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CN102011190B - Method for preparing nano-structure barium strontium titanate ferroelectric film by utilizing nano-crystal self-assembly process - Google Patents

Method for preparing nano-structure barium strontium titanate ferroelectric film by utilizing nano-crystal self-assembly process Download PDF

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CN102011190B
CN102011190B CN2010105997704A CN201010599770A CN102011190B CN 102011190 B CN102011190 B CN 102011190B CN 2010105997704 A CN2010105997704 A CN 2010105997704A CN 201010599770 A CN201010599770 A CN 201010599770A CN 102011190 B CN102011190 B CN 102011190B
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strontium
nanocrystalline
barium titanate
barium
oleic acid
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CN102011190A (en
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曾燕伟
莫雷清
杨晓伟
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Nanjing Tech University
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Abstract

The invention provides a method for preparing a barium strontium titanate ferroelectric film by utilizing a nanocrystalline self-assembly process. The technical scheme is that the barium strontium titanate nanocrystalline with the quasi-cubic morphology is subjected to oleic acid molecular surface modification under the condition of alcoholic heat (Glycothermal), and then is dispersed in a mixed reagent containing cyclohexane, normal hexane and normal octane to form the nanocrystalline dispersion liquid with high stability. Quantitatively transferring the nanocrystalline dispersion to chemically polished single crystal Si wafer or Pt/Ti/SiO by microliter injector2On the surface of the Si sheet substrate, the spreading speed of the nanocrystalline dispersion liquid on the surface of the substrate is adjusted by controlling the volatilization speed of the organic solvent, and the ferroelectric film with closely arranged nano-structure characteristics is self-assembled on the surface of the substrate by means of the interaction force among barium strontium titanate nanocrystalline particles. The method has important application value for preparing the planar nano ordered array structure of the ultra-high density ferroelectric memory.

Description

A kind of method of utilizing nanocrystalline self assembling process to prepare the nanostructure barium strontium titanate ferroelectric film
Technical field:
The invention belongs to advanced nano structural material and devices field; Relate to and a kind ofly prepare the method for nanostructure barium strontium titanate ferroelectric film, VHD ferroelectric memory plane nano oldered array structure is had significant application value with relevant microelectronics or nanoelectronics preparation of devices through nanocrystalline self assembling process.
Background technology:
Nano material is from 20th century the mid-80 a kind of advanced material of obtaining developing rapidly.Owing to itself have quantum size effect, surface effects, small-size effect and macro quanta tunnel effect,, purposes widely arranged in chemical industry, electronics, food, biology and medicine and other fields so often show the character and the function of many uniquenesses.Especially at the microelectronics manufacture field; People adopt the pattern of " (top down) from top to bottom " that the large-scale integrated circuit live width has been run into difficulty when nanoscale advances; Nanometer self-assembling technique and ordered structural material thereof based on " (bottom up) from bottom to top " notion have shown huge potential, thereby the research of micro-nanometer ordered structure material and device becomes the research focus in the current field of nanometer material technology.The micro-nanometer ordered structure material is to be built into panoramic nanostructure or device to nano structured unit according to certain rules in two dimension or three-dimensional space; Its performance depends on the character of structural unit and the interaction between structural unit; People can realize the MC to the micro-nanometer ordered structure material property through the size and the interaction parameter of adjustment nano structured unit.
The structural unit that is used to construct inorganic nano ordered structure functional materials or device at present mainly is the nanocrystalline of various semi-conductors and oxide compound, and they are that particle diameter is the single crystal particle of nanoscale.Because nanocrystalline band gap is bigger, thereby show electricity, magnetics and the optical property of many uniquenesses.For example the specific conductivity of metallic nano crystal is very low; The magnetic Nano crystalline substance shows superparamagnetism; The absorb light of semiconductor nano and radiative wavelength be variation etc. with nanocrystalline change of size, makes the nanocrystalline important integral part in the various micro-nano electron devices such as photodiode, single-electronic transistor, storer that becomes.Be expected to make data storage device after functional oxide nanocrystalline (nanocrystalline) self-assembly, greatly improve storage density and response speed, thereby further promote the microtronics technology to the nanoelectronics technical development like magnetic, ferroelectric, piezoelectric oxide etc.
Strontium-barium titanate is a kind of ferroelectric material of excellent performance; Have that high relative dielectric constant, low dielectric loss, Tc change along with composition and relative permittivity with characteristics such as electric field nonlinearities change; Its thin-film material has important use and is worth in fields such as ultra-large dynamic storage, non-volatility ferroelectric storer and microwave-tuned devices, be one of material of the broad research of semi-conductor-ferroelectric integrated micro devices field.At present, the preparation of high quality barium strontium titanate is mainly through magnetron sputtering method, chemical Vapor deposition process and pulsed laser deposition etc.For realizing the nano array structureization of ferroelectric membranc, planar micro electron device processing technologies such as focused ion beam technology, electron beam inscription and nano impression have at first obtained use.Obviously, these methods all depend on various film deposition apparatus and the meticulous microelectronic device processing unitss of costing an arm and a leg with technology.The present invention provides a kind of method of utilizing nanocrystalline self assembling process to prepare the nanostructure barium strontium titanate ferroelectric film; The advantage of this method be need not cost an arm and a leg thin film deposition growing apparatus and meticulous microelectronic device processing units, the assembling process easiness in handling.Nanocrystalline self-assembly forms the ferroelectric nano film to method of the present invention for other functional ferroelectric oxide, and the meaning of no less important is arranged.
Summary of the invention:
The purpose of this invention is to provide a kind of method of utilizing nanocrystalline self assembling process to prepare the nanostructure barium strontium titanate ferroelectric film, the advantage of this method be need not cost an arm and a leg film deposition apparatus and meticulous little processing units; Through the control that the preparation and the organic solvent of the nanocrystalline dispersion liquid of suitable concn are sprawled evaporation rate in the process at nanocrystalline dispersion liquid, realize that the direct self-assembly on the Si substrate plane of strontium-barium titanate ferroelectric nano crystalline substance forms the ferroelectric membranc with nanostructure.
Technical scheme of the present invention is: the present invention will have that the strontium-barium titanate of regular morphology is nanocrystalline to carry out finishing; Be dispersed in then to contain in the good organic reagent of spreading property and volatile performance and form the nanocrystalline dispersion liquid of high stable, and then nanocrystalline dispersion liquid is quantitatively transferred to single crystalline Si sheet or Pt/Ti/SiO 2On/Si sheet the substrate surface; Regulate and control the spreading rate of nanocrystalline dispersion liquid through control organic solvent evaporation rate at the Si substrate surface; By nano-crystalline granule interphase interaction power, on substrate surface, be self-assembled into compact arranged single or multiple lift nano-crystal film.
Concrete technical scheme of the present invention: a kind of method of utilizing nanocrystalline self assembling process to prepare the nanostructure barium strontium titanate ferroelectric film, its concrete steps are following:
The nanocrystalline oleic acid molecular that under alcohol heat (glycothermal) condition, carries out grain surface of strontium-barium titanate that A. will have regular morphology is modified, and disperses so that it reaches in non-polar organic solvent completely;
B. oleic acid molecular is modified that the back strontium-barium titanate is nanocrystalline to be isolated mutually from pure hydrothermal solution, removed remaining liquid phase of pure thermal process and physical adsorption oleic acid molecular through washing, it is nanocrystalline to obtain the strontium-barium titanate of oleic acid molecular modification through drying then;
C. be component solvent with analytical pure hexanaphthene, normal hexane and octane; Prepare mixed organic solvents by a certain percentage; The oleic acid modified strontium-barium titanate that step B is obtained is nanocrystalline to be scattered in the organic solvent of being prepared under ultrasound condition, forms the nanocrystalline dispersion liquid of strontium-barium titanate of transparent high stable;
D. will pass through the single crystalline Si sheet after the washing of acetone, alcohol or be the Pt/Ti/SiO of top electrode 2/ Si sheet lies in one glass of type Glass Containers, places circular middling speed filter paper in its periphery symmetry, and the Glass Containers opening is sealed with transparent plastic film;
E. be taken at the organic solvent of preparing among the step C with the metering syringe; Organic solvent is evenly dropped on the Si sheet filter paper on every side through mode at acanthopore on the plastics film; In the nearly saturated vapor pressure atmosphere of the inner formation of Glass Containers; Then, get on the disposable Si of the dropping in substrate of the nanocrystalline dispersion liquid of strontium-barium titanate with the metering syringe and to make it to sprawl, regulate the vaporator rate and the dispersion liquid of organic solvent through aperture size on the sealed plastic film and number and sprawl speed; The last strontium-barium titanate nano-crystal film that on substrate, obtains self assembling process formation;
F. the Si sheet that the surface is formed with strontium-barium titanate self-assembly nano-crystalline film carefully takes out from Glass Containers, transfers to the thermal treatment of annealing in the quick anneal oven, removes the oleic acid molecular of strontium-barium titanate nanocrystal surface, and makes the nanometer packaging assembly reach curing.
Among the above-mentioned optimization step A; The glycothermal condition that strontium-barium titanate nanocrystal surface oleic acid molecular is modified is: 0.3~0.5g strontium-barium titanate is nanocrystalline to be dispersed in 40~80ml1 through ultrasonic procedure; In 4 butyleneglycols-water mixed solvent, wherein the mass content of water is 5~10% in the mixed solvent; Then, this dispersion system is transferred in the reaction kettle, and (is benchmark with the 100ml mixed solvent) the oleic acid tensio-active agent that in this mixed solvent, adds 0.5~1.0ml/100ml, nitrogen purges, the tight back of lid is incubated 5~10 hours under 180~230 ℃ of conditions.
Among the above-mentioned optimization step B, oleic acid molecular is modified the nanocrystalline condition with liquid phase separation and washing of back strontium-barium titanate and is: rotating speed is the spinning of 8000~12000rpm, disengaging time 30~45min; Adopt remaining 1, the 4 butyleneglycol molecule of alcohol-water solution washing earlier, alcohol quality concentration is 30~60%; Adopt hexanaphthene-alcohol organic solvent washing physical adsorption oleic acid then, the hexanaphthene mass concentration is 30~50%; Adopt the nanocrystalline 0.5~1.0hr of drying treatment strontium-barium titanate under 500W ir lamp irradiation and-0.1~-0.2 atmospheric pressure again; Above-mentioned washing times is as the criterion with wash clean, generally can repeat 2-5 time.
Among the above-mentioned optimization step C; The percent by volume of component solvent is in the mixed solvent: hexanaphthene 60%-80%, normal hexane 5%-35% and octane 5%-35%, the nanocrystalline content of strontium-barium titanate that is scattered in wherein is 0.2~2.0g/100ml (is benchmark with the 100ml mixed solvent).Under 20~30 ℃ of conditions,, use ultrasonic power: 50~100W, ultrasonic time: 5~10min to 5~10ml dispersion liquid.
Among the above-mentioned optimization step E, the organic solvent that is incorporated on the Si sheet filter paper on every side by microliter syringe is 5~50 μ l/cm 2, the nanocrystalline dispersion liquid of strontium-barium titanate is pressed Si sheet surface and is introduced by 50~70% calculated amount of individual layer or the long-pending all standing amount of multi-layer nano crystal face.The diameter of regulating aperture on the required film of evaporation rate of solvent (being nanocrystalline spreading rate) is 5~10 of 0.2~1mm, aperture numbers.Among the above-mentioned optimization step E, thermal treatment temp is 450~550 ℃, and the time is 400~600s.
Beneficial effect:
The present invention provides a kind of and utilizes nanocrystalline self assembling process preparation to have the method for the barium strontium titanate ferroelectric film of nanostructure.The advantage of this method is: can be the nanocrystalline or brilliant film with nanostructure that closely is arranged in of multi-layer nano by individual layer through the formed film of the nanocrystalline self assembling process of strontium-barium titanate 1), have important value to developing the non-traditional technology of preparing of micro-nano electron device of new generation; 2) method provided by the invention realizes the compound preparation of heterogeneous multi-layer material film applicable to different substrate materials; 3) need not to cost an arm and a leg film deposition apparatus and meticulous little processing units, cost is low, and operating process is controlled easily; 4) be equally applicable to the preparation of other functional oxide nanocrystalline planar array structure.
Description of drawings:
The nanocrystalline FESEM photo that is self-assembled into the single layer nanometer structure surface on single crystalline Si sheet surface of Fig. 1 strontium-barium titanate;
The nanocrystalline FESEM photo that is self-assembled into the multi-layer nano body structure surface on single crystalline Si sheet surface of Fig. 2 strontium-barium titanate;
Fig. 3 is the Pt/Ti/SiO of Pt lower conducting dome 2/ Si substrate surface FESEM photo;
Fig. 4 strontium-barium titanate is nanocrystalline at Pt/Ti/SiO 2/ Si substrate surface is self-assembled into the FESEM photo of multi-layer nano body structure surface.
Embodiment:
Embodiment 1:
Utilize nanocrystalline self assembling process on the single crystalline Si sheet, to prepare strontium-barium titanate individual layer nano-crystal film, its operation steps is following:
A. with 0.3g have accurate cube of pattern peace all the length of side be that the nanocrystalline ultrasonication through 50W * 10min of strontium-barium titanate of 20nm is dispersed in 60ml1, in 4 butyleneglycols-water mixed solvent, wherein quality content is 10%.Then, this dispersion system is transferred in the reaction kettle, and in this mixed solvent, added 0.5ml oleic acid tensio-active agent, nitrogen purges, the insulation 6 hours under 200 ℃ of conditions of the tight back of lid.
B. with nanocrystalline in the reaction kettle and liquid phase separation, centrifugal rotational speed is 10000rpm, time 35min.With remaining 1, the 4 butyleneglycol molecule of 50wt% alcohol-water solution washing; With 50wt% hexanaphthene-spirituous solution washing physics adsorbed oil acid; After 3 washings and spinning, gained is wet nanocrystalline with drying treatment under 500W ir lamp irradiation and-0.1 atmospheric pressure 0.5 hour.
C. be that hexanaphthene 80%, normal hexane 10% and octane 10% are mixed with mixed organic solvents with volume ratio; Under 20 ℃ of conditions; 75mg is scattered under power and time are the ultrasonication of 50W * 8min in the organic solvent that 5ml prepares through the strontium-barium titanate of oleic acid modified is nanocrystalline, forms the nanocrystalline dispersion liquid of strontium-barium titanate of transparent high stable;
D. will passing through the single crystalline Si sheet that is of a size of 15x15mm after the washing of acetone, alcohol, to be placed on diameter be 40mm, high in the cup type Glass Containers of 25mm, at the circular middling speed filter paper of its periphery symmetry placement, then the Glass Containers opening sealed with transparent plastic film;
E. get the mixed organic solvents that 20 μ l prepare with microliter syringe in step B, organic solvent is evenly dropped on the Si sheet filter paper on every side through mode at acanthopore on the plastics film.Then; Press Si sheet surface by 60% metering of nanocrystalline individual layer overlay capacity; Use microliter syringe to get the nanocrystalline solid content of 1.2 μ l strontium-barium titanates as making it to sprawl on the disposable Si of the dropping in substrate of the dispersion liquid of 15mg/ml; And the hole that 5 diameters of thorn are about 0.3mm on sealed plastic film regulates and control the vaporator rate of organic solvent, and solvent evaporates fully on the Si substrate.
F. the Si sheet that the surface is formed with strontium-barium titanate self-assembly nano-crystalline film carefully takes out from vial; Transfer in the quick anneal oven; In temperature is to handle 550s under 450 ℃ of conditions, removing the oleic acid molecular of strontium-barium titanate nanocrystal surface, and makes the nanometer packaging assembly reach curing.
To prepare the barium strontium titanate sample through above-mentioned steps is placed under the field emission scanning electron microscope (FESEM) and observes; The nanocrystalline film with single layer nanometer structure that under the aforesaid operations condition, formed of strontium-barium titanate on the Si substrate, its microstructure features is shown in FESEM photo among Fig. 1.
Embodiment 2:
Utilize nanocrystalline self assembling process on the single crystalline Si sheet, to prepare nanostructure strontium-barium titanate multilayer film, its operation steps is following:
A. with 0.4g have accurate cube of pattern peace all the length of side be that the nanocrystalline ultrasonication through 60W * 8min of strontium-barium titanate of 20nm is dispersed in 70ml1, in 4 butyleneglycols-water mixed solvent, wherein quality content is 8%.Then, this dispersion system is transferred in the reaction kettle, and in this mixed solvent, added 0.6ml oleic acid tensio-active agent, nitrogen purges, the insulation 8 hours under 190 ℃ of conditions of the tight back of lid.
B. with nanocrystalline in the reaction kettle and liquid phase separation, centrifugal rotational speed is 8000rpm, time 45min.With remaining 1, the 4 butyleneglycol molecule of 40wt% alcohol-water solution washing; With 40wt% hexanaphthene-spirituous solution washing physics adsorbed oil acid; After 4 washings and spinning, gained is wet nanocrystalline with drying treatment under 500W ir lamp irradiation and-0.15 atmospheric pressure 0.8 hour.
C. be hexanaphthene 60%, normal hexane 25% and octane 15% preparation mixed organic solvents with volume ratio; Under 22 ℃ of conditions; 100mg is scattered under power and time are the ultrasonication of 70W * 10min in the organic solvent that 5ml prepares through the strontium-barium titanate of oleic acid modified is nanocrystalline, forms the nanocrystalline dispersion liquid of strontium-barium titanate of transparent high stable;
D. will passing through the single crystalline Si sheet that is of a size of 15x15mm after the washing of acetone, alcohol, to be placed on diameter be 40mm, high in the cup type Glass Containers of 25mm, at the circular middling speed filter paper of its periphery symmetry placement, then the Glass Containers opening sealed with transparent plastic film;
E. get the mixed organic solvents that 25 μ l prepare with microliter syringe in step B, organic solvent is evenly dropped on the Si sheet filter paper on every side through mode at acanthopore on the plastics film.Then; Press Si sheet surface by 70% of nanocrystalline 3 layers of overlay capacity; Use microliter syringe to get the nanocrystalline solid content of 2 μ l strontium-barium titanates as making it to sprawl on the disposable Si of the dropping in substrate of the dispersion liquid of 20mg/ml; And the hole that 7 diameters of thorn are 0.4mm on the sealed plastic film vaporator rate of regulating organic solvent, solvent evaporates fully on the Si substrate.
F. the Si sheet that the surface is formed with strontium-barium titanate self-assembly nano-crystalline film carefully takes out from vial; Transfer in the quick anneal oven; Be thermal treatment 500s under 480 ℃ the condition in temperature, removing the oleic acid molecular of strontium-barium titanate nanocrystal surface, and make the nanometer packaging assembly reach curing.
To prepare the barium strontium titanate sample through above-mentioned steps is placed under the field emission scanning electron microscope (FESEM) and observes; The nanocrystalline nano structure membrane with average about 3 bed thickness, even compact that under the aforesaid operations condition, formed of strontium-barium titanate on the Si substrate, its microstructure features is shown in FESEM photo among Fig. 2.
Embodiment 3:
Utilize nanocrystalline self assembling process at Pt/Ti/SiO with microstructure features shown in FESEM photo among Fig. 3 2Preparation nanostructure strontium-barium titanate multilayer film on the/Si sheet, its operation steps is following:
A. with 0.4g have accurate cube of pattern peace all the length of side be that the nanocrystalline ultrasonication through 60W * 8min of strontium-barium titanate of 20nm is dispersed in 80ml1, in 4 butyleneglycols-water mixed solvent, wherein quality content is 10%.Then, this dispersion system is transferred in the reaction kettle, and in this mixed solvent, added 0.5ml oleic acid tensio-active agent, nitrogen purges, the insulation 10 hours under 220 ℃ of conditions of the tight back of lid.
B. with nanocrystalline in the reaction kettle and liquid phase separation, centrifugal rotational speed is 12000rpm, time 30min.With remaining 1, the 4 butyleneglycol molecule of 55wt% alcohol-water solution washing; With 55wt% hexanaphthene-spirituous solution washing physics adsorbed oil acid; After 4 washings and spinning, gained is wet nanocrystalline with drying treatment under 500W ir lamp irradiation and-0.2 atmospheric pressure 1 hour.
C. be hexanaphthene 70%, normal hexane 20% and octane 10% preparation mixed organic solvents with volume ratio; Under 25 ℃ of conditions; 100mg is scattered under power and time are the ultrasonication of 80W * 10min in the organic solvent that 5ml prepares through the strontium-barium titanate of oleic acid modified is nanocrystalline, forms the nanocrystalline dispersion liquid of strontium-barium titanate of transparent high stable;
D. will pass through the Pt/Ti/SiO that is of a size of 15x15mm after the washing of acetone, alcohol 2It is 40mm, high in the cup type Glass Containers of 25mm that/Si sheet is placed on diameter, places circular middling speed filter paper in its periphery symmetry, then the Glass Containers opening is sealed with transparent plastic film;
E. get the mixed organic solvents that 35 μ l prepare with microliter syringe in step B, the mode through acanthopore on plastics film evenly drops in Pt/Ti/SiO with organic solvent 2On the filter paper around the/Si sheet.Then, press Pt/Ti/SiO 2/ Si sheet surface is used microliter syringe to get the nanocrystalline solid content of 2 μ l strontium-barium titanates and is the disposable Pt/Ti/SiO of dropping in of the dispersion liquid of 20mg/ml by 60% of nanocrystalline 3 layers of overlay capacity 2Make it to sprawl on/Si the substrate, and the hole that 6 diameters of thorn are 0.5mm on the sealed plastic film vaporator rate of regulating organic solvent, until Pt/Ti/SiO 2Solvent evaporates fully on the/Si substrate.
F. the surface is formed with the Pt/Ti/SiO of strontium-barium titanate self-assembly nano-crystalline film 2/ Si sheet carefully takes out from vial, transfers in the quick anneal oven, is thermal treatment 400s under 550 ℃ the condition in temperature, removing the oleic acid molecular of strontium-barium titanate nanocrystal surface, and makes the nanometer packaging assembly reach curing.
To prepare the barium strontium titanate sample through above-mentioned steps is placed under the field emission scanning electron microscope (FESEM) and observes Pt/Ti/SiO 2The nanocrystalline nano structure membrane with average about 3 bed thickness, even compact that under the aforesaid operations condition, formed of strontium-barium titanate on the/Si substrate, its microstructure features is shown in FESEM photo among Fig. 4.

Claims (6)

1. method of utilizing nanocrystalline self assembling process to prepare the nanostructure barium strontium titanate ferroelectric film, its concrete steps are following:
The nanocrystalline oleic acid molecular that under pure heat condition, carries out grain surface of strontium-barium titanate that (1) will have regular morphology is modified, and disperses so that it reaches in non-polar organic solvent completely;
(2) oleic acid molecular is modified the back strontium-barium titanate is nanocrystalline to be isolated mutually from pure hydrothermal solution, removed remaining liquid phase of pure thermal process and physical adsorption oleic acid molecular through washing, the strontium-barium titanate that obtains the oleic acid molecular modification is nanocrystalline;
(3) be component solvent with analytical pure hexanaphthene, normal hexane and octane, the preparation mixed organic solvents, wherein the percent by volume of component solvent is in the mixed solvent: hexanaphthene 60%-80%, normal hexane 5%-35% and octane 5%-35%; To under ultrasound condition, be scattered in the organic solvent of being prepared through the strontium-barium titanate of oleic acid modified is nanocrystalline, form the transparent nanocrystalline dispersion liquid of stable strontium-barium titanate; The nanocrystalline content of strontium-barium titanate that wherein is scattered in wherein is 0.2~2.0g/100ml;
(4) will pass through the single crystalline Si sheet after the washing of acetone, alcohol or be the Pt/Ti/SiO of top electrode 2/ Si sheet lies in one glass of type Glass Containers, places circular middling speed filter paper in its periphery symmetry, after the vial opening is sealed with transparent plastic film;
(5) be taken at the organic solvent of preparing in the step (3) with the metering syringe, organic solvent evenly dropped on the Si sheet filter paper on every side, in Glass Containers, form nearly saturated vapor pressure atmosphere through mode at acanthopore on the plastics film; Then, get on the disposable Si of the dropping in substrate of the nanocrystalline dispersion liquid of strontium-barium titanate with the metering syringe and to make it to sprawl, and sprawl speed through vaporator rate and dispersion liquid that aperture size on the sealed plastic film and number are regulated organic solvent; Wherein the nanocrystalline dispersion liquid of strontium-barium titanate is pressed Si sheet surface by 50~70% calculated amount introducing of individual layer or the long-pending all standing amount of multi-layer nano crystal face; The adjusting evaporation rate of solvent is that the diameter of aperture on the required film of nanocrystalline spreading rate is 0.2~1mm, 5~10 of aperture numbers, and solvent evaporates fully on the Si substrate; The last strontium-barium titanate nano-crystal film that on substrate, obtains self assembling process formation;
(6) the Si sheet that the surface is formed with strontium-barium titanate self-assembly nano-crystalline film takes out from Glass Containers, transfers to the thermal treatment of annealing in the lehre, removes the oleic acid molecular of strontium-barium titanate nanocrystal surface, and makes the nanometer packaging assembly reach curing.
2. the method for preparing the nanostructure barium strontium titanate ferroelectric film according to claim 1; It is characterized in that in the step (1); The pure heat condition that strontium-barium titanate nanocrystal surface oleic acid molecular is modified is: be dispersed in 40~80ml1 so that 0.3~0.5g strontium-barium titanate is nanocrystalline through ultrasonic procedure; In 4 butyleneglycols-water mixed solvent, wherein the mass content of water is 5~10% in the mixed solvent; Then, this dispersion system is transferred in the reaction kettle, and in this mixed solvent, added 0.5~1.0ml/100ml oleic acid tensio-active agent, nitrogen purges, the tight back of lid is incubated 5~10 hours under 180~230 ℃ of conditions.
3. the method for preparing the nanostructure barium strontium titanate ferroelectric film according to claim 1; It is characterized in that strontium-barium titanate nanocrystalline condition with liquid phase separation and washing in oleic acid molecular modification back is in the step (2): rotating speed is the spinning of 8000~12000rpm, and disengaging time is 30~45min; Adopt remaining 1, the 4 butyleneglycol molecule of alcohol-water solution washing, alcohol quality concentration is 30~60%; Adopt hexanaphthene-alcohol organic solvent washing physical adsorption oleic acid then, the hexanaphthene mass concentration is 30~50%; Adopt the nanocrystalline 0.5~1.0hr of drying treatment strontium-barium titanate under 500W ir lamp irradiation and-0.1~-0.2 atmospheric pressure again.
4. the method for preparing the nanostructure barium strontium titanate ferroelectric film according to claim 1 is characterized in that the ultrasound condition described in the step (3) is: under 20~30 ℃ of conditions, use ultrasonic power: 50~100W, ultrasonic time: 5~10min.
5. the method for preparing the nanostructure barium strontium titanate ferroelectric film according to claim 1 is characterized in that in the step (5), and the organic solvent that is incorporated on the Si sheet filter paper on every side by microliter syringe is 5~50 μ l/cm 2
6. the method for preparing the nanostructure barium strontium titanate ferroelectric film according to claim 1 is characterized in that in the step (6), thermal treatment temp is 450~550 ℃, and the time is 400~600s.
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CN100516140C (en) * 2007-05-18 2009-07-22 西安交通大学 Method for preparing strontium-barium titanate/polymide dielectric adjustable composite material thick film
CN100558939C (en) * 2007-07-26 2009-11-11 同济大学 The low temperature preparation method of alcohol heat assistant ferro-electricity film
CN101220187A (en) * 2008-01-31 2008-07-16 复旦大学 Magnetic composite microsphere with nucleocapsid structure and method for producing the same
CN101748489A (en) * 2009-10-16 2010-06-23 齐齐哈尔大学 Method for self-assembling Bi4-xYxTi3O12 ferroelectric film at low temperature

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