Dr. Charles H. Winter Profile

Dr. Charles H. Winter

at Wayne State Univ

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Proceedings Article | 9 April 2024 Presentation + Paper

Development of ALD precursors for low resistivity Zr, Hf, and Nb nitride films

Syeda Sameen, Charles Winter

Proceedings Volume 12958, 129580J (2024) https://doi.org/10.1117/12.3010175

KEYWORDS: Atomic layer deposition, Crystals, Thermal stability, Zirconium, Spectroscopy, Nitrogen, X-rays, Potassium, Niobium, Graphite

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The synthesis, spectroscopic properties, and suitability for use as precursors in atomic layer deposition (ALD) processes are described for the ZrCp₃ and HfCp₃. ZrCp₃ was prepared by a literature procedure entailing reduction of ZrCp₄ with potassium graphite and was isolated as brown crystals in 34% yield. HfCp₄ was isolated in 57% yield as yellow-brown crystals by a similar route employing reduction of HfCp₄ with potassium graphite. ZrCp₃ and HfCp₃ showed broad paramagnetic resonances in the ¹H NMR spectra that were centered at δ 6.2 and 6.0ppm, respectively, which are assigned to the cyclopentadienyl hydrogen atoms. Additionally, the ¹H NMR spectra of the ZrCp₃ and HfCp₃ crystals revealed resonances arising from the diamagnetic complexes Cp₃ZrH and Cp₃HfH, which are proposed to arise from hydrolysis of ZrCp₃ and HfCp₃ by traces of water in the NMR solvent. The identities of ZrCp₃ and HfCp₃ were established by determination of their x-ray crystal structures, which exactly matched previously reported molecular structures. Thermogravimetric analyses of ZrCp₃ and HfCp₃ were conducted to assess their volatilities and thermal stabilities. ZrCp₃ showed the onset of mass loss at about 125 °C and revealed a single-step evaporation up to about 225 °C, at which point decomposition limited further mass loss. Mass loss for HfCp₃ started at about 150 °C and continued up to about 270 °C, at which point decomposition limited further mass loss. ZrCp₃ and HfCp₃ decomposed extensively during preparative sublimation experiments at 0.5 Torr, and do not appear to have promising properties as ALD precursors.

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