atomic layer deposition of hfo2 thin films and nanolayered hfo2-al2o3-nb2o5 dielectrics

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JOURNAL OF MATERIALS SCIENCE: MATERIALS IN ELECTRONICS 14 (2003) 361±367 Atomic layer deposition of HfO 2 thin ®lms and nanolayered HfO 2 ±Al 2 O 3 ±Nb 2 O 5 dielectrics KAUPO KUKLI*, MIKKO RITALA, MARKKU LESKELA È University of Helsinki, Department of Chemistry, P.O. Box 55, FIN-00014 Helsinki, Finland E-mail: [email protected] TIMO SAJAVAARA, JUHANI KEINONEN University of Helsinki, Accelerator Laboratory, P.O. Box 43, FIN-00014 Helsinki, Finland DAVID C. GILMER, RAMA HEGDE, RAGHAW RAI, LATA PRABHU Motorola, Advanced Products Research and Development Laboratory, 3501 Ed Bluestein Boulevard, Austin, TX 78721, USA Smooth, 4±6-nm thick hafnium oxide ®lms were grown by atomic layer deposition from HfI 4 or HfCl 4 and H 2 O on SiO 2 /Si(1 0 0) substrates at 300 C. Non-uniform ®lms were obtained on hydrogen-terminated Si(1 0 0). The stoichiometry of the ®lms corresponded to that of HfO 2 . The ®lms contained small amounts of residual chlorine and iodine. The ®lms deposited on SiO 2 /Si(1 0 0) were amorphous, but crystallized upon annealing at 1000 C. In order to decrease the conductivity, the HfO 2 ®lms were mixed with Al 2 O 3 , and to increase the capacitance, the ®lms were mixed with Nb 2 O 5 . The capacitance±voltage curves of the Hf±Al±O mixture ®lms showed hysteresis. The capacitance±voltage curves of HfO 2 ®lms and mixtures of Hf±Al±Nb±O were hysteresis free. # 2003 Kluwer Academic Publishers 1. Introduction HfO 2 and ZrO 2 are candidates for high-permittivity (high-k) gate dielectrics in the microelectronics industry to replace SiO 2 [1, 2], owing to their expected stability in contact with silicon [3]. However, an interfacial silicon oxide layer forms between ZrO 2 -based dielectrics and Si either during the deposition process [4, 5] or after the growth, presumably assisted by the susceptibility of ZrO 2 to oxygen diffusion [6]. A structurally commensurate, epitaxial, zirconia/Si interface has been found to be more stable against oxidation [7], but this epitaxy occurs only after stabilizing the cubic ZrO 2 phase with dopants. Although the chemical and physical properties of HfO 2 are otherwise quite similar to those of ZrO 2 , HfO 2 demonstrates somewhat higher calculated [8] and experimentally veri®ed [9] thermal stability than ZrO 2 . However, HfO 2 is, similarly to ZrO 2 , prone to oxygen exchange and diffusion [10], and the interfacial SiO 2 or silicates also form at HfO 2 =Si interfaces [11]. Interfacial layers possess low permittivity and the resulting capacitance dramatically decreases below the value expected for pure HfO 2 . One can expect that the capacitance decrease to be partially compensated by mixing HfO 2 with a material having a higher permit- tivity, such as TiO 2 or Nb 2 O 5 . Furthermore, if the oxygen diffusion is enhanced by the crystalline nature of HfO 2 , it may be suppressed by mixing the HfO 2 layers with a material restricting the crystal growth. This would also eliminate leakage currents along grain boundaries. However, if the additive is a material of low permittivity, the overall capacitance will decrease further. It is known that Al 2 O 3 serves as an ef®cient amorphizing additive in ZrO 2 [12], and also decreases the grain-boundary conductivity in polycrystalline zirconia [13]. So far, Zr±Al±O composite ®lms have been analyzed as dielectric materials, in general, [14] as well as candidates for gate oxides [5, 15, 16], whereas few reports about Hf±Al±O ®lms are available [2, 17]. In addition, hafnium silicates [16] have been of interest. This study is aimed at the preliminary examination of the possibility to grow ultrathin HfO 2 ®lms and HfO 2 - based mixtures from halide precursors by ALD. In order to check the possibility to tune the conductivity and structural stability, the HfO 2 layers were mixed with Al 2 O 3 . In order to compensate the decrease of the effective permittivity caused by adding Al 2 O 3 , the mixture of HfO 2 and Al 2 O 3 was additionally mixed with Nb 2 O 5 . 2. Experimental The HfO 2 ®lms, mixtures of HfO 2 and Al 2 O 3 (Hf±Al±O), and mixtures of HfO 2 , Al 2 O 3 , and Nb 2 O 5 (Hf±Al±Nb±O) were grown in an F-120 ALD reactor [18] onto (1 0 0)p-Si substrates at 300 C. Some experiments were carried out at 350 and 400 C. Native SiO 2 was, prior to deposition, etched in HF (1% solution) for 30 s and the Si surface was then rinsed in distilled water. In some experiments, *Also at: University of Tartu, Institute of Experimental Physics and Technology, Ta Èhe 4, EE-51010 Tartu, Estonia. 0957±4522 # 2003 Kluwer Academic Publishers 361

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