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Title: Thermal reaction of polycrystalline AlN with XeF{sub 2}

Abstract

Detailed studies on the thermal reaction behavior of polycrystalline aluminum nitride (AlN) with effusive xenon difluoride (XeF{sub 2}) have been carried out over the sample temperature (T{sub s}) range from 300 to 920 K using molecular beam mass spectrometry combined with a time-of-flight technique and ex situ surface analyses, i.e., X-ray photoelectron spectroscopy, Auger electron spectroscopy, and scanning electron microscopy (SEM). The species desorbed from the AlN/XeF{sub 2} system were monitored using molecular beam mass spectrometry, as a function of sample temperature. Above T{sub s}=800 K, the desorbed reaction products were identified as N{sub 2} and AlF{sub 3}, and their flux intensities increase monotonically as the sample temperature is increased. The flux intensity of XeF{sub 2} desorbed after physisorption to the AlN surface is found to decrease as T{sub s} is raised above T{sub s}=800 K, and approximately one half of the incoming XeF{sub 2} is consumed by the thermal reaction at 920 K. The results of surface analyses show that the thermal reaction of AlN with XeF{sub 2} starts at approximately T{sub s}=700 K, forming a reaction layer composed of AlF{sub 3}. The AlF{sub 3} layer becomes thick as T{sub s} is increased from T{sub s}=700-800 K. Above T{submore » s}=800 K, however, as a result of fast desorption of AlF{sub 3} and F atoms from the AlF{sub 3} layer, only partially fluorinated AlF{sub x} (x=1 and/or 2) layers are formed and the bulk AlN is revealed again. The SEM photographs indicate that the surfaces exposed above T{sub s}=850 K are strongly etched but a slight change is observed at T{sub s}{<=}800 K. On the basis of these results, three reaction stages are proposed for the AlN/XeF{sub 2} reaction depending on the sample temperature range: Stage 1 (300{<=}T{sub s}<700 K); no reaction, stage 2 (700{<=}T{sub s}<800 K); surface fluorination, and stage 3 (800{<=}T{sub s}); etching. At stage 3, AlF{sub 3} formed on the surface starts to evaporate and fast etching proceeds, since the vapor pressure of AlF{sub 3} is high enough in this temperature range.« less

Authors:
; ; ; ; ; ; ; ;  [1];  [2]
  1. Materials Research Laboratory, NGK INSULATORS, LTD., 2-56 Suda-cho, Mizuho, Nagoya 467-8530 (Japan)
  2. (Japan)
Publication Date:
OSTI Identifier:
20723212
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Vacuum Science and Technology. A, Vacuum, Surfaces and Films; Journal Volume: 23; Journal Issue: 6; Other Information: DOI: 10.1116/1.2110395; (c) 2005 American Vacuum Society; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ADSORPTION; ALUMINIUM FLUORIDES; ALUMINIUM NITRIDES; AUGER ELECTRON SPECTROSCOPY; DESORPTION; ETCHING; FLUORINATION; LAYERS; MASS SPECTROSCOPY; MOLECULAR BEAMS; POLYCRYSTALS; SCANNING ELECTRON MICROSCOPY; SEMICONDUCTOR MATERIALS; TEMPERATURE RANGE 0273-0400 K; TEMPERATURE RANGE 0400-1000 K; THERMAL ANALYSIS; TIME-OF-FLIGHT METHOD; VAPOR PRESSURE; X-RAY PHOTOELECTRON SPECTROSCOPY; XENON FLUORIDES

Citation Formats

Watanabe, Morimichi, Mori, Yukimasa, Ishikawa, Takahiro, Sakai, Hiroaki, Iida, Takashi, Akiyama, Keijiro, Narita, Shogo, Sawabe, Kyoichi, Shobatake, Kosuke, and Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603. Thermal reaction of polycrystalline AlN with XeF{sub 2}. United States: N. p., 2005. Web. doi:10.1116/1.2110395.
Watanabe, Morimichi, Mori, Yukimasa, Ishikawa, Takahiro, Sakai, Hiroaki, Iida, Takashi, Akiyama, Keijiro, Narita, Shogo, Sawabe, Kyoichi, Shobatake, Kosuke, & Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603. Thermal reaction of polycrystalline AlN with XeF{sub 2}. United States. doi:10.1116/1.2110395.
Watanabe, Morimichi, Mori, Yukimasa, Ishikawa, Takahiro, Sakai, Hiroaki, Iida, Takashi, Akiyama, Keijiro, Narita, Shogo, Sawabe, Kyoichi, Shobatake, Kosuke, and Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603. Tue . "Thermal reaction of polycrystalline AlN with XeF{sub 2}". United States. doi:10.1116/1.2110395.
@article{osti_20723212,
title = {Thermal reaction of polycrystalline AlN with XeF{sub 2}},
author = {Watanabe, Morimichi and Mori, Yukimasa and Ishikawa, Takahiro and Sakai, Hiroaki and Iida, Takashi and Akiyama, Keijiro and Narita, Shogo and Sawabe, Kyoichi and Shobatake, Kosuke and Department of Molecular Design and Engineering, Graduate School of Engineering, Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603},
abstractNote = {Detailed studies on the thermal reaction behavior of polycrystalline aluminum nitride (AlN) with effusive xenon difluoride (XeF{sub 2}) have been carried out over the sample temperature (T{sub s}) range from 300 to 920 K using molecular beam mass spectrometry combined with a time-of-flight technique and ex situ surface analyses, i.e., X-ray photoelectron spectroscopy, Auger electron spectroscopy, and scanning electron microscopy (SEM). The species desorbed from the AlN/XeF{sub 2} system were monitored using molecular beam mass spectrometry, as a function of sample temperature. Above T{sub s}=800 K, the desorbed reaction products were identified as N{sub 2} and AlF{sub 3}, and their flux intensities increase monotonically as the sample temperature is increased. The flux intensity of XeF{sub 2} desorbed after physisorption to the AlN surface is found to decrease as T{sub s} is raised above T{sub s}=800 K, and approximately one half of the incoming XeF{sub 2} is consumed by the thermal reaction at 920 K. The results of surface analyses show that the thermal reaction of AlN with XeF{sub 2} starts at approximately T{sub s}=700 K, forming a reaction layer composed of AlF{sub 3}. The AlF{sub 3} layer becomes thick as T{sub s} is increased from T{sub s}=700-800 K. Above T{sub s}=800 K, however, as a result of fast desorption of AlF{sub 3} and F atoms from the AlF{sub 3} layer, only partially fluorinated AlF{sub x} (x=1 and/or 2) layers are formed and the bulk AlN is revealed again. The SEM photographs indicate that the surfaces exposed above T{sub s}=850 K are strongly etched but a slight change is observed at T{sub s}{<=}800 K. On the basis of these results, three reaction stages are proposed for the AlN/XeF{sub 2} reaction depending on the sample temperature range: Stage 1 (300{<=}T{sub s}<700 K); no reaction, stage 2 (700{<=}T{sub s}<800 K); surface fluorination, and stage 3 (800{<=}T{sub s}); etching. At stage 3, AlF{sub 3} formed on the surface starts to evaporate and fast etching proceeds, since the vapor pressure of AlF{sub 3} is high enough in this temperature range.},
doi = {10.1116/1.2110395},
journal = {Journal of Vacuum Science and Technology. A, Vacuum, Surfaces and Films},
number = 6,
volume = 23,
place = {United States},
year = {Tue Nov 15 00:00:00 EST 2005},
month = {Tue Nov 15 00:00:00 EST 2005}
}
  • Studies on the thermal reaction behavior of polycrystalline cubic silicon carbide (SiC) with effusive xenon difluoride (XeF{sub 2}) have been carried out over the sample temperature (T{sub s}) range from 300 to 900 K using molecular beam quadrupole mass spectrometry combined with a time-of-flight technique and ex situ surface analyses, i.e., x-ray photoelectron spectroscopy (XPS) and scanning Auger microscopy (SAM). Above T{sub s}=700 K, the reaction product desorbed from the SiC surface was identified as SiF{sub 4}. The flux intensity of SiF{sub 4} increases monotonically as a function of T{sub s} above 700 K. The flux intensity of XeF{sub 2}more » desorbed from the SiC surface decreases above T{sub s}=700 K, and at T{sub s}=900 K, approximately 10% of the incident XeF{sub 2} was found to be consumed by the thermal reaction. No ions at m/e=31 (CF{sup +}), 50 (CF{sub 2}{sup +}), and 69 (CF{sub 3}{sup +}) to be ascribed to carbon fluoride species were detected under the present experimental conditions, and thus C atoms in SiC were found to remain as residue. From the XPS and SAM observations of the SiC samples exposed to XeF{sub 2} vapor at 1.8x10{sup -4} Torr, we find that fluorination of a native oxide layer formed on the SiC surface takes place at T{sub s}=300 K. At T{sub s}=520 K, the native oxide layer was partially removed from the surface, and the presence of a reaction layer composed of partially fluorinated C atoms was observed. As T{sub s} is increased above 520 K, the reaction layer becomes thicker. Above T{sub s}=700 K, a thick reaction layer mainly composed of C atoms is formed, while only the near-surface reaction layer is fluorinated. The fast desorption of SiF{sub 4} products reduces the Si concentration in the SiC surface and the residual C atoms having comprised the SiC lattice are left as the reaction layer.« less
  • A fusion temperature versus composition curve has been obtained for the system XeF/sub 2//XeF/sub 5/AsF/sub 6/. X-ray single-crystal and powder diffraction methods have been used in combination with Raman spectroscopy to characterize the various phases that are formed. The fusion temperature/composition curve indicates compound formation at XeF/sub 2/ to XeHeF/sub 5/AsF/sub 6/ ratios (fusion temperature in parentheses): 1:2 (89.5 /sup 0/C), 2:1 (59.5 /sup 0/C), and 3:1 (74.0 /sup 0/C). Other simple integer combinations are also suggested at the ratios 1:1 (56.5 /sup 0/C) and 3:2 (56.0 /sup 0/C).
  • The formation of Ti{sub 2}AlN by solid state reaction between layers of wurtzite-AlN and {alpha}-Ti was characterized by in situ x-ray scattering. The sequential deposition of these layers by dual magnetron sputtering onto Al{sub 2}O{sub 3}(0001) at 200 deg. C yielded smooth, heteroepitaxial (0001) oriented films, with abrupt AlN/Ti interfaces as shown by x-ray reflectivity and Rutherford backscattering spectroscopy. Annealing at 400 deg. C led to AlN decomposition and diffusion of released Al and N into the Ti layers, with formation of Ti{sub 3}AlN. Further annealing at 500 deg. C resulted in a phase transformation into Ti{sub 2}AlN(0001) after onlymore » 5 min.« less
  • The change in surface adhesion after fluorination of Al and Al{sub 2}O{sub 3} surfaces using XeF{sub 2} was investigated with atomic force microscopy. The chemical interaction between XeF{sub 2} and Al and Al{sub 2}O{sub 3} surfaces was studied by in situ x-ray photoelectron spectroscopy. Fresh Al and Al{sub 2}O{sub 3} surfaces were obtained by etching top silicon layers of Si/Al and Si/Al{sub 2}O{sub 3} with XeF{sub 2}. The surface adhesion and chemical composition were measured after the exposure to air or annealing (at 200 deg. C under vacuum). The correlation between the adhesion force increase and presence of AlF{sub 3}more » on the surface was revealed.« less