry out the hydroxylation transformation under the optical excitation of UV-light simultaneously.
1.3, the preparation of reaction solution
With (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid (wherein the mol ratio of Bi and Ti is 4: 3) of 0.01mol/l, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10.
1.4, the preparation Bi 4Ti 3O 12Film
With lifting thin films, pull rate is 1mm/min.
1.5, the post-processed of film
Prepare Bi with liquid phase deposition 4Ti 3O 12Film is often wanted post-processed such as annealed further to improve the microtexture of film and is improved the performance of film.In the experiment, annealing schedule is that film is incubated 30min down at 550-650 ℃, to analyze annealing temperature to Bi 4Ti 3O 12The influence of film crystallization degree.
Embodiment 4:
1, patterning Bi 4Ti 3O 12The preparation of film (crystal pulling method)
1.1, the pre-treatment of substrate
At first glass substrate is placed deionized water for ultrasonic ripple washing 10min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain.
1.2, the deposition of OTS self-assembly rete
After substrate is cleaned, carry out the deposition preparation of OTS self-assembly rete.At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution.After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s～20min, and this process is carried out in homemade atmosphere protection reactor, passes to nitrogen protection, prevents airborne moisture contamination and oxygenizement.Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then.Toast 5min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate.
The substrate level that deposits OTS is put into the uviolizing instrument, the ultraviolet radiation ripple is 184.9nm, and at 1 normal atmosphere, keeping irradiation distance is under the situation of 1cm, shine the different time respectively, make the alkyl of OTS head base under the optical excitation of UV-light, carry out the hydroxylation transformation.
1.3, the preparation of reaction solution
With (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid (wherein the mol ratio of Bi and Ti is 4: 3) of 0.01mol/l, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10.
1.4, the preparation Bi 4Ti 3O 12Film
With lifting thin films, pull rate is 1mm/min.
1.5, the post-processed of film
Prepare Bi with liquid phase deposition 4Ti 3O 12Film is often wanted post-processed such as annealed further to improve the microtexture of film and is improved the performance of film.In the experiment, annealing schedule is that film is incubated 30min down at 550-650 ℃, to analyze annealing temperature to patterning Bi 4Ti 3O 12The influence of film crystallization degree.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of being submitted to.

Claims (4)

1. a method for preparing the bismuth titanates function film on glass substrate is characterized in that, according to following steps:
(1) pre-treatment substrate: at first glass substrate is placed deionized water for ultrasonic ripple washing 10-15min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15-20min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain;
(2) deposition OTS self-assembly rete: substrate cleaned in the step (1) is carried out the deposition preparation of OTS self-assembly rete; At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution; After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s～20min, and this process is carried out in homemade atmosphere protection reactor, passes to nitrogen protection, prevents airborne moisture contamination and oxygenizement; Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then; Toast 5-10min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate;
(3) preparation reaction solution: with (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid of 0.0050-0.03mol/l, and wherein the mol ratio of Bi and Ti is 4: 3, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10;
(4) liquid phase method deposit film: the substrate after the OTS functionalization vertically is positioned in the precursor liquid that has configured, under different condition, carries out the depositing of thin film preparation respectively;
(5) post-processed of film: film is incubated 0.5-1h down at 550-650 ℃ carries out anneal, obtain the bismuth titanates function film.
2. a kind of according to claim 1 method that on glass substrate, prepares the bismuth titanates function film, it is characterized in that, described step (1) is meant: at first glass substrate is placed deionized water for ultrasonic ripple washing 10min, 12.5min or 15min, with the dust and the broken foam of glass of flush away substrate surface; Again with difference supersound washing 15min, 17.5min or 20min in dehydrated alcohol and the acetone, with flush away surface organic pollutant and oil stain.
3. a kind of according to claim 1 method for preparing the bismuth titanates function film on glass substrate is characterized in that, described step (2) is meant: deposition OTS self-assembly rete: substrate cleaned in the step (1) is carried out the deposition preparation of OTS self-assembly rete; At first octadecyl trichlorosilane and toluene are prepared OTS-toluene solution with volume fraction at 1: 99: under stirring condition, OTS is added drop-wise in the toluene solution; After then above-mentioned cleaned substrate nitrogen being dried up, put into the OTS-toluene solution, controlling reaction time is 30s, 1min, 5min, 10min or 20min, and this process is carried out in homemade atmosphere protection reactor, pass to nitrogen protection, prevent airborne moisture contamination and oxygenizement; Taking-up deposited the substrate of OTS, put into anhydrous propanone rapidly and carried out ultrasonic washing 5min, dried up with nitrogen then; Toast 5min, 7.5min or 10min down at 120 ℃ subsequently, discharge remained on surface solution, make OTS self-assembly rete combine tightr with substrate.
4. a kind of according to claim 1 method for preparing the bismuth titanates function film on glass substrate is characterized in that described step (3) is meant: with (NH 4) 2TiF 6And Bi (NO 3) 35H 2O is a raw material, and compound concentration is the precursor liquid of 0.0050mol/l, 0.0lmol/l or 0.03mol/l, and wherein the mol ratio of Bi and Ti is 4: 3, uses rare nitric acid titration precursor liquid again, obtains the precursor liquid of pH value for 1.40-1.10.
CN 201010287622 2010-09-20 2010-09-20 Method for preparing bismuth titanate functional membrane on glass substrate Pending CN101955323A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534610A (en) * 2012-02-24 2012-07-04 陕西科技大学 Method for depositing compact barium strontium titanate film on glass substrate
CN102557473A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing porous bismuth ferrate thin film by CSD (Chemical Solution Deposition) method
CN102557475A (en) * 2012-02-24 2012-07-11 陕西科技大学 Method for preparing functional film through reverse adsorption from bottom to top based on electrostatic attraction
CN103482691A (en) * 2013-09-04 2014-01-01 陕西科技大学 Doped Bi4Ti3O12 film and preparation method thereof
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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659520A (en) * 2009-09-17 2010-03-03 陕西科技大学 Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659520A (en) * 2009-09-17 2010-03-03 陕西科技大学 Method for preparing bismuth iron functional film on glass substrate by utilizing liquid-phase self-assembly method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《无机化学学报》 20090331 刘剑等 OTS自组装单层膜诱导定向生长SrTiO3功能陶瓷薄膜 517-521 1-4 第25卷, 第3期 2 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102557473A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing porous bismuth ferrate thin film by CSD (Chemical Solution Deposition) method
CN102534610A (en) * 2012-02-24 2012-07-04 陕西科技大学 Method for depositing compact barium strontium titanate film on glass substrate
CN102557475A (en) * 2012-02-24 2012-07-11 陕西科技大学 Method for preparing functional film through reverse adsorption from bottom to top based on electrostatic attraction
CN102557475B (en) * 2012-02-24 2014-06-04 陕西科技大学 Method for preparing functional film through reverse adsorption from bottom to top based on electrostatic attraction
CN103482691A (en) * 2013-09-04 2014-01-01 陕西科技大学 Doped Bi4Ti3O12 film and preparation method thereof
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

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