The effect of intermediate anneal on the ferroelectric properties of direct-patternable PZT films

Jae Seob Hwang; Woo Sik Kim; Hyung Ho Park; Tae Song Kim

doi:10.1016/j.sna.2004.05.033

The effect of intermediate anneal on the ferroelectric properties of direct-patternable PZT films

Jae Seob Hwang, Woo Sik Kim, Hyung Ho Park, Tae Song Kim

Department of Materials Science and Engineering

Research output: Contribution to journal › Article › peer-review

18 Citations (Scopus)

Abstract

The effect of intermediate annealing ambient was investigated for the preparation of thick direct-patternable lead zirconium titanate (PbZr _xTi_1-xO₃; PZT, x = 0.52) films using photosensitive stock solution containing diethanolamine (DEA) as stabilizer and ortho-nitrobenzaldehyde (NBAL) as cross-linking agent by metal-organic deposition method. The intermediate anneal was done at 400°C; for 20 min under air or O₂ ambient. The intermediate anneal under O₂ brought almost complete removal of organic species, however after anneal under air, carbon and hydrogen atomic species as organic fragment remained in the film. This incomplete removal of organic fragments induced the grain growth of PZT film without influencing from Pt substrate and the formation of micro-voids on film surface during final anneal for the crystallization of PZT film with perovskite structure. The growth direction and surface microstructure of PZT film was revealed to highly affect on leakage, capacitance, fatigue, and piezoelectric properties of PZT film. For PZT film with intermediate anneal under O₂, a good piezoelectric property, d₃₃ = 336 pC/N was obtained with pneumatic loading method, and this film showed 26.2 μC/cm² of remnant polarization (P_r), 35.6kV/cm of coercive field (E_c) and well-developed and saturated hysteretic loop. The dielectric constant was obtained as 1795 from the C-V measurement at 1 MHz and 40% of initial polarization value was remained after 10⁹ switching cycles through bipolar square wave of ±10 V at 500 kHz. From the comparison of physical and electrical properties of PZT films prepared with different intermediate anneal ambient such as O₂ or air, it can be said that the intermediate annealing condition is very important procedure to control the properties of PZT film for applying it to piezoelectric system devices.

Original language	English
Pages (from-to)	137-142
Number of pages	6
Journal	Sensors and Actuators, A: Physical
Volume	117
Issue number	1
DOIs	https://doi.org/10.1016/j.sna.2004.05.033
Publication status	Published - 2005 Jan 3

Bibliographical note

Funding Information:
This research, under the contract project code MS-02-133-01, has been supported by the intelligent Microsystem Research Center (IMC: http://www.microsystem.re.kr ), which carries out one of the 21st century’s Frontier R & D Projects sponsored by the Korea Ministry of Science & Technology.

All Science Journal Classification (ASJC) codes

Electronic, Optical and Magnetic Materials
Instrumentation
Condensed Matter Physics
Surfaces, Coatings and Films
Metals and Alloys
Electrical and Electronic Engineering

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10.1016/j.sna.2004.05.033

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title = "The effect of intermediate anneal on the ferroelectric properties of direct-patternable PZT films",

abstract = "The effect of intermediate annealing ambient was investigated for the preparation of thick direct-patternable lead zirconium titanate (PbZr xTi1-xO3; PZT, x = 0.52) films using photosensitive stock solution containing diethanolamine (DEA) as stabilizer and ortho-nitrobenzaldehyde (NBAL) as cross-linking agent by metal-organic deposition method. The intermediate anneal was done at 400°C; for 20 min under air or O2 ambient. The intermediate anneal under O2 brought almost complete removal of organic species, however after anneal under air, carbon and hydrogen atomic species as organic fragment remained in the film. This incomplete removal of organic fragments induced the grain growth of PZT film without influencing from Pt substrate and the formation of micro-voids on film surface during final anneal for the crystallization of PZT film with perovskite structure. The growth direction and surface microstructure of PZT film was revealed to highly affect on leakage, capacitance, fatigue, and piezoelectric properties of PZT film. For PZT film with intermediate anneal under O2, a good piezoelectric property, d33 = 336 pC/N was obtained with pneumatic loading method, and this film showed 26.2 μC/cm2 of remnant polarization (Pr), 35.6kV/cm of coercive field (Ec) and well-developed and saturated hysteretic loop. The dielectric constant was obtained as 1795 from the C-V measurement at 1 MHz and 40% of initial polarization value was remained after 109 switching cycles through bipolar square wave of ±10 V at 500 kHz. From the comparison of physical and electrical properties of PZT films prepared with different intermediate anneal ambient such as O2 or air, it can be said that the intermediate annealing condition is very important procedure to control the properties of PZT film for applying it to piezoelectric system devices.",

author = "Hwang, {Jae Seob} and Kim, {Woo Sik} and Park, {Hyung Ho} and Kim, {Tae Song}",

note = "Funding Information: This research, under the contract project code MS-02-133-01, has been supported by the intelligent Microsystem Research Center (IMC: http://www.microsystem.re.kr ), which carries out one of the 21st century{\textquoteright}s Frontier R & D Projects sponsored by the Korea Ministry of Science & Technology. ",

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N1 - Funding Information: This research, under the contract project code MS-02-133-01, has been supported by the intelligent Microsystem Research Center (IMC: http://www.microsystem.re.kr ), which carries out one of the 21st century’s Frontier R & D Projects sponsored by the Korea Ministry of Science & Technology.

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The effect of intermediate anneal on the ferroelectric properties of direct-patternable PZT films

Abstract

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