CN102557473A - Method for preparing porous bismuth ferrate thin film by CSD (Chemical Solution Deposition) method - Google Patents

Method for preparing porous bismuth ferrate thin film by CSD (Chemical Solution Deposition) method Download PDF

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CN102557473A
CN102557473A CN2011104449247A CN201110444924A CN102557473A CN 102557473 A CN102557473 A CN 102557473A CN 2011104449247 A CN2011104449247 A CN 2011104449247A CN 201110444924 A CN201110444924 A CN 201110444924A CN 102557473 A CN102557473 A CN 102557473A
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ito
glass substrate
thin film
csd
substrate surface
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谈国强
程蒙
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Shaanxi University of Science and Technology
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Abstract

The invention provides a method for preparing a porous bismuth ferrate thin film by a CSD (Chemical Solution Deposition) method. The method comprises the steps of: (1) cleaning an ITO (Indium Tin Oxide)/glass substrate, blow-drying with nitrogen gas, and irradiating with an ultraviolet illumination instrument for 20min; (2) respectively dissolving Fe(NO3)3.9H2O and Bi(NO3)3.5H2O in ethylene glycol monomethyl ether and glacial acetic acid, mixing to form a precursor solution, and magnetically stirring to obtain a stable BiFeO3 precursor; and (3) carrying out coating treatment on the substrate surface with the precursor, drying after coating is finished, repeating coating treatment multiple times to obtain set thin film thickness, finally rapidly heating to 350 DEG C, pre-annealing for 5min, and then annealing at 500 DEG C for 30-120min. The bismuth ferrate thin film prepared by the method is few in internal defects and high in catalysis performance.

Description

A kind of CSD legal system is equipped with the method for vesicular bismuth ferrite thin film
Technical field
The invention belongs to field of functional materials; Relate to a kind of chemical solution deposition (Chemical Solution Deposition; CSD) prepare the method for ferrous acid bismuth porous membrane; Utilize the characteristic that precursor can comparatively fast decompose in the CSD method to obtain the vesicular film,, thereby improve its photocatalysis performance through the pore increasing specific surface area.
Background technology
BiFeO 3Having the calcium titanium ore structure of tripartite distortion, is one of single-phase ferromagnetic electric material that has simultaneously under the minority room temperature ferroelectricity and magnetic, and two kinds of having simultaneously under the room temperature are structurally ordered, promptly ferroelectric (T in order C=810 ℃) and G type antiferromagnetic order (T N=380 ℃), make it become one of important candidate material of magnetoelectric material.While BiFeO 3Can also be as a kind of photocatalyst, because BiFeO 3Have narrower energy gap (2.2eV), have high photosensitivity and carrier mobility, the effective degradable organic pollutant of ability under the visible light effect will be so it will have potential application in photocatalysis field.
Be used to prepare BiFeO at present 3The method of film has a lot, like sol-gel (Sol-Gel) method, chemical vapor deposition (CVD) method, magnetron sputtering (rf magnetron sputtering) method, metallorganics deposit (MOD) method, metal organic chemical vapor deposition (MOCVD) method, liquid phase deposition (LPD), molecular beam epitaxy (MBE) method and pulsed laser deposition (PLD) method etc.The CSD method; Be chemical solution deposition, presoma is dissolved in presoma in organic solvent or the water according to certain ratio, through obtaining stable solution state; Precursor exists with ionic species; Through super-dry, remove organic composition and moisture and can obtain amorphous film, and annealed crystallization obtains crystalline film.This method equipment is cheap, simple to operate, and does not need exacting terms such as high temperature, vacuum, and raw material consumption is less, is easy to control, and film forming is even and matter crystal internal defect is few.
The major influence factors of ferrous acid bismuth material light catalysis property is the defective of crystals.Too much defective also possibly become the deathnium of electrons/and reduce reactive behavior, and defective is mainly because ferrous acid bismuth material exists factors such as oxygen room, stoichiometric ratio is unbalance to cause.Adopt the CSD method among the present invention, film is crystallization more easily, and without the chemical reaction process of hydrolytie polycondensation, lattice defect can reduce significantly, thereby can improve the catalytic performance of film.
The present invention has adopted the CSD legal system to be equipped with bismuth ferrite thin film, owing to without hydrolysis condensation reaction, the sol-gel legal system can not occur and be equipped with BiFeO 3Shrink that takes place during film or acetal reaction; Organism be easy to remove and not again the surface of film stay defectives such as bubble; Can not introduce defective simultaneously yet, therefore can make bismuth ferrite thin film rapid drying obtain cavernous pure phase bismuth ferric film, increase the specific surface area of film because of the hydrolysis of precursor; Through the improvement of specific surface area, improve the photocatalysis performance of film.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of CSD legal system is equipped with the vesicular bismuth ferrite thin film; This method is through simple CSD method; Prepare the less vesicular bismuth ferrite thin film of subsurface defect, through to unified control, the pattern of instrumentality phase composite, film and pore.Increase the specific surface area of film mutually through pore, improve catalytic performance.
For realizing above-mentioned purpose, the invention provides the method that a kind of CSD legal system is equipped with ferrous acid bismuth porous membrane, may further comprise the steps:
Step 1: selecting the ITO/glass substrate for use is substrate, after the ITO/glass substrate of well cutting is cleaned up, dries up with nitrogen;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ";
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.01～1.0mol/L in the adjusting precursor liquid, and magnetic agitation obtains stable BiFeO 3Presoma.
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Behind the even glued bundle, drying repeats even glue processing and obtains setting film thickness several times; The 350 ℃ of preannealing 5min that are rapidly heated at last are then at 500 ℃ of annealing 30～120min.
In said step 1, be to the ITO/glass substrate cleaning step of well cutting: place washing composition, acetone, ethanol ultrasonic cleaning successively, removing the impurity of ITO/glass substrate surface, after each ultrasonic cleaning with a large amount of distilled water flushing substrates;
In said step 4, even glue speed is 3000～6000r/min.
The method that CSD legal system of the present invention is equipped with ferrous acid bismuth porous membrane has the following advantages at least: the present invention is through simple technology; Require lower experiment condition; Obtain even compact, the less vesicular pure phase bismuth ferric film of defective; And utilize its bigger specific surface area, the photocatalysis performance of enhancement film.Can be through the concentration of control precursor liquid, the pattern and the pore of control film.
Description of drawings
Fig. 1 is the XRD figure of bismuth ferrite thin film of the present invention;
Fig. 2 is the SEM figure of bismuth ferrite thin film of the present invention.
Embodiment
Embodiment 1
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate after step 1 processing; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.01～1.0mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 3000～6000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 30min.
Embodiment 2
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate after step 1 processing; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.01mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 3000～4000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 60min.
Embodiment 3
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate after step 1 processing; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.1mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 4000～6000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 120min.
Embodiment 4
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate of cleaning; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.5mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 3000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 30min.
Embodiment 5
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate after step 1 processing; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.7mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 5000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 80min.
Embodiment 6
Step 1: selecting the ITO/glass substrate for use is substrate; The ITO/glass substrate of well cutting is placed washing composition, acetone, ethanol ultrasonic cleaning successively; Remove the impurity such as grease of ITO/glass substrate surface; With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic cleaning;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate after step 1 processing; Make substrate surface reach " atomic cleanliness degree "; The high-energy of uv irradiating can make oxide compound bond rupture wherein, forms wetting ability hydroxyl preferably, improves the wetting ability of substrate;
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 1.0mol/L in the adjusting precursor liquid, and magnetic agitation 0.5h obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Wherein even glue speed is 6000r/min; Behind the even glued bundle, then 60 ℃ of dryings, after repeating even glue and obtaining demand thickness several times; Be rapidly heated to 350 ℃ of preannealing 5min, at 500 ℃ of annealing 100min.
Thing phase composite structure with the XRD determining powder; Measure the microscopic appearance of powder with SEM; Its result is as depicted in figs. 1 and 2, therefrom can know, sol-gel method prepares the film that the new annealing way of ferrous acid bismuth multiferroic film obtains and has the distortion calcium titanium ore structure; Pure do not have impurity mutually, and pore is evenly distributed on the surface of film mutually.
The above is merely one embodiment of the present invention; It or not whole or unique embodiment; The conversion of any equivalence that those of ordinary skills take technical scheme of the present invention through reading specification sheets of the present invention is claim of the present invention and contains.

Claims (3)

1. a CSD legal system is equipped with the method for vesicular bismuth ferrite thin film, it is characterized in that: may further comprise the steps:
Step 1: selecting the ITO/glass substrate for use is substrate, after the ITO/glass substrate of well cutting is cleaned up, dries up with nitrogen;
Step 2: place ultraviolet radiation instrument to shine 20min the ITO/glass substrate of cleaning, make substrate surface reach " atomic cleanliness degree ";
Step 3: with Fe (NO 3) 39H 2O and Bi (NO 3) 35H 2O is dissolved in respectively in EGME and the Glacial acetic acid min. 99.5, and the formation precursor liquid is mixed in the dissolving back, and Bi, Fe ionic concn are 0.01～1.0mol/L in the adjusting precursor liquid, and magnetic agitation obtains stable BiFeO 3Presoma;
Step 4: the presoma that the substrate surface after step 2 is handled obtains with step 3 is spared glue and is handled; Behind the even glued bundle, drying repeats even glue processing and obtains setting film thickness several times; The 350 ℃ of preannealing 5min that are rapidly heated at last are then at 500 ℃ of annealing 30～120min.
2. a kind of CSD legal system as claimed in claim 1 is equipped with the method for vesicular bismuth ferrite thin film; It is characterized in that; In step 1; ITO/glass substrate cleaning step to well cutting is: place washing composition, acetone, ethanol ultrasonic cleaning successively, removing the impurity of ITO/glass substrate surface, after each ultrasonic cleaning with a large amount of distilled water flushing substrates.
3. be equipped with the method for vesicular bismuth ferrite thin film like a kind of CSD legal system as claimed in claim 1, it is characterized in that, in said step 4, even glue speed is 3000～6000r/min.
CN2011104449247A 2011-12-19 2011-12-19 Method for preparing porous bismuth ferrate thin film by CSD (Chemical Solution Deposition) method Pending CN102557473A (en)

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CN103723770A (en) * 2013-12-20 2014-04-16 陕西科技大学 High-dielectric-constant Bi0.92Ho0.08Fe[1-x]MnxO3 ferroelectric film and preparation method thereof
CN103771527A (en) * 2013-12-20 2014-05-07 陕西科技大学 Bi0.92Dy0.08Fe(1-x)MnxO3 ferroelectric film with low coercive field and preparation method of film
CN106892481A (en) * 2017-02-24 2017-06-27 江苏维尔利环保科技股份有限公司 Magnetic coupling algicide and its application method
CN107604408A (en) * 2017-08-25 2018-01-19 洛阳师范学院 A kind of bismuth ferrite thin film and preparation method thereof
CN108441957A (en) * 2017-12-08 2018-08-24 新疆大学 A kind of preparation method of bismuth ferrite photocatalysis film
CN115432738A (en) * 2022-09-05 2022-12-06 南京理工大学 BiFeO for depositing amorphous layer 3 Film and method for producing same

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CN103663564A (en) * 2013-12-20 2014-03-26 陕西科技大学 Bi0.90Dy0.10Fe1-XMnxO3 ferroelectric film with high dielectric constant, and preparation method for Bi0.90Dy0.10Fe1-XMnxO3 ferroelectric film with high dielectric constant
CN103723770A (en) * 2013-12-20 2014-04-16 陕西科技大学 High-dielectric-constant Bi0.92Ho0.08Fe[1-x]MnxO3 ferroelectric film and preparation method thereof
CN103771527A (en) * 2013-12-20 2014-05-07 陕西科技大学 Bi0.92Dy0.08Fe(1-x)MnxO3 ferroelectric film with low coercive field and preparation method of film
CN103663564B (en) * 2013-12-20 2015-07-01 陕西科技大学 Bi0.90Dy0.10Fe1-XMnxO3 ferroelectric film with high dielectric constant, and preparation method for Bi0.90Dy0.10Fe1-XMnxO3 ferroelectric film with high dielectric constant
CN103723770B (en) * 2013-12-20 2015-07-15 陕西科技大学 High-dielectric-constant Bi0.92Ho0.08Fe[1-x]MnxO3 ferroelectric film and preparation method thereof
CN103771527B (en) * 2013-12-20 2015-08-12 陕西科技大学 A kind of Bi of low coercive field 0.92dy 0.08fe 1-xmn xo 3ferroelectric membranc and preparation method thereof
CN106892481A (en) * 2017-02-24 2017-06-27 江苏维尔利环保科技股份有限公司 Magnetic coupling algicide and its application method
CN107604408A (en) * 2017-08-25 2018-01-19 洛阳师范学院 A kind of bismuth ferrite thin film and preparation method thereof
CN107604408B (en) * 2017-08-25 2019-11-08 洛阳师范学院 A kind of bismuth ferrite thin film and preparation method thereof
CN108441957A (en) * 2017-12-08 2018-08-24 新疆大学 A kind of preparation method of bismuth ferrite photocatalysis film
CN115432738A (en) * 2022-09-05 2022-12-06 南京理工大学 BiFeO for depositing amorphous layer 3 Film and method for producing same

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Application publication date: 20120711