CN102557475B - Method for preparing functional film through reverse adsorption from bottom to top based on electrostatic attraction - Google Patents
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- CN102557475B CN102557475B CN201210044213.5A CN201210044213A CN102557475B CN 102557475 B CN102557475 B CN 102557475B CN 201210044213 A CN201210044213 A CN 201210044213A CN 102557475 B CN102557475 B CN 102557475B
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Abstract
The invention discloses a method for preparing a functional film through reverse adsorption from bottom to top based on electrostatic attraction. The method comprises the following steps of: suspending one functional side of a substrate on the surface of a solution downwards, reversely adsorbing complexing ions in the solution on the substrate through the electrostatic attraction from bottom to top to prepare a film, drying at room temperature, and annealing to obtain a crystallized functional film. Self-assembled octadecyltrichlorosilane (OTS) monolayers (OTS-SAMs) are taken as a template and subjected to surface modification by a short-wave ultraviolet irradiation instrument, a liquid phase deposition method is combined, and a simple and economic method is designed by a technology of reverse adsorption from bottom to top based on the electrostatic attraction; the influence of gravity is eliminated by the reverse adsorption technology, large particles and complexing ions are deposited downwards, small complexing ions are adsorbed on the substrate upwards under the action of the electrostatic attraction, and the film prepared by the method has a flat and uniform surface; and when reverse adsorption achieves balance and the ions are not adsorbed, the thickness of the prepared film is high in controllability.
Description
[technical field]
The invention belongs to field of functional materials, relate to a kind of based on electrostatic attraction from bottom to top reverse adsorption method prepare the method for function film.
[background technology]
Ferromagnetic electric material is a kind of material that causes ferroelectricity and magnetic to coexist because electromagnetism is orderly and have magneto-electric coupled character.Coexisting of ferroelectricity and magnetic makes this material to produce magnetization M by electric field E induction, and magnetic field H also can be brought out iron electric polarization P simultaneously, and this character is called as magnetoelectric effect ME (Magnetoelectric effect).BiFeO
3(BFO) be one of minority material at room temperature simultaneously with ferroelectricity and magnetic, it has triangle distortion perovskite structure, BFO long-range electricity in order and long-range magnetic order make it there is ferroelectricity and antiferromagnetism simultaneously, the two characteristic coexisting provides solid theoretical basis and important realistic meaning for development of new memory device.
At present for BiFeO
3the preparation method of film mainly contains pulsed laser deposition, magnetron sputtering method etc.Its advantage of pulsed laser deposition is to reduce base reservoir temperature, can keep good stoichiometric ratio, film quality good (density is high), adhesion property are strong, the film of the complicated component that is suitable for growing, and need tackle the major problem is how to obtain large area uniform film.Sputtering method can big area film forming, and film quality is high, but the speed of growth is slow, and microstructure and the composition homogeneity of film are held improvement.Above these preparation technology's equipment comparatively complicated, need strict vacuum environment and process system, cost costliness, and a small amount of impurity often containing is difficult to remove and can not get pure phase, as Bi
2fe
4o
9and Bi
25feO
40.Chemical liquid deposition method is a kind of wet chemical method, and it does not need expensive device, is suitable for big area and prepares film, is widely used in synthetic various functional materialss, and has obtained huge success.
Self-assembled monolayer (self-assembled monolayers) technology (being called for short SAMs technology) is the core technology of bionical synthesis technique, it is by producing chemisorption between an activity base of tensio-active agent and substrate, the orderly molecule assembled layers of spontaneous formation on interface.Utilize at present SAMs technology can be in the substrates such as metal, silicon single crystal, pottery from top to bottom forward Absorption Growth go out multiple inorganics film, comprise FeOOH, SnO
2, CdS, TiO
2, CdSe, SrTiO
3, ZrO
2, V
2o
5, Y
2o
3with multiple inorganic ceramic films such as ZnO.Prepare BiFeO for self-assembling technique
3film, is all that substrate is put in solution bottom, prepares BiFeO by gravity and adsorptive power
3film, not only prepares BiFeO
3a little less than film and substrate junction are made a concerted effort, and owing to being subject to the impact of gravity, some larger particles also can deposit on substrate, make the planeness of prepared film surface and homogeneity poor, film in uneven thickness and uncontrollable, has directly caused adopting prepared in this way BiFeO
3film leakage conductance is large especially, and dielectric and ferroelectric properties cannot be measured.
[summary of the invention]
The object of the present invention is to provide a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, it can prepare surfacing densification, does not have macrobead to occur and the controlled function film of thickness.
To achieve these goals, the present invention adopts following technical scheme:
A kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, functional substrateization one is faced down and is suspended in solution surface, complexing ion reverse adsorption in solution is prepared to film to substrate from bottom to top by electrostatic attraction, prepare the function film of crystallization at drying at room temperature after annealing.
The present invention further improves and is: in functional substrateization one side, be formed with one deck self-assembled monolayer.
The present invention further improves and is: the method for functional substrate is: substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min; Under UV-light, irradiate after 20min, in OTS-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism; Finally under UV-light, irradiate 40min, obtain the substrate of functionalization; In OTS-toluene solution, the volumetric concentration of OTS is 1%.
The present invention further improves and is: in solution, complexing ion is ironic citrate and bismuth citrate.
The present invention further improves and is: solution is Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2the mixing solutions of O, Glacial acetic acid, citric acid and distilled water composition.
The present invention further improves and is: in described solution, Glacial acetic acid is pH value conditioning agent, and citric acid is complexing agent.
The present invention further improves and is: Bi (NO in described solution
3)
35H
2o concentration is 0.01mol/L, Fe (NO
3)
39H
2o concentration is 0.01～0.045mol/L, and the volumetric concentration of Glacial acetic acid is 2%, and citric acid concentration is 0.02mol/L.
The present invention further improves and is: functional substrateization one is faced down and is suspended in solution surface, at the temperature of 60 DEG C～90 DEG C, complexing ion reverse adsorption in solution is prepared to film to substrate from bottom to top by electrostatic attraction, depositing time is 6h～30h; After drying at room temperature, 550 DEG C of annealing 10min～120min prepare the function film of crystallization.
To achieve these goals, the present invention can also adopt following technical scheme:
Based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, comprise the following steps:
Step 1: the configuration of precursor liquid: take 0.970g Bi (NO
3)
35H
2o, 2.101g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml; Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until the precursor liquid of solution clarification;
Step 2: the functionalization of substrate: FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min; Then under UV-light, irradiate after 20min, in OTS-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism; Finally under UV-light, irradiate 40min, obtain the substrate of functionalization; In OTS-toluene solution, the volumetric concentration of OTS is 1%.
Step 3: the deposition of film: face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction by the ironic citrate in precursor liquid and bismuth citrate, reverse adsorption, to substrate surface, is prepared noncrystalline membrane at 70 DEG C of deposition 20h from bottom to top;
Step 4: the crystallization of film: prepared noncrystalline membrane is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 10min.
With respect to prior art, the present invention adopts following technical scheme: the present invention is taking self-assembly octadecyl trichlorosilane alkane (OTS) unitary film as template, radiothermy UV-light (λ=184.9nm) radiation instrument carries out surface modification to OTS-SAMs, in conjunction with liquid phase deposition, and adopt based on electrostatic attraction reverse adsorption technical project from bottom to top a kind of simple, the economic method of technique.Adopt reverse adsorption technology to overcome the impact of gravity, some macrobeads and complexing ion will deposit downwards, and little complexing ion will upwards be adsorbed onto on substrate under the effect of electrostatic attraction, and the prepared film surface of this method is smooth evenly.And adsorbed ion no longer after reverse adsorption reaches balance, the thickness of prepared film has good controllability.This novel technology of preparing not only to liquid phase self-assembly to prepare function ceramics film itself be a kind of innovation and supplement, and the BiFeO that can prepare liquid phase self-assembly
3the performance of film produces the impact of matter.
The invention has the beneficial effects as follows by simple technique, equipment, require lower experiment condition, obtain the controlled film of even compact, surfacing and thickness.
[brief description of the drawings]
Fig. 1 is the XRD figure that reverse adsorption is prepared bismuth ferrite thin film from bottom to top.
Fig. 2 a is the SEM figure that reverse adsorption is prepared bismuth ferrite thin film from bottom to top, and Fig. 2 b is the SEM figure that forward deposition is prepared bismuth ferrite thin film from top to bottom.
Fig. 3 is the section SEM figure that reverse adsorption is prepared bismuth ferrite thin film from bottom to top.
[embodiment]
Embodiment 1 (reverse adsorption):
The present invention a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, technical process is as follows:
Step 1: the configuration of precursor liquid.Take 0.970g Bi (NO
3)
35H
2o, 2.101g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml.Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until solution clarification.
Step 2: the functionalization of substrate.FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min.Under UV-light, irradiate after 20min, in OTS (1vol%)-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism.Finally under UV-light, irradiate 40min, obtain the substrate of functionalization.
Step 3: the deposition of film.Face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction, by the complex compound-ironic citrate in solution and bismuth citrate, reverse adsorption is to substrate surface from bottom to top.Prepare noncrystalline membrane at 70 DEG C of deposition 20h.
Step 4: the crystallization of film.Prepared film is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 10min.
Step 5: the sign of film.Characterize the thing phase composite of film with XRD, characterize surface and the cross-section morphology of film with SEM.
Embodiment 2 (reverse adsorption):
The present invention a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, technical process is as follows:
Step 1: the configuration of precursor liquid.Take 0.970g Bi (NO
3)
35H
2o, 0.808g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml.Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until solution clarification.
Step 2: the functionalization of substrate.FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min.Under UV-light, irradiate after 20min, in OTS (1vol%)-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism.Finally under UV-light, irradiate 40min, obtain the substrate of functionalization.
Step 3: the deposition of film.Face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction, by the complex compound-ironic citrate in solution and bismuth citrate, reverse adsorption is to substrate surface from bottom to top.Prepare noncrystalline membrane at 60 DEG C of deposition 25h.
Step 4: the crystallization of film.Prepared film is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 120min.
Embodiment 3 (reverse adsorption):
The present invention a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, technical process is as follows:
Step 1: the configuration of precursor liquid.Take 0.970g Bi (NO
3)
35H
2o, 1.616g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml.Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until solution clarification.
Step 2: the functionalization of substrate.FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min.Under UV-light, irradiate after 20min, in OTS (1vol%)-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism.Finally under UV-light, irradiate 40min, obtain the substrate of functionalization.
Step 3: the deposition of film.Face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction, by the complex compound-ironic citrate in solution and bismuth citrate, reverse adsorption is to substrate surface from bottom to top.Prepare noncrystalline membrane at 90 DEG C of deposition 6h.
Step 4: the crystallization of film.Prepared film is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 100min.
Embodiment 4 (reverse adsorption):
The present invention a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, technical process is as follows:
Step 1: the configuration of precursor liquid.Take 0.970g Bi (NO
3)
35H
2o, 3.636g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml.Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until solution clarification.
Step 2: the functionalization of substrate.FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min.Under UV-light, irradiate after 20min, in OTS (1vol%)-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism.Finally under UV-light, irradiate 40min, obtain the substrate of functionalization.
Step 3: the deposition of film.Face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction, by the complex compound-ironic citrate in solution and bismuth citrate, reverse adsorption is to substrate surface from bottom to top.Prepare noncrystalline membrane at 75 DEG C of deposition 15h.
Step 4: the crystallization of film.Prepared film is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 50min.
Embodiment 5 (forward deposition):
Step 1: the configuration of precursor liquid.Take 0.970g Bi (NO
3)
35H
2o, 2.101g Fe (NO
3)
39H
2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml.Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until solution clarification.
Step 2: the functionalization of substrate.Substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min.Under UV-light, irradiate after 20min, in OTS (1vol%)-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism.Finally under UV-light, irradiate 40min, obtain the substrate of functionalization.
Step 3: the deposition of film.Face up and be placed in precursor liquid bottom one of functional substrate, prepare noncrystalline membrane by the 70 DEG C of deposition 20h that act on of adsorptive power and gravity.
Step 4: the crystallization of film.Prepared film is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 10min.
Step 5: the sign of film.Characterize the thing phase composite of film with XRD, characterize surface and the cross-section morphology of film with SEM.
Specific experiment result:
Refer to shown in Fig. 1 to Fig. 3, through the thing phase composite structure of XRD determining film, known after the microscopic appearance of SEM mensuration film and cross-section morphology, the perovskite structure that is typical distortion by the prepared bismuth ferrite thin film of embodiment 1 reverse adsorption, the smooth densification of film surface, film does not have pore phase, and is combined with substrate closely; Grain-size is approximately 100nm.Wherein, in Fig. 3, thick 320nm layer is FTO conducting film; 40nm layer be based on electrostatic attraction from bottom to top reverse adsorption prepare function film.
The present invention a kind of based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, the method feature is taking functionalization self-assembled monolayer as template, at a certain temperature functional substrateization one being faced down is suspended in solution surface and prepares film by reverse adsorption, prepares the ultra-thin function film of crystallization at drying at room temperature after annealing.Than traditional forward deposition, reverse adsorption is adsorbed in substrate by particle and is formed chemical bond by electrostatic attraction and is firmly incorporated into substrate surface, and when granule for absorbing, its adsorption rate is less, prepared film and substrate junction make a concerted effort strong and surfacing, homogeneous, there is no oarse-grained appearance, and there is good controllability because the existence of adsorption equilibrium makes prepared film thickness.The present invention is to prepare bismuth ferrite function film as example, with Bi (NO
3)
35H
2o, Fe (NO
3)
39H
2o is that raw material is dissolved in distilled water, with Glacial acetic acid regulator solution pH value, taking citric acid as complexing agent, using FTO glass substrate as substrate, preparing unitary film by self-assembly is thereon template, making at a certain temperature functional substrateization one to be faced down after its functionalization by UV-irradiation is suspended in solution surface and prepares film by reverse adsorption, after drying at room temperature in 300 DEG C of insulation 10min to remove organism, prepare the bismuth ferrite function film of crystallization at 550 DEG C of insulation annealings.Employing reactant concn is: Bi (NO
3)
35H
2o concentration is 0.01mol/L, Fe (NO
3)
39H
2o concentration is 0.01～0.045mol/L, and Glacial acetic acid add-on is 2vol%, and citric acid concentration is 0.02mol/L.Adopting depositing temperature is 60 DEG C～90 DEG C, and employing depositing time is 6h～30h, and adopting annealing temperature is 550 DEG C, and employing annealing time is 10min～120min.Adopt the prepared smooth densification of film surface of the method, there is no oarse-grained appearance, and the method is simple to operation.
In step 3 of the present invention, what adsorb by reverse electrostatic attraction is all less complex compound, and adsorption rate is less, is conducive to the control to film morphology.And due to the existence of adsorption equilibrium, there is a maximum value in adsorptive capacity, makes the thickness of prepared film have good controllability.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skill in the art take technical solution of the present invention by reading specification sheets of the present invention, is claim of the present invention and contains.
Claims (2)
- One kind based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, it is characterized in that, functional substrateization one is faced down and is suspended in solution surface, at the temperature of 60 DEG C～90 DEG C, complexing ion reverse adsorption in solution is prepared to film to substrate from bottom to top by electrostatic attraction, depositing time is 6h～30h; After drying at room temperature, 550 DEG C of annealing 10min～120min prepare the function film of crystallization;In functional substrateization one side, be formed with one deck self-assembled monolayer;The method of functional substrate is: substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min; Under UV-light, irradiate after 20min, in OTS-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism; Finally under UV-light, irradiate 40min, obtain the substrate of functionalization; In OTS-toluene solution, the volumetric concentration of OTS is 1%;In solution, complexing ion is ironic citrate and bismuth citrate;Solution is Bi (NO 3) 35H 2o, Fe (NO 3) 39H 2the mixing solutions of O, Glacial acetic acid, citric acid and distilled water composition;In described solution, Glacial acetic acid is pH value conditioning agent, and citric acid is complexing agent;Bi (NO in described solution 3) 35H 2o concentration is 0.01mol/L, Fe (NO 3) 39H 2o concentration is 0.01～0.045m ol/L, the volumetric concentration of Glacial acetic acid is 2%, citric acid concentration is 0.02m ol/L.
- Based on electrostatic attraction from bottom to top reverse adsorption prepare the method for function film, it is characterized in that, comprise the following steps:Step 1: the configuration of precursor liquid: take 0.970g Bi (NO 3) 35H 2o, 2.101g Fe (NO 3) 39H 2o, measures 4ml Glacial acetic acid, is dissolved in distilled water and is configured to the solution of 200ml; Stirring at room temperature, to clarification completely, adds 0.841g citric acid, continues stirring at room temperature until the precursor liquid of solution clarification;Step 2: the functionalization of substrate: FTO glass substrate is placed in respectively to deionized water, acetone, dehydrated alcohol supersound washing 10min; Then under UV-light, irradiate after 20min, in OTS-toluene solution, soak 30min and prepare OTS unitary film, in 120 DEG C of dry 5min with remove organism; Finally under UV-light, irradiate 40min, obtain the substrate of functionalization; In OTS-toluene solution, the volumetric concentration of OTS is 1%;Step 3: the deposition of film: face down and be suspended in precursor liquid surface one of functional substrate, by electrostatic attraction by the ironic citrate in precursor liquid and bismuth citrate, reverse adsorption, to substrate surface, is prepared noncrystalline membrane at 70 DEG C of deposition 20h from bottom to top;Step 4: the crystallization of film: prepared noncrystalline membrane is put into retort furnace after drying at room temperature, to remove organism, obtain the film of crystallization in 300 DEG C of insulation 10min in 550 DEG C of insulation annealing 10min.
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| CN105859273B (en) * | 2016-03-29 | 2019-07-30 | 陕西科技大学 | A kind of 2-2 type BiFeO3-CuFe2O4 laminated film and preparation method thereof |
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| CN1546241A (en) * | 2003-12-05 | 2004-11-17 | 武汉理工大学 | Processes and apparatus for preparing ionic self-assembly films |
| CN101955323A (en) * | 2010-09-20 | 2011-01-26 | 陕西科技大学 | Method for preparing bismuth titanate functional membrane on glass substrate |
| CN102163486A (en) * | 2010-12-30 | 2011-08-24 | 陕西科技大学 | Photoethcing self assembly preparation method of patterned BiFeO3 film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546241A (en) * | 2003-12-05 | 2004-11-17 | 武汉理工大学 | Processes and apparatus for preparing ionic self-assembly films |
| CN101955323A (en) * | 2010-09-20 | 2011-01-26 | 陕西科技大学 | Method for preparing bismuth titanate functional membrane on glass substrate |
| CN102163486A (en) * | 2010-12-30 | 2011-08-24 | 陕西科技大学 | Photoethcing self assembly preparation method of patterned BiFeO3 film |
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