大气压射频Ar/H_2/SiCl_4等离子体射流实验诊断及其沉积硅薄膜研究
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摘要
大气压冷等离子体射流技术是近年来新兴的一种等离子体技术,其宏观低温特性及其中含有的大量活性物种使其在材料加工、生物改性、杀菌消毒等领域有广泛的应用前景。其操作简便并可在开放环境下工作的特点也使其备受青睐。本文设计了一种大气压冷等离子体射流源并对其进行参数诊断,在此基础上在薄膜沉积工作方面进行一些尝试。硅薄膜因其优异的性能而在太阳能电池、集成电路、传感领域中具有广泛应用,其制备多在真空或较高气压环境下,往往需要反应腔及真空设备。我们在采用自行设计的等离子体源,以较为安全的SiCl4为硅源,在开放环境中进行了硅薄膜沉积研究。以大气压等离子体射流发生装置的设计、等离子体参数的诊断以及薄膜的沉积为主线开展了以下工作：
描述了自行设计制作的两种大气压等离子体射流源及其放电现象。给出了放电的照片、放电电流、电压曲线以及伏安曲线,并从理论上对放电现象的变化加以解释,为确定适合进行薄膜沉积的大气压等离子体源寻求依据。发现平行平板打孔的结构电极较适合于薄膜沉积工作。随着功率的增加,条形孔和圆形孔电极的放电模式都经历了α模式向γ模式的转变,并且在一定的功率范围内α与Y模式可以共存,5slpm的纯氩气放电这一范围是50W-70W。从放电的稳定性及可长时间宽范围工作的角度考虑,不锈钢材料的圆孔结构电极是比较理想的选择。
对自行设计的装置产生的等离子体采用等效电路法计算了电子密度,采用发射光谱法诊断了温度。研究了一种新的利用全电路欧姆定律计算电子密度的方法,考察了两种孔型的平行平板结构电极的电子密度随外加功率、电流电压相位差、电极间距以及气体流速变化的趋势。对于单一种类气体的射频容性放电,只要满足ωpe>>ω、vm2>>ωpe2,都可以通过测量电流电压峰峰值获得电子密度。对同一个电极而言,大的外加功率、小的电极间距以及合适的流速会产生电子密度相对较高的等离子体。采用发射光谱法分别对纯氩气放电和混合气体放电进行了诊断。在纯氩气放电中,分别采用氮气和OH(A2∑→X2п)的谱带拟合了振动温度和转动温度,氩原子谱线拟合了电子激发温度,转动温度随功率的增加而增加,随气体流速的增加而降低趋势,但电子激发温度变化不大。在混合气体放电中,利用硅原子谱线强度计算了电子激发温度,研究了放电功率、气体流量等参数对其的影响。由于采用硅原子谱线计算得到的电子激发温度是解离消耗掉一部分电子后剩余电子的激发温度,可以认为其变化趋势与解离得到的硅原子总数相反。随着功率、SiCl4流量和氩气流量的增加电子激发温度均呈下降趋势。氢气分子与SiCl4分子的解离能相差不大而“抢夺”电子能量,氢气的混入导致硅原子发射强度明显减小。
采用自行设计的大气压等离子体射流装置,以氩气、四氯化硅和氢气的混合气体为放电气体,在开放环境中分别以单晶硅、陶瓷和普通玻璃为衬底进行了硅薄膜沉积研究。对薄膜的厚度、成分、表面形貌及沉积温度等进行了表征。发现沉积出的薄膜存在氧化层,解释了氧化机理,比较了沉积时间、氢气流量对薄膜成分的影响。薄膜沉积初期衬底温度不高,此时的氧化过程主要由空气中的氧气被等离子体分解产生自由基造成,氧化过程与等离子体参数密切相关。沉积时间增加使衬底温度增加,超过150°时,SiCl4直接水解为二氧化硅,此时的氧化过程还与SiCl4流量有关。氢气流量从多方面影响薄膜生长过程：氢气流量越大,薄膜的沉积速率和氧化速度都低,Si-H键对抑制薄膜氧化有相当重要的作用。但过大的氢气流量会使放电熄灭。较小的氩气流量有利于抑制薄膜的氧化过程同时节约成本,但过小的氩气流量会影响放电及其作为射流的特性。过大的四氯化硅流量不但造成浪费,也容易使薄膜被氧化。
Atmospheric pressure cold plasma jet has many applications in various areas, such as materials modification and sterilization because of its low temperature and activity species contained. This technique is easy to handle and can work in an open environment, which makes it very popular. In this thesis we design two experimental equipments to generate atmospheric pressure cold plasma jet. diagnose plasma parameters, and attempt to use it in film deposition. The silicon film has successful use in solar cell, integrated circuit and thin film transistors. The preparation of the silicon film works at low pressure and high temperature mostly, which need vacuum equipment and complicatedly to operate. This thesis aims to experiment a novel method to deposit silicon film at open air using atmospheric pressure plasma and SiCl4 as raw materials. This thesis is divided into exordium, the device for generation of the atmospheric pressure plasma jet. the diagnostics of plasma parameter and the deposition of silicon film.
We describe two self-designed devices for the generation of atmospheric pressure plasma jet. Some photographs of the discharge, the discharge waveform and its current-voltage curve are presented, base on which the explanation of the change of the discharge phenomena are discussed. The discharge phenomena using deferent electrodes are compared to select a good electrode structure for film deposition. The discharges translate from a-mode to y-mode for both the electrodes with rectangle holes and round holes. The two discharge modes exist together in some power range at different flow rate of discharge gas. which for 5slpm of pure Argon is 50W-70W.
A novel method to diagnose the electron density of the atmospheric plasma jet using an equivalent circuit of the plasma discharge is studied. Based on the circuit model, the electron density can be obtained according to the Ohm's law. By using the method, the effects of the electrode shape, the gas flow rate and the discharge gap on the electron density are discussed. The electron density increases with the increase of input power and the decrease of electrodes gap. The electron density decreases as flow rate increasing for the electrodes with rectangle holes, but almost no response for the electrodes with round holes due to its smaller outlet area. By using this method the electron density in atmospheric pressure radio frequency conductive pure gas discharge can be determined. whenωpe>>ωand vm2>>ωpe2 are satisfied.
OES has been used to diagnose the rotational and vibrational temperature in Ar discharge, and the electron excitation temperature in the Ar/SiCl4 mixture discharge. In Ar discharge as increasing the RF power the rotational temperature increases and the vibrational temperature decreases, which mean that the system trends to thermal balance. The electron excitation temperature has little change with RF power. In Ar/SiCl4 discharge the electron excitation temperature is calculated by the Si atom spectral lines. The electron excitation temperature belongs to the remained electrons.after dissociate SiCl4. The electron excitation temperature decreases with the increasing of the RF power. the SiCl4 flow rate and the Ar flow rate. The bond energy of H2 and SiCl4 are close, while partial electron energy is consumed to dissociate H2. As a result, the H2 influx weakens the discharge.
We deposit the film with the layered structure on the substrate of monocrystalline silicon. ceramic and glass, using self-assembled radio frequency atmospheric plasma jet in open air. The discharge gas is the mixture of Ar, H2 and SiCl4 gas bubbled by Ar. The film thickness, the film content, the content profile along the depth and surface topography have been investigated by step profiler. XPS and SEM respectively. The film has been layered from pure silicon near the substrate to SiO2 close to the film surface. We analyze the mechanism of oxidation process during film deposition, and investigate the reason of layered structure of the films. At the beginning of the film deposition the substrate temperature is low and the oxidation process is attributed to the oxidative radicals, which were generated from decomposition of O2 in the air by atmospheric plasma jet. As time passed by. the substrate temperature becomes higher. When it reached the decomposition temperature of met silicate (150℃). the SiO2 produced by decomposition of met silicate was the primary film pollutant. The flow rate of SiCl4 is the key factor of oxidation rate at the high substrate temperature. The H2 flow rate is very important for Si film growth and oxidation, because it determines the plasma temperature and density. Besides, the hydrogen atom bonding to silicon atom to form Si-H group is an important reason to stop the film oxidation. Therefore although the deposited film is oxidative partially, but properly control the discharge gas flow rate and the substrate temperature should be beneficial to form pure silicon film.
描述了自行设计制作的两种大气压等离子体射流源及其放电现象。给出了放电的照片、放电电流、电压曲线以及伏安曲线,并从理论上对放电现象的变化加以解释,为确定适合进行薄膜沉积的大气压等离子体源寻求依据。发现平行平板打孔的结构电极较适合于薄膜沉积工作。随着功率的增加,条形孔和圆形孔电极的放电模式都经历了α模式向γ模式的转变,并且在一定的功率范围内α与Y模式可以共存,5slpm的纯氩气放电这一范围是50W-70W。从放电的稳定性及可长时间宽范围工作的角度考虑,不锈钢材料的圆孔结构电极是比较理想的选择。
对自行设计的装置产生的等离子体采用等效电路法计算了电子密度,采用发射光谱法诊断了温度。研究了一种新的利用全电路欧姆定律计算电子密度的方法,考察了两种孔型的平行平板结构电极的电子密度随外加功率、电流电压相位差、电极间距以及气体流速变化的趋势。对于单一种类气体的射频容性放电,只要满足ωpe>>ω、vm2>>ωpe2,都可以通过测量电流电压峰峰值获得电子密度。对同一个电极而言,大的外加功率、小的电极间距以及合适的流速会产生电子密度相对较高的等离子体。采用发射光谱法分别对纯氩气放电和混合气体放电进行了诊断。在纯氩气放电中,分别采用氮气和OH(A2∑→X2п)的谱带拟合了振动温度和转动温度,氩原子谱线拟合了电子激发温度,转动温度随功率的增加而增加,随气体流速的增加而降低趋势,但电子激发温度变化不大。在混合气体放电中,利用硅原子谱线强度计算了电子激发温度,研究了放电功率、气体流量等参数对其的影响。由于采用硅原子谱线计算得到的电子激发温度是解离消耗掉一部分电子后剩余电子的激发温度,可以认为其变化趋势与解离得到的硅原子总数相反。随着功率、SiCl4流量和氩气流量的增加电子激发温度均呈下降趋势。氢气分子与SiCl4分子的解离能相差不大而“抢夺”电子能量,氢气的混入导致硅原子发射强度明显减小。
采用自行设计的大气压等离子体射流装置,以氩气、四氯化硅和氢气的混合气体为放电气体,在开放环境中分别以单晶硅、陶瓷和普通玻璃为衬底进行了硅薄膜沉积研究。对薄膜的厚度、成分、表面形貌及沉积温度等进行了表征。发现沉积出的薄膜存在氧化层,解释了氧化机理,比较了沉积时间、氢气流量对薄膜成分的影响。薄膜沉积初期衬底温度不高,此时的氧化过程主要由空气中的氧气被等离子体分解产生自由基造成,氧化过程与等离子体参数密切相关。沉积时间增加使衬底温度增加,超过150°时,SiCl4直接水解为二氧化硅,此时的氧化过程还与SiCl4流量有关。氢气流量从多方面影响薄膜生长过程：氢气流量越大,薄膜的沉积速率和氧化速度都低,Si-H键对抑制薄膜氧化有相当重要的作用。但过大的氢气流量会使放电熄灭。较小的氩气流量有利于抑制薄膜的氧化过程同时节约成本,但过小的氩气流量会影响放电及其作为射流的特性。过大的四氯化硅流量不但造成浪费,也容易使薄膜被氧化。
Atmospheric pressure cold plasma jet has many applications in various areas, such as materials modification and sterilization because of its low temperature and activity species contained. This technique is easy to handle and can work in an open environment, which makes it very popular. In this thesis we design two experimental equipments to generate atmospheric pressure cold plasma jet. diagnose plasma parameters, and attempt to use it in film deposition. The silicon film has successful use in solar cell, integrated circuit and thin film transistors. The preparation of the silicon film works at low pressure and high temperature mostly, which need vacuum equipment and complicatedly to operate. This thesis aims to experiment a novel method to deposit silicon film at open air using atmospheric pressure plasma and SiCl4 as raw materials. This thesis is divided into exordium, the device for generation of the atmospheric pressure plasma jet. the diagnostics of plasma parameter and the deposition of silicon film.
We describe two self-designed devices for the generation of atmospheric pressure plasma jet. Some photographs of the discharge, the discharge waveform and its current-voltage curve are presented, base on which the explanation of the change of the discharge phenomena are discussed. The discharge phenomena using deferent electrodes are compared to select a good electrode structure for film deposition. The discharges translate from a-mode to y-mode for both the electrodes with rectangle holes and round holes. The two discharge modes exist together in some power range at different flow rate of discharge gas. which for 5slpm of pure Argon is 50W-70W.
A novel method to diagnose the electron density of the atmospheric plasma jet using an equivalent circuit of the plasma discharge is studied. Based on the circuit model, the electron density can be obtained according to the Ohm's law. By using the method, the effects of the electrode shape, the gas flow rate and the discharge gap on the electron density are discussed. The electron density increases with the increase of input power and the decrease of electrodes gap. The electron density decreases as flow rate increasing for the electrodes with rectangle holes, but almost no response for the electrodes with round holes due to its smaller outlet area. By using this method the electron density in atmospheric pressure radio frequency conductive pure gas discharge can be determined. whenωpe>>ωand vm2>>ωpe2 are satisfied.
OES has been used to diagnose the rotational and vibrational temperature in Ar discharge, and the electron excitation temperature in the Ar/SiCl4 mixture discharge. In Ar discharge as increasing the RF power the rotational temperature increases and the vibrational temperature decreases, which mean that the system trends to thermal balance. The electron excitation temperature has little change with RF power. In Ar/SiCl4 discharge the electron excitation temperature is calculated by the Si atom spectral lines. The electron excitation temperature belongs to the remained electrons.after dissociate SiCl4. The electron excitation temperature decreases with the increasing of the RF power. the SiCl4 flow rate and the Ar flow rate. The bond energy of H2 and SiCl4 are close, while partial electron energy is consumed to dissociate H2. As a result, the H2 influx weakens the discharge.
We deposit the film with the layered structure on the substrate of monocrystalline silicon. ceramic and glass, using self-assembled radio frequency atmospheric plasma jet in open air. The discharge gas is the mixture of Ar, H2 and SiCl4 gas bubbled by Ar. The film thickness, the film content, the content profile along the depth and surface topography have been investigated by step profiler. XPS and SEM respectively. The film has been layered from pure silicon near the substrate to SiO2 close to the film surface. We analyze the mechanism of oxidation process during film deposition, and investigate the reason of layered structure of the films. At the beginning of the film deposition the substrate temperature is low and the oxidation process is attributed to the oxidative radicals, which were generated from decomposition of O2 in the air by atmospheric plasma jet. As time passed by. the substrate temperature becomes higher. When it reached the decomposition temperature of met silicate (150℃). the SiO2 produced by decomposition of met silicate was the primary film pollutant. The flow rate of SiCl4 is the key factor of oxidation rate at the high substrate temperature. The H2 flow rate is very important for Si film growth and oxidation, because it determines the plasma temperature and density. Besides, the hydrogen atom bonding to silicon atom to form Si-H group is an important reason to stop the film oxidation. Therefore although the deposited film is oxidative partially, but properly control the discharge gas flow rate and the substrate temperature should be beneficial to form pure silicon film.
引文
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