CN102163486A - Photoethcing self assembly preparation method of patterned BiFeO3 film - Google Patents
Photoethcing self assembly preparation method of patterned BiFeO3 film Download PDFInfo
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- CN102163486A CN102163486A CN2010106157501A CN201010615750A CN102163486A CN 102163486 A CN102163486 A CN 102163486A CN 2010106157501 A CN2010106157501 A CN 2010106157501A CN 201010615750 A CN201010615750 A CN 201010615750A CN 102163486 A CN102163486 A CN 102163486A
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Abstract
The invention discloses a photoethcing self assembly preparation method of a patterned BiFeO3 film. The method comprises the following steps: (1) selecting a common slide glass as a substrate, cutting the glass substrate, performing ultrasonic cleaning, drying, and irradiation in an ultraviolet light irradiation instrument, respectively; (2) immersing the glass substrate irradiated by ultraviolet light in OTS-toluene solution to form an OTS monomolecular film on the surface of the substrate, after the immersing, cleaning the substrate with acetone, blow-drying, stoving, irradiating the substrate, with a photomask covering thereon, under ultraviolet light to obtain a patterned functional self-assembled film; (3) preparing BiFeO3 precursor solution, placing an OTS-SAMs matrix of the patterned functional self-assembled film in the prepared precursor solution, performing deposition, supersonic wave concussion cleaning and annealing to obtain the photoetching self-assembled patterned BiFeO3 film. The method provided by the invention combines liquid phase deposition method and photoetching self-assembled monolayers technology to obtain the patterned BiFeO3 film. The film has the following advantages: the edge contour is clear, and the film is firmly bonded to the substrate.
Description
Technical field
The present invention relates to a kind of Magnetic Sensor and electric capacity-inductor integrated device BiFeO
3Film, particularly a kind of patterning BiFeO
3The photoetching self-assembly preparation method thereof of film.
Background technology
In recent years, a kind of novel ferromagnetic electric material BiFeO
3Caused the great interest of people.BiFeO
3Having the perovskite structure of tripartite distortion, is one of single-phase ferromagnetic electric material that has simultaneously under the minority room temperature ferroelectricity and magnetic.It can produce magnetic field by electric field, and electric polarization also can be brought out in magnetic field simultaneously, and this character is called as magnetoelectric effect.This magnetic and electricity be controlled at information stores, spin electric device aspect mutually, all there is extremely important application prospect Magnetic Sensor and electric capacity-aspects such as inductor integrated device.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.
The patterned surface technology is meant and is generating nanoscale or micron-sized regular surfaces structure on the one dimension direction at least that it all has important scientific meaning and using value at aspects such as supermolecule science, materialogy, microelectronics and cell biologies.Therefore, little processing of structure and character or be patterned to center on micron and the nanoscale into contemporary science and technology, at microelectronic, people have begun the patterned surface material is used as the high density magnetic-based storage media.And BiFeO
3Material is as important ferromagnetic electric material, and its patterning preparation has potential using value.Photoetching technique is a kind of patterning techniques that is widely used, and at modern manufacturing industry, is especially bringing into play irreplaceable effect in the large scale integrated circuit manufacturing.
Self-assembled monolayer (self-assembled monolayers) technology (being called for short the SAMs technology) is the core technology of bionical synthesis technique, it is by producing chemisorbed between an activity base of surfactant and the substrate, the orderly molecule assembled layers of spontaneous formation on the interface.Because to be that organic molecule (perhaps organic molecule steam) in solution is spontaneous be adsorbed on formed ultra-thin organic membrane on the solid substrate by chemical bond to SAMs securely, so it has the spontaneous formation of original position, becomes that the key high-sequential is arranged, defective is few, adhesion is strong, be characteristics such as " crystalline states ".
Be used to prepare BiFeO at present
3The method of film has a lot, as sol-gel (Sol-Gel) method, chemical vapor deposition (CVD) method, magnetron sputtering (rf magnetron sputtering) method, metallorganic 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.Prepare BiFeO for adopting liquid phase deposition to combine with the photoetching self-assembling technique
3The research report of patterned film yet there are no, therefore the value that gets a good eye.
Summary of the invention
The purpose of this invention is to provide a kind of patterning BiFeO
3The photoetching self-assembly preparation method thereof of film, this method prepares BiFeO by adopting liquid phase deposition to combine with the photoetching self-assembling technique
3Patterned film, by this method can prepare edge contour clear, combine firm patterning BiFeO with substrate
3Film.
The objective of the invention is to realize by following technical proposals.
A kind of patterning BiFeO
3The photoetching self-assembly preparation method thereof of film, the concrete preparation process of this method is as follows:
(1) selecting common slide for use is substrate, and glass substrate is cut into the rectangle of 20mm * 10mm, and ultrasonic waves for cleaning is respectively removed the impurity such as grease of Si substrate surface, with a large amount of distilled water flushing substrates, dries up after each ultrasonic waves for cleaning; And place ultraviolet radiation instrument to shine 10-20min the clean glass substrate;
(2) glass substrate after UV-irradiation is placed concentration of volume percent 1% octadecyl trichlorosilane (OTS)-toluene solution, soak 20-40min at ambient temperature, make substrate surface form one deck OTS monomolecular film; Clean 2-3min with acetone after immersion is finished, and dry up, afterwards at 110-130 ℃ of baking 3-5min with nitrogen; Then with the OTS-SAMs matrix under the covering of photomask, under ultraviolet light, shine 30-40min, obtain the function self-assembled film of patterning;
(3) preparation BiFeO
3Precursor solution, and the OTS-SAMs matrix of the function self-assembled film of patterning vertically placed the precursor liquid for preparing, be incubated 7-8h down at 60-80 ℃, deposition finishes the back and cleans with ultrasonic oscillation, afterwards with film 550-620 ℃ annealing 2-3h, promptly get the patterning BiFeO of photoetching self assembly
3Film.
Ultrasonic waves for cleaning is respectively cleaned 10min for taking successively respectively with washing agent, acetone and ethanol in the described step (1), and each back of cleaning dries up with nitrogen with distilled water flushing substrate to clean back.
Described step (1) medium ultraviolet rayed instrument takes to get λ=184.9nm.
The OTS-toluene solution is prepared according to following method in the described step (2):
Take by weighing toluene in beaker with graduated cylinder, add that to account for the liquor capacity total amount be 1% octadecyl trichlorosilane solution again, stir on magnetic stirrer promptly, used instrument must keep dry in the operating process, because very easily hydrolysis of OTS.
BiFeO in the described step (3)
3Precursor solution is prepared according to following method:
With 0.01mol/LBi (NO
3)
35H
2Fe (the NO of O and 0.01mol/L
3)
39H
2O joins fully to stir in the 50mL acetum and makes it to dissolve fully, and the citric acid that adds 0.02mol/L then stirs 1h, and promptly De obtains stable BiFeO
3Precursor solution.
Described acetum is formulated by the glacial acetic acid of the distilled water of percent by volume 97.4% and 2.6%.
BiFeO at the preparation patterning
3In the film, crucial effects is played in the preparation of OTS self-assembled monolayer.OTS can form densification and orderly film at substrate surface, and the outer end is stretched on the methyl surface.Behind assembling OTS in the substrate, through UV-irradiation, the C-O key is interrupted, and surface conversion becomes hydrophilic hydroxyl (Si-OH) zone.At follow-up BiFeO
3In the deposition process, the BiFeO of hydroxyl surface
3Particle and substrate have stronger effect, and are deposited on the effect of the no chemical bond on methyl OTS surface, adhesion a little less than, can ultrasonicly remove.The film of this patterning will have huge application potential at microelectronic.
The invention has the beneficial effects as follows, with octadecyl trichlorosilane (OTS) is template, adopt ultraviolet radiation instrument as lithographic equipment, (λ=184.9nm) the OTS masterplate is carried out etching to obtain reticle pattern utilizes liquid phase to be self-assembled into membrane technology and prepare patterning BiFeO on the OTS-masterplate radiothermy ultraviolet light afterwards
3Film is applied to patterning BiFeO with this new technology of preparing
3The preparation of film has broad application prospects at microelectronic.
The patterning BiFeO that the present invention is prepared
3The fine and close homogeneous of film, edge contour is clear, combines firmly with substrate.And preparation technology is simple, and preparation process can not produce pollution, is a kind of eco-friendly patterned film technology of preparing.Can also change the patterning BiFeO that the photomask characteristic size is prepared the different surfaces micro-structural according to different actual needs
3Film.
Description of drawings
Fig. 1 is 70 ℃ for depositing temperature, sedimentation time 8h, gained BiFeO behind 600 ℃ of annealing 2h
3The X-Ray diffraction pattern of film.
Fig. 2 is 70 ℃ for depositing temperature, sedimentation time 8h, gained BiFeO behind 600 ℃ of annealing 2h
3The X-Ray photoelectron of film can general figure.
Fig. 3 is patterning BiFeO
3The stereoscan photograph of film.(a) and (b), (c) are the picture without the different amplification of ultrasonic oscillation, (d), (e) be the picture through the different amplification behind the ultrasonic oscillation, (f) is figure (e) BiFeO
3The partial enlarged drawing in film zone.
Fig. 4 and table 1, table 2 are patterning BiFeO
3The energy spectrum analysis of film.
Fig. 4-1 and table 1 are the constituent content analysis figure in silanol zone.
Fig. 4-2 and table 2 are the constituent content analysis figure in alkyl zone.
Embodiment
The present invention will be further described below in conjunction with specific embodiment.
(1) selecting common slide for use is substrate, and glass substrate is cut into the rectangle of 20mm * 10mm, uses commercially available washing agent, acetone, ethanol ultrasonic waves for cleaning 10min respectively, removes the impurity such as grease of glass substrate surface.With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic waves for cleaning.Place ultraviolet radiation instrument to shine 15min the substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
What (2) will the substrate after UV-irradiation place new preparation contains 1vol% octadecyl trichlorosilane (OTS)-toluene solution, soaks 30min at ambient temperature, makes substrate surface form one deck OTS monomolecular film.Clean 2min with acetone after immersion is finished, and dry up, afterwards at 120 ℃ of following baking 5min, to remove residual organic matter and to promote the chemisorbed of OTS-SAMs with nitrogen.Then with the OTS-SAMs matrix under the covering of photomask, (λ=184.9nm) is irradiation 30min down, obtains the function self-assembled film of patterning at ultraviolet light.OTS self assembly layer is subjected to the formation of the zone of UV-irradiation owing to silanol, and matrix surface is good hydrophilicity; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.
(3) with the Bi (NO of 0.01mol/L
3)
35H
2Fe (the NO of O and 0.01mol/L
3)
39H
2O joins fully to stir in the 50mL solution (glacial acetic acid by the distilled water of percent by volume 97.4% and 2.6% is formulated) and makes it to dissolve fully, and the citric acid that adds 0.02mol/L then stirs 1h, obtains stable BiFeO
3Precursor solution.The OTS-SAMs matrix of patterning is vertically placed the precursor liquid for preparing, and at 70 ℃ of following insulation 8h, deposition finishes the back cleans with ultrasonic oscillation, afterwards with film at 600 ℃ of annealing 2h, promptly get the patterning BiFeO of photoetching self assembly
3Film.
The OTS-toluene solution is prepared according to following method in the described step (2):
Take by weighing toluene in beaker with graduated cylinder, add that to account for OTS-toluene solution volume total amount be 1% octadecyl trichlorosilane solution again, stir on magnetic stirrer, used instrument must keep dry in the operating process, because very easily hydrolysis of OTS.
As can be seen from Figure 1, depositing temperature is 70 ℃, sedimentation time 8h, and behind 600 ℃ of annealing 2h, the gained film is the BiFeO of pure phase six sides distortion perovskite structure
3Film does not have other impurity peaks to occur.(101), (012), the diffraction peak intensity of (110) crystal face is higher, shows that crystal grain physically well develops, the crystallization degree height of film.
(1) selecting common slide for use is substrate, and glass substrate is cut into the rectangle of 20mm * 10mm, uses commercially available washing agent, acetone, ethanol ultrasonic waves for cleaning 10min respectively, removes the impurity such as grease of glass substrate surface.With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic waves for cleaning.Place ultraviolet radiation instrument to shine 10min the substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
What (2) will the substrate after UV-irradiation place new preparation contains 1vol% octadecyl trichlorosilane (OTS)-toluene solution, soaks 20min at ambient temperature, makes substrate surface form one deck OTS monomolecular film.Clean 3min with acetone after immersion is finished, and dry up, afterwards at 110 ℃ of following baking 4min, to remove residual organic matter and to promote the chemisorbed of OTS-SAMs with nitrogen.Then with the OTS-SAMs matrix under the covering of photomask, (λ=184.9nm) is irradiation 35min down, obtains the function self-assembled film of patterning at ultraviolet light.OTS self assembly layer is subjected to the formation of the zone of UV-irradiation owing to silanol, and matrix surface is good hydrophilicity; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.
(3) with the Bi (NO of 0.01mol/L
3)
35H
2Fe (the NO of O and 0.01mol/L
3)
39H
2O joins fully to stir in the 50mL solution (glacial acetic acid by the distilled water of percent by volume 97.4% and 2.6% is formulated) and makes it to dissolve fully, and the citric acid that adds 0.02mol/L then stirs 1h, obtains stable BiFeO
3Precursor solution.The OTS-SAMs matrix of patterning is vertically placed the precursor liquid for preparing, and at 60 ℃ of following insulation 7h, deposition finishes the back cleans with ultrasonic oscillation, afterwards with film at 550 ℃ of annealing 3h, promptly get the patterning BiFeO of photoetching self assembly
3Film.
OTS-toluene solution compound method is with embodiment 1 in the step (2).
Embodiment 3
(1) selecting common slide for use is substrate, and glass substrate is cut into the rectangle of 20mm * 10mm, uses commercially available washing agent, acetone, ethanol ultrasonic waves for cleaning 10min respectively, removes the impurity such as grease of glass substrate surface.With a large amount of distilled water flushing substrates, dry up with nitrogen at last after each ultrasonic waves for cleaning.Place ultraviolet radiation instrument to shine 20min the substrate of cleaning, make substrate surface reach " atomic cleanliness degree ".
What (2) will the substrate after UV-irradiation place new preparation contains 1vol% octadecyl trichlorosilane (OTS)-toluene solution, soaks 40min at ambient temperature, makes substrate surface form one deck OTS monomolecular film.Clean 3min with acetone after immersion is finished, and dry up, afterwards at 130 ℃ of following baking 3min, to remove residual organic matter and to promote the chemisorbed of OTS-SAMs with nitrogen.Then with the OTS-SAMs matrix under the covering of photomask, (λ=184.9nm) is irradiation 40min down, obtains the function self-assembled film of patterning at ultraviolet light.OTS self assembly layer is subjected to the formation of the zone of UV-irradiation owing to silanol, and matrix surface is good hydrophilicity; And be not the alkyl zone by the zone of UV-irradiation, matrix surface presents original hydrophobicity.
(3) with the Bi (NO of 0.01mol/L
3)
35H
2Fe (the NO of O and 0.01mol/L
3)
39H
2O joins fully to stir in the 50mL solution (glacial acetic acid by the distilled water of percent by volume 97.4% and 2.6% is formulated) and makes it to dissolve fully, and the citric acid that adds 0.02mol/L then stirs 1h, obtains stable BiFeO
3Precursor solution.The OTS-SAMs matrix of patterning is vertically placed the precursor liquid for preparing, and at 80 ℃ of following insulation 7.5h, deposition finishes the back cleans with ultrasonic oscillation, afterwards with film at 620 ℃ of annealing 2.5h, promptly get the patterning BiFeO of photoetching self assembly
3Film.
OTS-toluene solution compound method is with embodiment 1 in the step (2).
As can be seen from Figure 2, the peak value of Fe2p3/2 and Fe2p1/2 appears at 710.9eV and 724.4eV respectively.For Fe
3+, the peak value of Fe2p3/2 should be between 710.6eV and 711.2eV, and for Fe
2+, peak value should be at 709.4eV.This shows that prepared film is pure phase BiFeO
3Film, the oxidation state of Fe are Fe
3+, do not have Fe
2+Occur.
Fig. 3 is the BiFeO of patterning
3Film, (a) and (b), (c) are the picture without the different amplification of ultrasonic oscillation, (d), (e) be the picture through the different amplification behind the ultrasonic oscillation, (f) is figure (e) BiFeO
3The partial enlarged drawing in film zone.As can be seen from the figure, the BiFeO of alkyl area deposition
3Particle is discontinuous, under ultrasonic oscillation, comes off easily, and at the BiFeO of silanol area deposition
3The film edge clear-cut, fine and close homogeneous combines firmly difficult drop-off under ultrasonic oscillation with substrate.
Fig. 4 and table 1,2 is the patterning BiFeO behind the ultrasonic oscillation
3The power spectrum of film zones of different.
The constituent content in the constituent content table 2 alkyl zone in table 1 silanol zone
Fig. 4-1 is the constituent content in silanol zone corresponding to table 1, and the content of visible Bi and Fe is respectively 2.83mol% and 2.61mol%, measures than 1: 1 near the Bi/Fe theoretical chemistry.Fig. 4-2 is the constituent content in alkyl zone corresponding to table 2, does not contain the Fe element, and the Bi element of minute quantity is arranged, and Na, Mg, Si, Ca are contained element in the glass substrate.This shows, BiFeO
3Film is in the absorption of silanol regioselectivity, growth.
Comprehensive above-mentioned X-Ray diffraction, ESEM and energy spectrum analysis show: utilize liquid deposition and photoetching self-assembled monolayer membrane technology successfully to prepare patterning BiFeO
3Film.
Claims (6)
1. patterning BiFeO
3The photoetching self-assembly preparation method thereof of film is characterized in that, this method comprises following preparation process:
(1) selecting common slide for use is substrate, and the glass substrate difference ultrasonic waves for cleaning with well cutting dries up; And place ultraviolet radiation instrument to shine 10-20min the clean glass substrate;
(2) glass substrate after UV-irradiation is placed concentration of volume percent 1% octadecyl trichlorosilane OTS-toluene solution, soak 20-40min at ambient temperature, make substrate surface form one deck OTS monomolecular film; Clean 2-3min with acetone after immersion is finished, and dry up, afterwards at 110-130 ℃ of baking 3-5min with nitrogen; Then with the OTS-SAMs matrix under the covering of photomask, under ultraviolet light, shine 30-40min, obtain the function self-assembled film of patterning;
(3) preparation BiFeO
3Precursor solution, and the OTS-SAMs matrix of the function self-assembled film of patterning vertically placed the precursor liquid for preparing, be incubated 7-8h down at 60-80 ℃, deposition finishes the back and cleans with ultrasonic oscillation, afterwards with film 550-620 ℃ annealing 2-3h, promptly get the patterning BiFeO of photoetching self assembly
3Film.
2. a kind of patterning BiFeO according to claim 1
3The photoetching self-assembly preparation method thereof of film is characterized in that, ultrasonic waves for cleaning is respectively cleaned 10min for taking successively respectively with washing agent, acetone and ethanol in the described step (1), and each back of cleaning dries up with nitrogen with distilled water flushing substrate to clean back.
3. a kind of patterning BiFeO according to claim 1
3The photoetching self-assembly preparation method thereof of film is characterized in that, described step (1) medium ultraviolet rayed instrument takes to get λ=184.9nm.
4. a kind of patterning BiFeO according to claim 1
3The photoetching self-assembly preparation method thereof of film is characterized in that, the OTS-toluene solution is prepared according to following method in the described step (2):
Take by weighing toluene in beaker with graduated cylinder, add again that to account for the liquor capacity total amount be 1% octadecyl trichlorosilane solution, on magnetic stirrer, stir promptly.
5. a kind of patterning BiFeO according to claim 1
3The photoetching self-assembly preparation method thereof of film is characterized in that, BiFeO in the described step (3)
3Precursor solution is prepared according to following method:
Bi (NO with 0.01mol/L
3)
35H
2Fe (the NO of O and 0.01mol/L
3)
39H
2O joins fully to stir in the 50mL acetum and makes it to dissolve fully, and the citric acid that adds 0.02mol/L then stirs 1h, promptly obtains stable BiFeO
3Precursor solution.
6. a kind of patterning BiFeO according to claim 5
3The photoetching self-assembly preparation method thereof of film is characterized in that, described acetum is formulated by the glacial acetic acid of the distilled water of percent by volume 97.4% and 2.6%.
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