CN1513809A - Preparation method of high performance lead zirconium titanate thin film - Google Patents
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- CN1513809A CN1513809A CNA021606803A CN02160680A CN1513809A CN 1513809 A CN1513809 A CN 1513809A CN A021606803 A CNA021606803 A CN A021606803A CN 02160680 A CN02160680 A CN 02160680A CN 1513809 A CN1513809 A CN 1513809A
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Abstract
A process for preparing the high-performance ferroelectric lead zirconate titanate (PZT) film includes preparing its precursor solution by sol-gel method, preparing the substrte with PZT crystal seed layer, atomizing and accelerating said precursor solution to deposit it on said substrate to become film, and heat treating. Its advantages are high growth speed, low cost, great thickness and excellent piezoelectric and dielectric performance.
Description
Technical field:
The invention belongs to the preparation method of ferroelectric ceramic material, especially relate to the preparation method of ferroelectric lead zirconate titanate film.
Background technology:
(molecular formula is Pb (Zr to Pb-based lanthanumdoped zirconate titanates
xTi
1-x) O
3, be called for short PZT) as a kind of ferroelectric material of excellent performance, in microelectronics, be used widely already, as make non-volatile dynamic RAM (FRAM).In recent years, along with the development of microsystems technology, advantages such as the high piezoelectric constant of PZT and high-k are well suited for microsensor and the mini drive of manufacturing in the micro-system, are considered to one of the most promising sensing and driving material in the micro-system field.Be applied to the PZT ferroelectric membranc that microdrive is made, should have excellent piezoelectric property and the thickness more than 2 microns simultaneously, for device provides enough power.At present among the preparation method of PZT ferroelectric membranc commonly used, the film that makes with sol-gel method has excellent piezoelectricity, dielectric properties, but in the heat treatment process of wet film, because the volume of film can take place to shrink significantly, thereby between the inside of film and film and substrate, produce very big internal stress, the individual layer thickness that causes the most very much not ftractureing has only 0.1～0.2 micron, and the number of plies of film is when too much, can make heat treatment time long, cause the Pt bottom electrode to the PZT internal divergence, therefore be difficult to obtain thickness at the PZT ferroelectric membranc more than 2 microns; Other preparation method, as: magnetron sputtering method, laser pulse deposit, hydrothermal method, chemical vapor deposition etc., though can make thickness at the PZT ferroelectric membranc more than 2 microns, all equipment complexity, cost are very high, and be difficult to obtain excellent piezoelectric property (preferred orientation is poor).
Summary of the invention:
The object of the present invention is to provide and a kind ofly can under the prerequisite that guarantees PZT ferroelectric membranc excellent properties, obtain the preparation method of big film thickness simultaneously.
Technical solution of the present invention is as follows:
The preparation process of film is: 1. with sol-gel method preparation precursor aqueous solution; 2. make the substrate that has PZT crystallization Seed Layer; 3. with precursor aqueous solution atomizing and quicken, make it to be deposited on and form film on the substrate; And substrate and film heat-treated.
Perhaps: 1. with sol-gel method preparation precursor aqueous solution; 2. make the substrate that has PZT crystallization Seed Layer; 3. with precursor aqueous solution atomizing and quicken, make it to be deposited on and form film on the substrate, adopt the rotary plating method to plate one deck PZT film thereon again during every plated film 0.5～1 micron thickness; And substrate and film heat-treated.
The preparation process of described substrate is: adopt the rotary plating method at Pt/Ti/SiO
2Apply the PZT wet film on the/Si substrate, and wet film was toasted 40 minutes at 350～400 ℃,, form the strong PZT ferroelectric membranc that is orientated as the crystallization Seed Layer along (100) crystal orientation again 600 ℃ of bakings 15 minutes.
Described atomization process is: precursor aqueous solution is packed in the container of electrospray device, substrate is placed on the heated plate of shower nozzle below ground connection, precursor aqueous solution sprays, forms the uniform charged droplet of diameter in micron dimension from shower nozzle under the high-voltage electric field effect, under the booster action of electric field, droplet also finally deposits to substrate motion at a high speed and forms pzt thin film on the substrate.
Described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 20 ℃, less than 300 ℃; During every plated film 0.5～1 micron thickness with substrate and film 300～400 ℃ of bakings 40～60 minutes, again 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.Perhaps, in the atomization process to substrate heating and keep underlayer temperature more than or equal to 300 ℃, less than 400 ℃; During every plated film 1～2 micron thickness with substrate and film 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
That is to say that the present invention has done improvement to sol-gel method, formed a kind of new colloidal sol-electrospray method: at first utilize sol-gel method preparation precursor aqueous solution; Under the effect of high-voltage electric field, electrostatic force overcomes the surface tension of liquid then, makes precursor aqueous solution form charged droplet of uniform size, droplet under the acceleration of electric field at a high speed to substrate motion, thereby in the substrate surface film forming.Concrete grammar is as follows:
1. prepare the Pb-based lanthanumdoped zirconate titanates precursor aqueous solution with the sol-gel method of routine: used lead, zirconium, titanium three's salt should adopt easy volatile solvent to make, and is good with plumbic acetate, propyl alcohol zirconium, titanium isopropylate wherein.Earlier Glacial acetic acid lead is dissolved in acetic acid, the molconcentration ratio according to lead, zirconium, titanium three is Pb: Zr: Ti=1: X then: (1-X) ratio of (wherein 0＜X＜1) adds propyl alcohol zirconium and titanium isopropylate successively.Through vibration of ultrasonic wave, make solution stirring evenly after, adding with the volume ratio is deionized water: acetic acid: the mixing solutions of deionized water, acetic acid and Virahol that the mixed of Virahol=3: 5: 10 forms.Again through vibration of ultrasonic wave, make solution stirring evenly after, finally obtaining concentration is the PZT precursor aqueous solution (if concentration is improper, also available acetic acid and Virahol are suitably adjusted solution) of 0.4～0.5 mol.Formed precursor aqueous solution is water white liquid.
2. make substrate: at Pt/Ti/SiO commonly used
2Employing rotary plating legal system is equipped with the PZT ferroelectric membranc of individual layer (about 80～120 nanometer thickness) on/Si substrate, and wet film was toasted 40 minutes at 350～400 ℃, again 600 ℃ of bakings 15 minutes, makes it to be orientated strongly along (100) crystal orientation.Crystallization Seed Layer when it can be used as film growth in the subsequent process also can be orientated the PZT ferroelectric membranc of spray deposition strongly along (100) crystal orientation.
3. with precursor aqueous solution atomizing, make it to be deposited on and form film on the substrate: atomisation unit can adopt conventional electrospray device.It comprises (as shown in Figure 1) such as precursor aqueous solution plenum system, dc high-voltage origin system, temperature controlling systems.The PZT precursor aqueous solution is added in the container of electrospray device, advance by direct-current machine; Substrate is placed on the heated plate of shower nozzle below, but heated plate ground connection is to use as ground electrode; Atomizer is a tubulose, and internal diameter is below 1 millimeter; Under the high direct voltage of thousands of volts (about 4000～7000 volts), precursor aqueous solution is atomized into the charged droplet (see figure 2) that diameter is a micron dimension (0.5～2 micron) in the shower nozzle exit.In the scope of 70～90 ° of angles of divergence, size, the speed of droplet are even, form even mist field.Droplet at a high speed to substrate motion, is deposited on the Pt/Ti/SiO of crystallization Seed Layer under the acceleration of electric field
2On/Si the substrate, form wet film.Distance between shower nozzle and the substrate should be decided (for the substrate of diameter at 2～3 inches, the distance between shower nozzle and the substrate is generally 5～8 centimetres) according to the area size of the PZT ferroelectric membranc of the angle of divergence of even mist field and required preparation; Solution flow then on shower nozzle internal diameter size and and substrate between the voltage height decide (being generally 0.4～1 milliliter/hour); The height of voltage is then decided on the distance between precursor aqueous solution specific conductivity and shower nozzle and the substrate.
Substrate and film are heat-treated: under the effect of substrate heating, the solvent in the wet film is able to continuous volatilization, helps to form continuous stressless film.The substrate heating can realize by heated plate.If control underlayer temperature be 20～100 ℃ (more than or equal to 20 ℃, less than 100 ℃) time, during about 0.5 micron thickness of every plated film, substrate and film are put into resistance furnace 300～400 ℃ of bakings 40～60 minutes (remaining organic solvent is volatilized fully), and then about 600 ℃, toast 15～20 minutes (film that promotes to have prepared is along (100) crystal orientation crystallization, to guarantee preferred orientation); If the control underlayer temperature be 100～300 ℃ (more than or equal to 100 ℃, less than 300 ℃) time, carry out above-mentioned baking during about 1 micron thickness of every plated film; If the control underlayer temperature be 300～400 ℃ (more than or equal to 300 ℃, less than 400 ℃) time, during about 2 micron thickness of every plated film directly 600 ℃ of bakings 15～20 minutes.Substrate and the film that reaches desired thickness 600 ℃ of annealing 2～4 hours down in the saturated atmosphere of PbO the most at last make the big thickness PZT ferroelectric membranc of the strong orientation along (100) crystal orientation.
In sum, colloidal sol-electrospray legal system that the present invention adopts is equipped with the PZT ferroelectric membranc, compares with traditional sol-gel method, has outstanding advantage: accurate, the control easily of the composition of 1. having inherited sol-gel method, device is simple, cost is low, and advantage such as gained film preferred orientation; 2. underlayer temperature can be set to suitable temperature as required arbitrarily in the preparation process, because the formation of wet film is a successive process, under the effect of underlayer temperature, the internal stress that the wet film volumetric shrinkage causes can obtain release progressively, therefore film growth rates is fast, and the individual layer thickness under 25 ℃, 100 ℃ and 350 ℃ can reach 0.5 micron, 1 micron, 2 microns respectively.3. since in the atomization process waste of precursor aqueous solution few, thereby soln using rate height; 4. apparatus structure is simple, cost is very low, and can be compatible mutually with MEMS (micro electro mechanical system) complete processing commonly used, helps getting involved on the production line of microsensor or mini drive.The PZT ferroelectric membranc that utilizes the present invention to prepare can obtain big film thickness and excellent film performance (and having excellent piezoelectricity, dielectric properties simultaneously) simultaneously, can satisfy the needs of microsensor and mini drive in the micro-system substantially.
Description of drawings:
Figure 1 shows that electrospray process and schematic representation of apparatus.Figure 2 shows that formation photo one example of shower nozzle exit drop atomizing.Figure 3 shows that the XRD spectrum of the PZT ferroelectric membranc that (example 1) made when underlayer temperature was 25 ℃, film becomes single uhligite phase, and is orientated strongly along (100) crystal orientation.Figure 4 shows that the atomic force micrograph of the PZT ferroelectric membranc that (example 2) made when underlayer temperature was 100 ℃, the homogeneous grain size unanimity is about 0.2 micron.Figure 5 shows that the light micrograph of the PZT ferroelectric membranc that (example 3) made when underlayer temperature was 350 ℃, the smooth surface flawless; Figure 6 shows that the ferroelectric hysteresis loop of the PZT ferroelectric membranc that (example 4) made when underlayer temperature was 25 ℃, show the residual polarization 12.5 μ c/cm of film
2, the strong 32kV/cm of coercive field.
Embodiment:
Further illustrate substantive distinguishing features of the present invention and obvious improvement below by example, yet the present invention only limits to described example by no means.
Example 1
Glacial acetic acid lead is dissolved in acetic acid, and the molconcentration ratio according to lead, zirconium, titanium three is Pb: Zr: Ti=1 then: 0.53: 0.47 ratio adds propyl alcohol zirconium and titanium isopropylate successively.After stirring with vibration of ultrasonic wave, adding with the volume ratio is deionized water: acetic acid: the mixing solutions of deionized water, acetic acid and the Virahol of Virahol=mix at 3: 5: 10.After vibration of ultrasonic wave stirs, use acetic acid and Virahol with solution dilution to 0.4 mol.Obtained precursor aqueous solution is added electrospray device, and flow control is 0.6 milliliter/hour, and the atomizer internal diameter is 0.25 millimeter, and the distance between shower nozzle and the substrate is 5 centimetres, adds 4500 volts volts DS.Used substrate is: basis thermal oxidation method before prepares SiO on the Si substrate
2Film, sputtering method prepare Ti film and Pt film, again at this Pt/Ti/SiO
2Employing rotary plating method has prepared the PZT crystallization Seed Layer of individual layer 100 nanometer thickness on the/Si substrate, and wet film was toasted 40 minutes at 350 ℃, again 600 ℃ of bakings 15 minutes, makes it to be orientated strongly along (100) crystal orientation.Substrate temperature is set at 25 ℃, the plated film time is 20 minutes, wherein every plated film 5 minutes clock time (about 0.5 micron thickness) is put into resistance furnace 350 ℃ of bakings 60 minutes with substrate and film, again 600 ℃ of bakings 20 minutes, then substrate and the film that reaches desired thickness were annealed 4 hours in 600 ℃ of saturated atmosphere of PbO, obtain complete uhligite phase and the thickness of strong orientation is 2 microns PZT ferroelectric membranc along (100) crystal orientation.
Example 2
All the other conditions are with example 1, and dominant discharge is 0.8 milliliter/hour, and the atomizer internal diameter is 0.4 millimeter, and the distance between shower nozzle and the substrate is 6 centimetres, adds 4800 volts volts DS.Underlayer temperature is set at 100 ℃, the plated film time is 20 minutes, wherein every plated film 10 minutes clock time (about 1 micron thickness) is put into resistance furnace 350 ℃ of bakings 40 minutes with substrate and film, again 600 ℃ of bakings 20 minutes, then substrate and the film that reaches desired thickness were annealed 4 hours in 600 ℃ of saturated atmosphere of PbO, obtain complete uhligite phase and the thickness of strong orientation is 2 microns PZT ferroelectric membranc along (100) crystal orientation.
Example 3
All the other conditions are with example 1, and dominant discharge is 1 milliliter/hour, and the atomizer internal diameter is 0.6 millimeter, and the distance between shower nozzle and the substrate is 7 centimetres, adds 5500 volts volts DS.Underlayer temperature is set at 350 ℃, the plated film time is 40 minutes, wherein every plated film 20 minutes clock time (about 2 micron thickness) is put into resistance furnace 600 ℃ of bakings 15 minutes with substrate and film, then substrate and the film that reaches desired thickness were annealed 2 hours in 600 ℃ of saturated atmosphere of PbO, obtain complete uhligite phase and be 4 microns PZT ferroelectric membranc along the thickness of (100) crystal orientation preferred orientation.
Example 4
All the other conditions are with example 1, underlayer temperature is set at 25 ℃, the plated film time is 20 minutes, and every plated film 5 minutes, after same thermal treatment, with rotary plating method plating one deck PZT film (about 100 nanometer thickness), with the compactness and the preferred orientation of enhanced film, the PZT film of rotary plating method preparation also will be through Overheating Treatment, 350 ℃ of bakings 40 minutes,, obtain the PZT ferroelectric membranc of 2 micron thickness again 600 ℃ of bakings 15 minutes, be complete uhligite phase, and be orientated strongly along (100) crystal orientation.The relative permittivity of film is 960, residual polarization 12.5 μ c/cm
2, the strong 32kV/cm of coercive field.
Claims (11)
1, a kind of preparation method of high-performance PZT thin film is characterized in that: preparation process is: 1. with sol-gel method preparation precursor aqueous solution; 2. make the substrate that has PZT crystallization Seed Layer; 3. with precursor aqueous solution atomizing and quicken, make it to be deposited on and form film on the substrate; And substrate and film heat-treated.
2, a kind of preparation method of high-performance PZT thin film is characterized in that: preparation process is: 1. with sol-gel method preparation precursor aqueous solution; 2. make the substrate that has PZT crystallization Seed Layer; 3. with precursor aqueous solution atomizing and quicken, make it to be deposited on and form film on the substrate, adopt the rotary plating method to plate one deck PZT film thereon again during every plated film 0.5～1 micron thickness; And substrate and film heat-treated.
3, preparation method as claimed in claim 1 or 2 is characterized in that: the preparation process of described substrate is: adopt the rotary plating method at Pt/Ti/SiO
2Apply the PZT wet film on the/Si substrate, and wet film was toasted 40 minutes at 350～400 ℃,, form the strong PZT ferroelectric membranc that is orientated as the crystallization Seed Layer along (100) crystal orientation again 600 ℃ of bakings 15 minutes; The thickness of crystallization Seed Layer is controlled in 80～120 nanometers.
4, preparation method as claimed in claim 1 or 2, it is characterized in that: described atomization process is: precursor aqueous solution is packed in the container of electrospray device, substrate is placed on the heated plate of shower nozzle below ground connection, precursor aqueous solution sprays, forms the uniform charged droplet of diameter in micron dimension from shower nozzle under the high-voltage electric field effect, under the booster action of electric field, droplet also finally deposits to substrate motion at a high speed and forms pzt thin film on the substrate.
5, preparation method as claimed in claim 3, it is characterized in that: described atomization process is: precursor aqueous solution is packed in the container of electrospray device, substrate is placed on the heated plate of shower nozzle below ground connection, precursor aqueous solution sprays, forms the uniform charged droplet of diameter in micron dimension from shower nozzle under the high-voltage electric field effect, under the booster action of electric field, droplet also finally deposits to substrate motion at a high speed and forms pzt thin film on the substrate.
6, as claim 1 or 2 or 5 described preparation methods, it is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 20 ℃, less than 300 ℃; During every plated film 0.5～1 micron thickness with substrate and film 300～400 ℃ of bakings 40～60 minutes, again 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
7, preparation method as claimed in claim 3 is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 20 ℃, less than 300 ℃; During every plated film 0.5～1 micron thickness with substrate and film 300～400 ℃ of bakings 40～60 minutes, again 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
8, preparation method as claimed in claim 4 is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 20 ℃, less than 300 ℃; During every plated film 0.5～1 micron thickness with substrate and film 300～400 ℃ of bakings 40～60 minutes, again 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
9, as claim 1 or 2 or 5 described preparation methods, it is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 300 ℃, less than 400 ℃; During every plated film 1～2 micron thickness with substrate and film 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
10, preparation method as claimed in claim 3 is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 300 ℃, less than 400 ℃; During every plated film 1～2 micron thickness with substrate and film 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
11, preparation method as claimed in claim 4 is characterized in that: described heat treatment process is: in the atomization process to substrate heating and keep underlayer temperature more than or equal to 300 ℃, less than 400 ℃; During every plated film 1～2 micron thickness with substrate and film 600 ℃ of bakings 15～20 minutes; With the 600 ℃ of annealing 2～4 hours in the saturated atmosphere of PbO of substrate and the film that reaches desired thickness.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100355697C (en) * | 2006-03-03 | 2007-12-19 | 清华大学 | Method for preparing high curie point piezoelectric using water base sol-gel method |
| CN100365776C (en) * | 2005-09-23 | 2008-01-30 | 中国科学院上海技术物理研究所 | Production of thin-film ferroelectric materials with lead zirconate-titanate with reading circuit integration |
| CN100557737C (en) * | 2006-09-30 | 2009-11-04 | 中国科学技术大学 | Transparent epitaxial ferroelectric film capacitor and preparation method thereof |
| CN102992260A (en) * | 2011-08-17 | 2013-03-27 | 波音公司 | Method and system of fabricating PZT nanoparticle ink based piezoelectric sensor |
| CN107643228A (en) * | 2017-08-31 | 2018-01-30 | 中国船舶重工集团公司第七〇九研究所 | Measure chip of mercury vapour and preparation method thereof, sensor and its application method |
| CN109761605A (en) * | 2019-03-18 | 2019-05-17 | 大连瑞林数字印刷技术有限公司 | One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation |
| CN115974548A (en) * | 2022-12-16 | 2023-04-18 | 佛山仙湖实验室 | Lead-free high-entropy ferroelectric film and preparation method and application thereof |
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2002
- 2002-12-31 CN CNA021606803A patent/CN1513809A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365776C (en) * | 2005-09-23 | 2008-01-30 | 中国科学院上海技术物理研究所 | Production of thin-film ferroelectric materials with lead zirconate-titanate with reading circuit integration |
| CN100355697C (en) * | 2006-03-03 | 2007-12-19 | 清华大学 | Method for preparing high curie point piezoelectric using water base sol-gel method |
| CN100557737C (en) * | 2006-09-30 | 2009-11-04 | 中国科学技术大学 | Transparent epitaxial ferroelectric film capacitor and preparation method thereof |
| CN102992260A (en) * | 2011-08-17 | 2013-03-27 | 波音公司 | Method and system of fabricating PZT nanoparticle ink based piezoelectric sensor |
| CN102992260B (en) * | 2011-08-17 | 2016-08-17 | 波音公司 | Manufacture the method and system of PZT nanoparticle inks base piezoelectric transducer |
| CN107643228A (en) * | 2017-08-31 | 2018-01-30 | 中国船舶重工集团公司第七〇九研究所 | Measure chip of mercury vapour and preparation method thereof, sensor and its application method |
| CN109761605A (en) * | 2019-03-18 | 2019-05-17 | 大连瑞林数字印刷技术有限公司 | One kind having the PZT thin film and preparation method thereof of (100) preferable grain orientation |
| CN115974548A (en) * | 2022-12-16 | 2023-04-18 | 佛山仙湖实验室 | Lead-free high-entropy ferroelectric film and preparation method and application thereof |
| CN115974548B (en) * | 2022-12-16 | 2023-11-21 | 佛山仙湖实验室 | Leadless high-entropy ferroelectric film, preparation method and application thereof |
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