研究目的
To analyze the effect of PbOx and TiOx nucleation layers deposited by ALD on the crystallization of ALD PbTiO3 films and to provide detailed electronic characterization along with scanning transmission electron microscope cross-section images to inform the nucleation properties.
研究成果
ALD PbTiO3 films crystallized into phase-pure, randomly oriented perovskite grains with good ferroelectric and dielectric properties. Seed layers and RTA variations had minimal effect on texture. Electrical characterization showed promising figures of merit, with improvements after recovery anneals.
研究不足
The seed layers (PbOx and TiOx) did not significantly affect grain orientation due to random nucleation throughout the film. Films were not fully densified after a single anneal, requiring additional recovery anneals to improve electrical properties. Leakage current was higher in the negative field direction.
1：Experimental Design and Method Selection:
ALD was used for film deposition with specific precursors and oxidizers. Rapid thermal annealing (RTA) was employed for crystallization. Characterization methods included XRD, RBS, STEM, ellipsometry, impedance analysis, and ferroelectric testing.
2：Sample Selection and Data Sources:
Films were deposited on sputtered Pt-coated Si substrates. Samples with varying PbOx:TiOx cycle ratios (1:1 to 4:1) were prepared and analyzed.
3：List of Experimental Equipment and Materials:
ALD reactor (Kurt J. Lesker ALD-150LX), precursors (Pb(DMAMP)2, TDMAT), oxidizers (H2O, ozone), RTA systems (AG Associates 610, Allwin 21 810), ellipsometers (Film Sense FS-1, J.A. Woollam M-2000), XRD (Rigaku MiniFlex), STEM (FEI Titan G2), impedance analyzer (HP/Agilent 4192A), ferroelectric test system (Radiant Technologies RT66-A).
4：Experimental Procedures and Operational Workflow:
ALD deposition at 250°C with specific pulse and purge sequences. Post-deposition RTA at various temperatures and times. Top electrode deposition and patterning for electrical measurements. Characterization using XRD, RBS, STEM, ellipsometry, impedance, and ferroelectric tests.
5：Data Analysis Methods:
XRD for phase identification, RBS for stoichiometry, STEM for microstructure, ellipsometry for thickness and roughness, impedance analysis for dielectric properties, ferroelectric testing for polarization and leakage current.
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Ellipsometer
FS-1
Film Sense
In situ and ex situ thickness and roughness measurements
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Spectroscopic ellipsometer
M-2000
J.A. Woollam
Ex situ thickness and roughness measurements
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X-ray diffractometer
MiniFlex
Rigaku
Crystal phase and texture identification
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Ferroelectric test system
RT66-A
Radiant Technologies Inc.
Polarization vs voltage and leakage current measurements
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FIB/SEM system
Quanta 3D
FEI
Sample preparation for TEM
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STEM microscope
Titan G2
FEI
High-resolution imaging and chemical analysis
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ALD reactor
ALD-150LX
Kurt J. Lesker Company
Used for atomic layer deposition of PbTiO3 films
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Impedance analyzer
4192A
HP/Agilent
Capacitance and loss tangent measurements
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RTA system
610
AG Associates
Rapid thermal annealing for crystallization
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RTA system
810
Allwin 21
Alternative RTA for varying thermal treatments
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Ozone generator
Nano
Absolute Ozone
Supplying ozone as an oxidizer
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