CN102534610A - Method for depositing compact barium strontium titanate film on glass substrate - Google Patents
Method for depositing compact barium strontium titanate film on glass substrate Download PDFInfo
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- CN102534610A CN102534610A CN2012100442027A CN201210044202A CN102534610A CN 102534610 A CN102534610 A CN 102534610A CN 2012100442027 A CN2012100442027 A CN 2012100442027A CN 201210044202 A CN201210044202 A CN 201210044202A CN 102534610 A CN102534610 A CN 102534610A
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Abstract
The invention discloses a method for depositing a compact barium strontium titanate film on a glass substrate, which comprises the following steps: 1. preparing a precursor solution; 2. putting the prepared precursor solution together with a beaker into a vacuum chamber to carry out vacuum treatment until no bubble is discharged from the precursor solution; 3. putting a hydrophilic glass substrate with an OTS monomolecular film into the precursor solution subjected to vacuum treatment to carry out selfassembly growth of the film; and 4. annealing the deposited film at 600 DEG C for 2 hours to finally obtain the compact barium strontium titanate film. The precursor solution vacuum treatment technology and frequent induction adsorption liquid-phase selfassembly method are utilized to prepare the compact barium strontium titanate film on the glass substrate; and thus, the compact barium strontium titanate film has high surface density and functional uniformity, and the treatment process is simple and convenient to operate.
Description
[technical field]
The invention belongs to field of functional materials, relate to a kind of wet-chemical liquid phase method and prepare the densification film process.
[background technology]
Strontium-barium titanate (Ba
xSr
1-xTiO
3) ferroelectric membranc have leakage current little, be difficult for tired, Tc is adjustable, pyroelectric coefficient is high, non-linear characteristics such as strong, can be widely used in dynamic random holder (DRAM), pyroelectric infrared detector, dielectric phase shifter, H
2In the devices such as detector, be that one of ferroelectric thin-flim materials of application prospect is arranged most.Have and prepare Ba with pulsed laser deposition (PLD), magnetron sputtering, sol-gel (sol-gel), metal-organic chemical vapor deposition equipment methods such as (MOCVD)
xSr
1-xTiO
3Film.Uniformity of film is poor in the pulsed laser deposition, is difficult to make the high quality large area film, and apparatus expensive.The growth velocity of magnetron sputtering is slow in the magnetron sputtering method, thin film composition usually and target certain deviation is arranged.Film is prone to crack performance in the sol-gel method, and processing parameter is difficult to be grasped.The starting material of the heavy method of Organometallic Chemistry gas phase and the price of equipment are all very expensive, and source material has severe toxicity usually.The liquid phase self-assembly process technology that comes into one's own has recently then overcome more above-mentioned shortcomings.Simple and easy to do, need not special device, be solvent with water usually, have the advantage of deposition process and membrane structure molecular level control.Can utilize the successive sedimentation different components, two dimension even three-dimensional more orderly structure between the preparation rete, functions such as the light of realization film, electricity, magnetic.Therefore, receive attention widely in recent years.Lean on electrostatic adhesion and valence bond cooperation with the preparation film but the liquid phase self-assembling technique prepares the function ceramics film, reactive force is less, has the low defective of film compactness of preparation, causes the dielectric properties and the ferroelectric properties of the film of this method preparation to test.
Therefore the method that provides the self-assembly of a kind of technology raising glass substrate liquid phase to prepare the density film becomes the present assistant officer in this area technical problem to be solved.
[summary of the invention]
The object of the present invention is to provide a kind of on glass substrate the method for deposition compact barium strontium titanate; This method utilizes vacuum-treat precursor liquid technology to prepare fine and close barium strontium titanate with repeatedly inducing absorption liquid phase self-assembly method at glass substrate; It not only can reach high surface compact degree, and functionalization is even, processing technological flow is simple, easy to operate.
To achieve these goals, the present invention adopts following technical scheme:
A kind of on glass substrate the method for deposition compact barium strontium titanate, may further comprise the steps:
Step 1: configuration precursor liquid solution: with Ba (NO
3)
2, Sr (NO
3)
2, (NH
4)
2TiF
6, H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation are even, after the vibration four kinds of solution poured in the beaker, and constant volume makes Ba (NO
3)
2Concentration be 0.002mol/L, Sr (NO
3)
2Concentration be 0.008mol/L, (NH
4)
2TiF
6Concentration be 0.01mol/L, H
3BO
3Concentration be 0.03mol/L; Place on the magnetic stirring apparatus at last to stir, dripping the nitre acid for adjusting pH value then is 2.0～3.1, makes the solution clear promptly get precursor liquid solution;
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker carry out vacuum-treat, open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 30-60mins, to making precursor liquid solution not have bubble to discharge;
Step 3: will have the wetting ability glass substrate of OTS unimolecular film to put into the self-assembled growth that precursor liquid solution after the vacuum-treat carries out film, depositing temperature is 50 ℃, and depositing time is 18～24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
The present invention further improves and is: said method is further comprising the steps of between step 3 and step 4; Step 3.1: repeating step 1,2; Then the last time is carried out glass substrate behind the self-assembled growth of film and put into the self-assembled growth that precursor liquid solution after the vacuum-treat carries out film; Depositing temperature is 50 ℃, and depositing time is 18～24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h.
The present invention further improves and is: before step 4 anneal, and repeating step 3.1 several times.
The present invention further improves and is: before step 4 anneal, and repeating step 3.1 3 to four times.
To achieve these goals, the present invention can also adopt following technical scheme:
A kind of on glass substrate the method for deposition compact barium strontium titanate, may further comprise the steps:
Step 1: configuration precursor liquid solution: with 0.0002mol Ba (NO
3)
2, 0.0008mol Sr (NO
3)
2, 0.001mol (NH
4)
2TiF
6, 0.003mol H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation 10min pours four kinds of solution in the beaker into after the vibration, is settled to 100ml; Place at last and stir 10min on the magnetic stirring apparatus, take off after having vibrated; Dripping rare nitre acid for adjusting pH value is 3.1, makes the solution clear promptly get precursor liquid solution;
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker, and open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 45mins, does not have bubble to discharge to solution;
Step 3: will have the wetting ability glass substrate of OTS unimolecular film to put into the self-assembled growth that precursor liquid solution after step 2 is handled carries out film, depositing temperature is 50 ℃, and depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: repeating step 1,2, front suction is placed the precursor liquid that does not have bubble with the glass substrate of precursor liquid solution, liquid phase self-assembly adsorbent thin film, depositing temperature is 50 ℃, depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h; Repeat above process three times;
Step 5: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
The present invention is with respect to prior art, and it has following beneficial effect: the inventive method overcomes the sol-gel method film and is prone to be full of cracks, and the starting material of the heavy method of Organometallic Chemistry gas phase and the price of equipment are all very expensive; Uniformity of film is poor in the pulsed laser deposition, and growth velocity is slow in the magnetron sputtering method, the shortcoming of the technology such as defective that existing liquid phase self-assembly process technique film compactness is low; Utilize vacuum-treat precursor liquid technology to prepare fine and close barium strontium titanate with repeatedly inducing absorption liquid phase self-assembly method at glass substrate, it not only can reach high surface compact degree, and functionalization is even, processing technological flow is simple, easy to operate.
[description of drawings]
Fig. 1: be the barium strontium titanate XRD figure (precursor liquid vacuumizes 45min, and the absorption inducing temperature is 50 ℃, and adsorption time is 24h, adsorbs three times) that the present invention prepares;
Fig. 2: be the barium strontium titanate SEM figure (precursor liquid vacuumizes 45min, and the absorption inducing temperature is 50 ℃, and adsorption time is 24h, adsorbs three times) that the present invention prepares;
Fig. 3 is the barium strontium titanate SEM figure (do not carry out precursor liquid and vacuumize 45min, the absorption inducing temperature is 50 ℃, and adsorption time is 24h, adsorbs three times) that the present invention prepares.
[embodiment]
Embodiment 1:
Step 1: configuration precursor liquid solution: with 0.0002mol Ba (NO
3)
2, 0.0008mol Sr (NO
3)
2, 0.001mol (NH
4)
2TiF
6, 0.003mol H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation 10min pours four kinds of solution in the beaker into after the vibration, is settled to 100mL; Place at last and stir 10min on the magnetic stirring apparatus, take off after having vibrated.Dripping rare nitre acid for adjusting pH value is 3.1, makes the solution clear promptly get precursor liquid solution.
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker, and open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 45mins, does not have bubble to discharge to solution;
Step 3: OTS (octadecyl-trichloro-silane will be arranged; The octadecyl trichlorosilane) the precursor liquid solution after the wetting ability glass substrate of unimolecular film is put into step 2 and handled carries out the self-assembled growth of film; Depositing temperature is 50 ℃; Depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: prepare precursor aqueous solution again, be-0.2Kg/cm in vacuum tightness
2, the pumpdown time is 45mins, causing solution does not have bubble to discharge; The glass substrate of front suction being had precursor liquid solution places the precursor liquid that does not have bubble, liquid phase self-assembly adsorbent thin film, and depositing temperature is 50 ℃; Depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h; Repeat above process three times;
Step 5: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
Embodiment 2:
Step 1: configuration precursor liquid solution: with 0.0002mol Ba (NO
3)
2, 0.0008mol Sr (NO
3)
2, 0.001mol (NH
4)
2TiF
6, 0.003mol H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation 10min pours four kinds of solution in the beaker into after the vibration, is settled to 100mL; Place at last and stir 10min on the magnetic stirring apparatus, take off after having vibrated.Dripping rare nitre acid for adjusting pH value is 2.0, makes the solution clear promptly get precursor liquid solution.
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker, and open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 60mins, does not have bubble to discharge to solution;
Step 3: OTS (octadecyl-trichloro-silane will be arranged; The octadecyl trichlorosilane) the precursor liquid solution after the wetting ability glass substrate of unimolecular film is put into step 2 and handled carries out the self-assembled growth of film; Depositing temperature is 50 ℃; Depositing time is 20h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: prepare precursor aqueous solution again, be-0.2Kg/cm in vacuum tightness
2, the pumpdown time is 60mins, does not have bubble to discharge to solution; The glass substrate of front suction being had precursor aqueous solution places the precursor liquid that does not have bubble, liquid phase self-assembly adsorbent thin film, and depositing temperature is 50 ℃; Depositing time is 20h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h; Repeat above process four times,
Step 5: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
Embodiment 3:
Step 1: configuration precursor liquid solution: with 0.0002mol Ba (NO
3)
2, 0.0008mol Sr (NO
3)
2, 0.001mol (NH
4)
2TiF
6, 0.003mol H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation 10min pours four kinds of solution in the beaker into after the vibration, is settled to 100mL; Place at last and stir 10min on the magnetic stirring apparatus, take off after having vibrated.Dripping rare nitre acid for adjusting pH value is 2.5, makes the solution clear promptly get precursor liquid solution.
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker, and open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 30mins, does not have bubble to discharge to solution;
Step 3: OTS (octadecyl-trichloro-silane will be arranged; The octadecyl trichlorosilane) the precursor liquid solution after the wetting ability glass substrate of unimolecular film is put into step 2 and handled carries out the self-assembled growth of film; Depositing temperature is 50 ℃; Depositing time is 18h, with glass substrate at 120 ℃ of dry 12h;
Step 4: prepare precursor aqueous solution again, be-0.2Kg/cm in vacuum tightness
2, the pumpdown time is 30mins, does not have bubble to discharge to solution; The glass substrate of front suction being had precursor aqueous solution places the precursor liquid that does not have bubble, liquid phase self-assembly adsorbent thin film, and depositing temperature is 50 ℃; Depositing time is 18h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h; Repeat above process three times;
Step 5: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
The inventive method, based on the thickness of the barium strontium titanate that will prepare, can repeat liquid phase self assembly absorption repeatedly, also can only carry out liquid phase self assembly absorption.
See also Fig. 1 to shown in Figure 3, Fig. 1 is the prepared barium strontium titanate XRD figure of the embodiment of the invention 1; Fig. 2 is the barium strontium titanate SEM figure of the embodiment of the invention 1 preparation; Fig. 3 does not carry out the barium strontium titanate SEM figure that precursor liquid vacuumizes preparation.Through analysis to Fig. 1 to Fig. 3, utilize this technology can make the barium strontium titanate on the glass substrate reach high surface compact degree, and functionalization is even, processing technological flow is simple, easy to operate.More tiny than there not being glass substrate processed (like Fig. 3) surface particles through vacuumizing glass substrate processed (like Fig. 2), size is even, and it is fine and close to distribute.Can know through the XRD figure analysis, sharp-pointed through the strontium-barium titanate diffraction peak that vacuumizes on the glass substrate processed, explain that percent crystallinity is good.
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 (5)
1. the method for a deposition compact barium strontium titanate on glass substrate is characterized in that, may further comprise the steps:
Step 1: configuration precursor liquid solution: with Ba (NO
3)
2, Sr (NO
3)
2, (NH
4)
2TiF
6, H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation are even, after the vibration four kinds of solution poured in the beaker, and constant volume makes Ba (NO
3)
2Concentration be 0.002mol/L, Sr (NO
3)
2Concentration be 0.008mol/L, (NH
4)
2TiF
6Concentration be 0.01mol/L, H
3BO
3Concentration be 0.03mol/L; Place on the magnetic stirring apparatus at last to stir, dripping rare nitre acid for adjusting pH value then is 2.0～3.1, makes the solution clear promptly get precursor liquid solution;
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker carry out vacuum-treat, open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 30-60mins, to making precursor liquid solution not have bubble to discharge;
Step 3: will have the wetting ability glass substrate of OTS unimolecular film to put into the self-assembled growth that precursor liquid solution after the vacuum-treat carries out film, depositing temperature is 50 ℃, and depositing time is 18～24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
2. method according to claim 1 is characterized in that, said method is further comprising the steps of between step 3 and step 4:
Step 3.1: repeating step 1,2; Then the last time is carried out glass substrate behind the self-assembled growth of film and put into the self-assembled growth that precursor liquid solution after the vacuum-treat carries out film; Depositing temperature is 50 ℃; Depositing time is 18～24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h.
3. method according to claim 2 is characterized in that, before step 4 anneal, and repeating step 3.1 several times.
4. method according to claim 2 is characterized in that, before step 4 anneal, and repeating step 3.1 3 to four times.
5. the method for a deposition compact barium strontium titanate on glass substrate is characterized in that, may further comprise the steps:
Step 1: configuration precursor liquid solution: with 0.0002mol Ba (NO
3)
2, 0.0008mol Sr (NO
3)
2, 0.001mol (NH
4)
2TiF
6, 0.003mol H
3BO
3Put into 4 beakers respectively; In 4 beakers, add deionized water respectively then, ultra-sonic oscillation 10min pours four kinds of solution in the beaker into after the vibration, is settled to 100ml; Place at last and stir 10min on the magnetic stirring apparatus, take off after having vibrated; Dripping rare nitre acid for adjusting pH value is 3.1, makes the solution clear promptly get precursor liquid solution;
Step 2: the precursor liquid solution couplet that configures is put into vacuum chamber with beaker, and open vacuum pump, vacuum pressure are adjusted to-0.2Kg/cm
2, the pumpdown time is 45mins, does not have bubble to discharge to solution;
Step 3: will have the wetting ability glass substrate of OTS unimolecular film to put into the self-assembled growth that precursor liquid solution after step 2 is handled carries out film, depositing temperature is 50 ℃, and depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h;
Step 4: repeating step 1,2, front suction is placed the precursor liquid that does not have bubble with the glass substrate of precursor liquid solution, liquid phase self-assembly adsorbent thin film, depositing temperature is 50 ℃, depositing time is 24h, after deposition is accomplished with glass substrate at 120 ℃ of dry 12h; Repeat above process three times;
Step 5: will deposit good film carries out 2h under 600 ℃ of conditions anneal at last; Obtain fine and close barium strontium titanate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102795853A (en) * | 2012-07-09 | 2012-11-28 | 陕西科技大学 | Method for preparing Bi2Ti2O7 dielectric ceramic film on surface of FTO (fluorine-doped tin oxide) substrate |
| US20150249172A1 (en) * | 2013-11-26 | 2015-09-03 | Hunt Energy Enterprises, L.L.C. | Titanate interfacial layers in perovskite material devices |
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| CN101654779A (en) * | 2009-08-28 | 2010-02-24 | 陕西科技大学 | Preparation method of Bi3.2Nd0.8Ti3O12 ferroelectric film |
| CN101955323A (en) * | 2010-09-20 | 2011-01-26 | 陕西科技大学 | Method for preparing bismuth titanate functional membrane on glass substrate |
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2012
- 2012-02-24 CN CN2012100442027A patent/CN102534610A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101654779A (en) * | 2009-08-28 | 2010-02-24 | 陕西科技大学 | Preparation method of Bi3.2Nd0.8Ti3O12 ferroelectric film |
| CN101955323A (en) * | 2010-09-20 | 2011-01-26 | 陕西科技大学 | Method for preparing bismuth titanate functional membrane on glass substrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795853A (en) * | 2012-07-09 | 2012-11-28 | 陕西科技大学 | Method for preparing Bi2Ti2O7 dielectric ceramic film on surface of FTO (fluorine-doped tin oxide) substrate |
| US20150249172A1 (en) * | 2013-11-26 | 2015-09-03 | Hunt Energy Enterprises, L.L.C. | Titanate interfacial layers in perovskite material devices |
| US9520512B2 (en) * | 2013-11-26 | 2016-12-13 | Hunt Energy Enterprises, L.L.C. | Titanate interfacial layers in perovskite material devices |
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Application publication date: 20120704 |