研究目的
To study the applicability of Co(BTSA)2(THF) and H2O in atomic layer deposition (ALD) of cobalt(II) oxide thin films, focusing on precursor properties, deposition characteristics, film properties, and reaction mechanisms.
研究成果
Co(BTSA)2(THF) enables low-temperature ALD of cobalt(II) oxide films with good saturation behavior, but impurities from the BTSA ligand are a significant drawback. The primary reaction mechanism is ligand exchange, but side reactions contribute to impurities. The precursor is best suited for low-temperature applications where impurity levels can be managed.
研究不足
The process leads to Si and H impurities in the films, with Si content increasing at higher deposition temperatures, limiting purity. The precursor may undergo partial decomposition or condensation, affecting film quality. The deposition temperature range is constrained by precursor volatility and decomposition, and the films are not fully crystalline at higher temperatures.
1:Experimental Design and Method Selection:
The study used atomic layer deposition (ALD) with Co(BTSA)2(THF) as the metal precursor and H2O as the coreactant. The design aimed to deposit cobalt(II) oxide films at low temperatures, with investigations into saturation behavior, film characterization, and in situ reaction mechanisms.
2:Sample Selection and Data Sources:
Substrates included native oxide terminated Si(100) and soda lime glass (SLG) cut to 5 × 5 cm2 squares. Silicon substrates were used as received; glass substrates were cleaned ultrasonically. Films were deposited in a temperature range of 75–250 °C.
3:List of Experimental Equipment and Materials:
Equipment included a commercial F-120 ALD reactor, thermogravimetric analyzer (TGA), ellipsometer, x-ray diffractometer, XPS spectrometer, AFM, ToF-ERDA setup, QCM, and QMS. Materials included Co(BTSA)2(THF), H2O, D2O, nitrogen gas, and various chemicals for synthesis.
4:Experimental Procedures and Operational Workflow:
Precursor synthesis was done under inert conditions. Film deposition involved alternating pulses of Co(BTSA)2(THF) and H2O with purging steps. In situ studies used QCM and QMS to monitor mass changes and gaseous by-products. Characterization included thickness measurements, structural analysis with GI-XRD, chemical analysis with XPS and ToF-ERDA, and morphological study with AFM.
5:Data Analysis Methods:
Data were analyzed using software packages like CASAXPS for XPS, and numerical integration for QMS and QCM data. Statistical methods included linear fitting for growth per cycle calculations.
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Film Sense FS-1 Multi-Wavelength ellipsometer
FS-1
Film Sense
Used for measuring film thicknesses via ellipsometry.
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PANalytical X'Pert Pro MPD diffractometer
X'Pert Pro MPD
PANalytical
Used for x-ray reflectivity (XRR) measurements.
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Hitachi U2000 spectrophotometer
U2000
Hitachi
Used for UV-Vis spectroscopy in reflectance mode.
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Rigaku SmartLab x-ray diffractometer
SmartLab
Rigaku
Used for grazing incidence x-ray diffraction (GI-XRD) measurements.
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Veeco V Multimode AFM
V Multimode
Veeco
Used for atomic force microscopy to study film morphology.
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Hiden HAL/3F 501 RC QMS
HAL/3F 501 RC
Hiden
Used for quadrupole mass spectroscopy in in situ studies.
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F-120 ALD reactor
F-120
ASM Microchemistry Ltd.
Used for atomic layer deposition of thin films.
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TGA850 thermobalance
TGA850
Mettler Toledo
Used for thermogravimetric analysis of precursors.
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Argus spectrometer
Argus
Omicron NanoTechnology GmbH
Used for x-ray photoelectron spectroscopy (XPS) measurements.
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Maxtek TM 400 QCM
TM 400
Maxtek
Used for quartz crystal microbalance measurements in in situ studies.
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