金属有机化学气相沉积法制备功能梯度材料的方法和机理的研究
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摘要
功能梯度材料(Functional Graded Materials，简称FGM)是一种成分、组织、结构、密度和功能特性在宏观上不均匀，但又逐渐变化的新型材料。它较目前广泛使用的隔热性耐热复合材料有许多优点，如可以消除材料间的界面，缓和热应力，具有较高的机械强度，抗热冲击性和耐高温性(达2000℃)等。功能梯度材料是21世纪最有发展前景的新型材料之一，其用途已由原来的宇航工业，扩大到核能源、电子、化学、生物医学等领域；其组成也由金属—陶瓷发展成为金属—金属、金属—合金、非金属—非金属、非金属—陶瓷等多种组合；其制备方法主要包括粉末冶金法，自蔓延高温合成法(SHS)、气相沉积法(CVD和PVD)、电沉积法，激光熔覆法，溶胶—凝胶法(sol-gel)等。金属有机化学气相沉积(MOCVD)法是化学气相沉积法的一种，主要选用金属有机化合物为物源进行化学气相沉积，是目前获取各类特殊功能材料和材料的有效方法之一。该技术能在不太高温度下大面积沉积材料，沉积速率较高，台阶覆盖性好，能够按设计精确控制材料的组成、结构和形态。本文在介绍功能梯度材料的研究进展，CVD、MOCVD技术的研究概况以及Mo(CO)_6，Fe(CO)_5的成膜机制和工艺条件之后，着重报道了利用MOCVD技术制备陶瓷薄膜，金属／金属和金属／陶瓷功能梯度材料。在系统实验的基础上探讨SiO_2薄膜沉积工艺条件及其影响因素，获取了SiO_2薄膜的最佳工艺条件；采用功能梯度材料(FGM)的逆设计思想，在最佳沉积条件的基础上成功制备出Fe／Mo和Mo／SiO_2功能梯度材料，并以X射线衍射，X射线光电子能谱，电镜扫描，膜台阶仪，金相显微镜等手段对材料进行成分测定和表面形态结构分析。
本研究论文主要研究了以下几个方面：
(1) 研究了以Si(OC_2H_5)_4为物源，在Al_2O_3陶瓷基片上制备SiO_2薄膜的工艺条件。在成膜机理的基础上，通过对不同沉积条件(如沉积温度，物源温度，沉积时间)下沉积速率和薄膜结构形态的测试和分析，我们发现，当系统的实验条件为：基片温度500℃—600℃，反应室压力260—400Pa，TEOS的温度在60℃左右，流量1mL．S~(-1)时将获得最佳沉积速率和膜的最佳结构形态。若稳定沉积时间越长，膜层厚度越厚。
中文摘要
(2)采用逆设计系统，对功能梯度材料进行成分优化设计，物理性质计算和
热应力模拟，研究发现:当成分分布指数p=1时，梯度材料的各物性参数缓和效
果最好，结构热应力平缓过渡。
(3)以Mo(CO)6，Fe(CO)5为物源，控制反应物不同的气流量，在基片温度500
“C，压力150一200 pa，Mo(CO)6和Fe(CO)s温度分别为600C和15oC条件下成功制
备出Fe侧。功能梯度材料。结果表明:该梯度材料主要由Fe和M。两相组成，成
分连续梯度变化，符合功能梯度材料的变化规律。Fe从。过渡层表面形貌呈现连续
固溶体状，晶粒细小，分布均匀且结构致密。各梯度层厚度可随机而取。
(4)利用Mo(CO)6，51(OCZHS);为物源，通过调节反应气源的温度和气流量，
在基片温度500℃一600℃，压力170一35OPa，每层沉积60min的条件下制备
Mo/SIOZ功能梯度材料。实验结果表明:材料组成连续梯度变化，符合功能梯度材
料的变化规律。Mo/Sio:过渡层表面形貌晶粒分布均匀且结构致密。
Functionally Graded Material(FGM) is a new generation of composites in which the composition of a dispersion phase is gradually and spatially varied, and thus the properties/microstructure relationships have continuous characteristics. FGM has many superior properties such as eliminating interface crack between the two materials, reducing the thermal and residual stress, thermal barrier, thermal shock resistance, anti-corrosion, increasing the bonding strength and toughness, high-temperature strength (to 2000 C) etc., as compared with traditional composite materials. The applications field of FGM include aerospace , electron, chemistry, biology and medicine fields; The composition change also from metal/ceramic to metal/metal, metal/alloy, non-metal/non-metal and non-metal/ceramic. Moreover, various methods including Powder Metallurgy, Self-propagating High-temperature Synthesis(SHS), Chemical and Physical Vapor Deposition (CVD and PVD), Electrodeposition, Laser Cladding Method, Plasma Sputtering and Sol-Gel
Method have been studed. Metal Organic Chemical Vapor Deposition (MOCVD), using Chemical Vapor Deposition of metal organic compounds, is an effective method for acquiring special function materials and membrane. With MOCVD film technology, film chemical composition is easier to control, deposition temperature lower, deposition speed higher, deposited film more compact, homogenous and flat.
In this paper, firstly, the study of FGMs ,the study of CVD and MOCVD, and the nucleation mechanism have been introduced. Secondly, the fabracations of metal/metal and metal/ceramic FGMs have been reported. Based on the experiment and analysis, the optimum conditions for preparation of Si02 films have been studied. Furthermore, using the inverse designing idea of FGMs, Fe/Mo and Mo/SiO2 FGMs have been successfully prepared. Finally, the composition and microstructure of the materials have been measured by X-ray Debey Powder Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Scanning Electon Microscope (SEM), Step Instrument and Metallgical Microscope.
The main points of our studies are as following:
(1).The preparation of SiO2 films on the substrate of Al2O3, using cold-wall reactor (MOII) and Chemical Vapor Deposition of Si(OC2H5)4, has been studied. Based on the analysis of relationship between the deposition rate and the deposition conditions (the main factor : substrate tenperature, TEOS temperature and deposition time), it is proved that the maximum deposition rate and the optimum surface state, structure of thin films are to be gotten, when the temperature of substrate is 500 to 600 C, the pressure of the reactor is 260 to 400 Pa, the temperature of TEOS is about 60 C, current is 1ml.s-1. The longer deposition time is, the deeper films are.
(2).According to the inverse design system, the structure optimization of FGMs is obtained. Based on the physical properties calculated and the thermal residual stress simulated, it is found that the optimum property parameters and the minimum thermal residual stress are to be gotten when the component distribution exponent P=l.
(3).The Fe/Mo FGMs have been successfully carried out, when the current of Fe(CO)5 and Mo(CO)6 is controlled, the temperature of substrate is 500 C, the pressure of the reactor is 150 to 200 Pa, the temperature of Fe(CO)5 and Mo(CO)6 is 15 C and 60-70 C. The results showed that the materials are consisted of two phases: Fe and Mo solid solution, in which the compositons are of compact texture, with their parculates being uniformed in distribution, fine grains being small. Furthermore, the compositons of the Fe/Mo FGMs are gradually varied and conformed the law of the gradient materials.
(4).The Mo/SiO2 FGMs have been developed using MOCVD with Mo(CO)6 and Si(OC2H5)4. By adjusting the temperature and current of the reactors, the most suitable conditions for preparation of the materials appear that the temperature of substrate is 500 to 600掳C, the pressure of the reactor is 170 to 350 Pa, the deposition time is 60min for every layer.
本研究论文主要研究了以下几个方面：
(1) 研究了以Si(OC_2H_5)_4为物源，在Al_2O_3陶瓷基片上制备SiO_2薄膜的工艺条件。在成膜机理的基础上，通过对不同沉积条件(如沉积温度，物源温度，沉积时间)下沉积速率和薄膜结构形态的测试和分析，我们发现，当系统的实验条件为：基片温度500℃—600℃，反应室压力260—400Pa，TEOS的温度在60℃左右，流量1mL．S~(-1)时将获得最佳沉积速率和膜的最佳结构形态。若稳定沉积时间越长，膜层厚度越厚。
中文摘要
(2)采用逆设计系统，对功能梯度材料进行成分优化设计，物理性质计算和
热应力模拟，研究发现:当成分分布指数p=1时，梯度材料的各物性参数缓和效
果最好，结构热应力平缓过渡。
(3)以Mo(CO)6，Fe(CO)5为物源，控制反应物不同的气流量，在基片温度500
“C，压力150一200 pa，Mo(CO)6和Fe(CO)s温度分别为600C和15oC条件下成功制
备出Fe侧。功能梯度材料。结果表明:该梯度材料主要由Fe和M。两相组成，成
分连续梯度变化，符合功能梯度材料的变化规律。Fe从。过渡层表面形貌呈现连续
固溶体状，晶粒细小，分布均匀且结构致密。各梯度层厚度可随机而取。
(4)利用Mo(CO)6，51(OCZHS);为物源，通过调节反应气源的温度和气流量，
在基片温度500℃一600℃，压力170一35OPa，每层沉积60min的条件下制备
Mo/SIOZ功能梯度材料。实验结果表明:材料组成连续梯度变化，符合功能梯度材
料的变化规律。Mo/Sio:过渡层表面形貌晶粒分布均匀且结构致密。
Functionally Graded Material(FGM) is a new generation of composites in which the composition of a dispersion phase is gradually and spatially varied, and thus the properties/microstructure relationships have continuous characteristics. FGM has many superior properties such as eliminating interface crack between the two materials, reducing the thermal and residual stress, thermal barrier, thermal shock resistance, anti-corrosion, increasing the bonding strength and toughness, high-temperature strength (to 2000 C) etc., as compared with traditional composite materials. The applications field of FGM include aerospace , electron, chemistry, biology and medicine fields; The composition change also from metal/ceramic to metal/metal, metal/alloy, non-metal/non-metal and non-metal/ceramic. Moreover, various methods including Powder Metallurgy, Self-propagating High-temperature Synthesis(SHS), Chemical and Physical Vapor Deposition (CVD and PVD), Electrodeposition, Laser Cladding Method, Plasma Sputtering and Sol-Gel
Method have been studed. Metal Organic Chemical Vapor Deposition (MOCVD), using Chemical Vapor Deposition of metal organic compounds, is an effective method for acquiring special function materials and membrane. With MOCVD film technology, film chemical composition is easier to control, deposition temperature lower, deposition speed higher, deposited film more compact, homogenous and flat.
In this paper, firstly, the study of FGMs ,the study of CVD and MOCVD, and the nucleation mechanism have been introduced. Secondly, the fabracations of metal/metal and metal/ceramic FGMs have been reported. Based on the experiment and analysis, the optimum conditions for preparation of Si02 films have been studied. Furthermore, using the inverse designing idea of FGMs, Fe/Mo and Mo/SiO2 FGMs have been successfully prepared. Finally, the composition and microstructure of the materials have been measured by X-ray Debey Powder Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Scanning Electon Microscope (SEM), Step Instrument and Metallgical Microscope.
The main points of our studies are as following:
(1).The preparation of SiO2 films on the substrate of Al2O3, using cold-wall reactor (MOII) and Chemical Vapor Deposition of Si(OC2H5)4, has been studied. Based on the analysis of relationship between the deposition rate and the deposition conditions (the main factor : substrate tenperature, TEOS temperature and deposition time), it is proved that the maximum deposition rate and the optimum surface state, structure of thin films are to be gotten, when the temperature of substrate is 500 to 600 C, the pressure of the reactor is 260 to 400 Pa, the temperature of TEOS is about 60 C, current is 1ml.s-1. The longer deposition time is, the deeper films are.
(2).According to the inverse design system, the structure optimization of FGMs is obtained. Based on the physical properties calculated and the thermal residual stress simulated, it is found that the optimum property parameters and the minimum thermal residual stress are to be gotten when the component distribution exponent P=l.
(3).The Fe/Mo FGMs have been successfully carried out, when the current of Fe(CO)5 and Mo(CO)6 is controlled, the temperature of substrate is 500 C, the pressure of the reactor is 150 to 200 Pa, the temperature of Fe(CO)5 and Mo(CO)6 is 15 C and 60-70 C. The results showed that the materials are consisted of two phases: Fe and Mo solid solution, in which the compositons are of compact texture, with their parculates being uniformed in distribution, fine grains being small. Furthermore, the compositons of the Fe/Mo FGMs are gradually varied and conformed the law of the gradient materials.
(4).The Mo/SiO2 FGMs have been developed using MOCVD with Mo(CO)6 and Si(OC2H5)4. By adjusting the temperature and current of the reactors, the most suitable conditions for preparation of the materials appear that the temperature of substrate is 500 to 600掳C, the pressure of the reactor is 170 to 350 Pa, the deposition time is 60min for every layer.
引文
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