Hydrogen Analysis by Using of Secondary Ion Mass Spectroscopy

使用二次离子质谱分析氢

• 批准号: 06650770
• 负责人: NARUSHIMA Takayuki
• 金额: $ 1.28万
• 依托单位: TOHOKU UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for General Scientific Research (C)
• 财政年份: 1994
• 资助国家: 日本
• 起止时间: 1994 至 1995
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-06650770/
• 关键词: SIMS; silicon carbide; silicon nitride; oxidation; cristobalite; tridymite; silica; water vapor

(1) Hydrogen analysisHydrogen analysis by using of secondary ion mass spectroscopy (SIMS) was carried out for the standard sample (SiO_2 on silicon) in which proton was implanted, and the optimum analytical conditions for hydrogen analysis were clarified. It is important for hydrogen analysis to control the raster size of an ion beam, neutralization, signal gating and so on.(2) Wet oxidation rateWet oxidation rates of chemically-vapor-deposited silicon carbide (CVD-SiC) and silicon nitride (CVD-Si_3N_4) were measured by a thermogravimetric technique. The oxidation films were analyzed by XRD and Raman spectroscopy. The oxidation rate was increased with increasing of water vapor pressure and decreasing of oxygen pressure in the atmosphere. This may be lead by the change of micro-defects in the oxide film (silica). Water vapor in the atmosphere accelerated the crystallization of oxide film at lower-temperatures (around 1373 K) and non-crystallization at higher-temperatures (>1873 K). It was clarified by laser Raman spectroscopy that amorphous silica was at around oxide/gas interface and cristobalite was at around oxide/ceramics interface, i.e., the oxide film formed was a duplex one. These results suggested that the formation of amorphous silica lowered the oxidation resistance of siliconbased ceramics for wet oxidation.

(1)氢分析对注入质子的标准样品（硅上SiO_2）进行了二次离子质谱（SIMS）分析，明确了氢分析的最佳分析条件。控制离子束的栅格尺寸、中和、信号门控等对氢分析具有重要意义。(2)湿氧化速率用热重法测定了化学气相沉积碳化硅（CVD-SiC）和氮化硅（CVD-Si_3N_4）的湿氧化速率。采用XRD和拉曼光谱对氧化膜进行了分析。氧化速率随大气中水蒸气压的增大和氧压的减小而增大。这可能是由氧化膜（二氧化硅）中微缺陷的变化引起的。大气中的水蒸气在较低温度下（约1373 K）加速了氧化膜的结晶，而在较高温度下（约1873 K）则不结晶。激光拉曼光谱分析表明，非晶态二氧化硅位于氧化物/气体界面周围，方石沸石位于氧化物/陶瓷界面周围，形成的氧化膜为双相氧化膜。这些结果表明，非晶二氧化硅的形成降低了硅基陶瓷湿氧化的抗氧化性。

项目成果

成島尚之: "シリコン基セラミックスの高温酸化" 新素材・新コーティングの高温耐環境性. 21-24 (1994)

成岛直之：“硅基陶瓷的高温氧化”新材料和新型涂料的耐高温环境性21-24（1994）。

井口泰孝: "二次イオン質量分析計によるセラミックスの高温酸化皮膜中の水素分析" 青葉工業会報. 39. 14-17 (1995)

Yasutaka Iguchi：“使用二次离子质谱仪分析陶瓷高温氧化膜中的氢”Aoba Kogyo Kaiho。39. 14-17 (1995)。

Y. Iguchi: "Complex Oxide Films Formed during Thermal Oxidation of Liquid Aluminum Alloys" Design Fundamentals of High Temperature Composites, Intermetallics and Metal-Ceramic Systems. 337-343 (1996)

Y. Iguchi：“液态铝合金热氧化过程中形成的复杂氧化膜”高温复合材料、金属间化合物和金属陶瓷系统的设计基础。

Iguchi et al.: "Complex Oxide Films Formed during Thermal Oxidation of Liquid Aluminum Alloys." Design Fundamentals of High Temperature Composites Intermetallics and Metal-Ceramic Systems. 337-343 (1996)

Iguchi 等人：“液态铝合金热氧化过程中形成的复杂氧化膜。”

T.Narushima: "In Situ Observation of Oxide Films Formed during Thermal Oxidation of SiC-B_4C Composite Using Raman Spectroscopy" Key Engineering Materials. 113. 99-104 (1995)

T.Narushima：“利用拉曼光谱原位观察SiC-B_4C复合材料热氧化过程中形成的氧化膜”关键工程材料。