Author Affiliations
1Laboratory of Thin Film Optics, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China2Key Laboratory of Materials for High Power Laser, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China3School of Optical-Electrical and Computer Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China4School of Physical Science and Technology, ShanghaiTech University, Shanghai 201210, Chinashow less
Fig. 1. Schematic diagrams of the structures of the nanolaminated films.
Fig. 2. Annealing programs of the samples at 400°C, 550°C, 700°C, and 850°C.
Fig. 3. Diffraction spectra of sample A-S0T4 before and after annealing; the inset shows the change in the diffraction angle.
Fig. 4. Surface morphologies of sample A-S0T4 before and after annealing: (a) before annealing, (b) after annealing at 400°C, (c) after annealing at 700°C, and (d) after annealing at 850°C.
Fig. 5. Diffraction spectra of the samples before and after annealing: (a) A-S1T3, (b) A-S2T2, and (c) A-S3T1.
Fig. 6. Surface morphologies of the samples before and after annealing: (a) before annealing of A-S1T3, (b) after annealing of A-S1T3 at 850°C, (c) before annealing of A-S2T2, (d) after annealing of A-S2T2 at 850°C, (e) before annealing of A-S3T1, and (f) after annealing of A-S3T1 at 850°C.
Fig. 7. XRR curves of sample A-S0T4 before and after annealing.
Fig. 8. Changes in the thickness and density of the four types of films with the annealing temperature.
Fig. 9. Changes in the elemental composition of the four types of films before and after annealing at 850°C.
Fig. 10. BE spectra for the four elements in different samples. (a) Ti 2p XPS core-line spectra: the BEs of Ti increased with decrease in the Ti content in the film before annealing. (b) Si 2p XPS core-line spectra: the BEs of Si increased with decrease in the Ti content in the film before annealing. (c) O 1s XPS core-line spectra: the BEs of O increased with decrease in the Ti content in the film before annealing. (d) Al 2p XPS core-line spectra: the BEs of Al increased with decrease in the Ti content in the film after annealing at 850°C.
Fig. 11. O 1s XPS core-line spectrum and the peak-fitting situation in sample A-S2T2 (a) before baking and (b) after annealing at 850°C.
Deposited Film | Precursor | Purity (N) | Precursor Temperature | Reaction Temperature (°C) | Thickness of One Circle (nm) |
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| 3DMAS () | | Room | 150 | 0.103 (S) | | TDMAT () | | 90°C | 150 | 0.057 (T) |
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Table 1. One Cycle of the SiO2 and TiO2 Process Conditions Using ALD
Sample | Total Thickness (nm) | Nano-Laminated Structure | Substrate |
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A-S0T4 | 30 | Sub/526T × 1 stack time | | A-S1T3 | 30 | Sub/(10S37T) × 10 stack times | | A-S2T2 | 30 | Sub/(10S12T) × 18 stack times | | A-S3T1 | 30 | Sub/(10S4T) × 24 stack times | |
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Table 2. Design Structures of the Nanolaminated Films
State | Type | Ti 2p | Si 2p | Al 2p | O 1s A (Ti–O) | O 1s B (Si–O) | O 1s C (Al–O) |
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Before baking | Atomic percentage (%) | 26.0 | 9.0 | – | 46.2 | 18.8 | – | Binding energy (eV) | 457.8 | 101.1 | – | 529.5 | 530.6 | – | After baking | Atomic percentage (%) | 18.9 | 11.1 | 5.7 | 29.8 | 22.7 | 11.8 | Binding energy (eV) | 458.0 | 102.1 | 73.1 | 529.6 | 531.6 | 530.7 |
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Table 3. Atomic Percentage and BE of Each Constituent Element of Sample A-S2T2 before and after Annealing at 850°C