一种新的SiC外延材料质量评估方法
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摘要
虽然现在SiC外延层在缺陷密度和尺寸等方面都有较大改进,但生长速率低、缺陷密度高、产量低、成本高以及不能大批量生产等因素依然限制着SiC外延层材料和器件的发展。提高SiC外延材料生长速率,降低其缺陷密度和生产成本,都需依据其质量特性参数寻找相应的解决方法,从而有目的地对外延工艺进行改进、优化。
光学无损表征是目前表征技术发展的新潮流。傅立叶变换红外反射谱(FTIR)不但费用低廉,而且具有无损和可在线测试的优点。由于在中红外区的13～10μm波段,SiC中的长波光学声子与红外光谐振产生剩余射线带,在该波段以外的区域,长波光学声子不与红外光谐振,因此在碳化硅中可传播较长的距离,因此根据红外响应介电函数和多层膜反射理论对红外镜面反射谱进行模拟和解析,可获得外延层与衬底系统的质量特性参数。
本文重点研究了用近垂直入射的红外镜面反射谱对SiC外延材料的无损表征,并将其解析结果与其它的表征技术如X射线光电子能谱(XPS)(原位宽扫描和窄扫描模式)、傅立叶变换红外衰减全反射谱、拉曼散射谱(RSS)(背散射模式)、X射线衍射(XRD)(θ-2θ模式、薄膜反射模式和ω扫描模式)和横截面扫描电子显微镜(SEM)等的所有解析结果进行了比较,获得了以下结果:
1)解析了SiC外延层表面的红外衰减全反射谱和XPS宽扫描谱,研究了拟合峰数目、峰型和背底对XPS窄扫描谱拟合结果的影响,确定的C1s、Si2p和O1s窄扫描谱的最优拟合参数为:位置、半高宽和峰面积不固定的10个高斯峰和Shirley背底;确定的SiC外延层表面化学态结构及其原子的芯电子束缚能分别为: Si(CH_2)_4(BE_(C1s)=282.50eV,BE_(Si2p)= 99.86eV),SiO(CH_2)_3(BE_(C1s)=283.18eV, BE_(Si2p)=100.41eV,BE_(O1s)=532.34eV),SiO_2(CH_2)_2/SiO_2(CH_3)_2(BE_(C1s)=284.99eV,BE_(Si2p)= 101.44eV,BE_(O1s)=532.95eV),SiO_3(CH_3)(BE_(C1s)=286.36eV,BE_(Si2p)=102.43eV),BE_(O1s)= 533.55eV),Si-Si(BE_(Si2p)=99.23eV),H_2O(BE_(O1s)=529.76eV),缔合OH(BE_(O1s)=530.96 eV),Si-OH(BE_(O1s)= 531.70eV),填隙O(BE_(O1s)= 533.96eV),O_2(BE_(O1s)= 541.50eV);
2)根据红外响应介电函数、能量损失函数和红外光与SiC外延层-衬度系统作用等对SiC外延层-衬底系统的测试红外镜面反射谱进行解析,得到的SiC外延层的ωT O和ωLO频率分别为796.4cm~(-1)和963.5cm~(-1),组分为SiC和Si-OH键,表面法线与光轴(c轴)夹角为90°,晶轴与表面法线垂直,高频介电常数为6.56;
3)构建了单面抛光SiC衬底的半无限体结构模型和半无限衬底上单层膜结构模型,根据菲涅耳公式和多层膜转移矩阵理论计算了模型系统的反射率,研究了其各个参数对系统红外镜面反射谱的影响,并用模型系统对衬底的测试红外镜面反射谱谱进行了模拟,结果表明半无限体结构模型不适合描述该SiC衬底结构,半无限衬底上单层膜结构模型非常适合描述其结构,衬底表面存在光学声子衰减常数远大于体材料光学声子衰减常数,等离子体频率大于体材料等离子体频率,等离子衰减常数小于体材料衰减常数的薄的非晶层。
4)除了构建外延层-衬底系统的半无限衬底上单层膜结构模型外,本文还构建了外延层-衬底系统的半无限衬底上双层膜和半无限衬底上三层膜结构模型,用红外响应介电函数和多层膜转移矩阵理论分别计算了其反射率,研究了其各参数对模型系统红外镜面反射谱的影响,并用模型系统分别对三个测试的谱形差异较大的外延层-衬底系统的红外镜面反射谱进行模拟,结果表明SiC外延层-衬底系统应用半无限衬底上三层膜结构模型来描述,外延层表层存在与前面衬底表层类似的薄非晶层,外延层与衬底间存在等离子体非零的界面层。
5)对比了SiC外延层样品红外镜面反射谱的解析结果与RSS谱、XRD、XPS和横截面SEM图的解析结果发现,红外镜面反射谱的解析结果,不但包含了其它表征技术提供的凄凉参数信息,而且其结果吻合地非常好。加之,红外镜面反射谱具有测试费用低、无需样品制备、无损及可在线检测的优点,由此作者指出,傅立叶变换红外镜面反射谱是一种新的SiC外延材料质量评估技术。
The fact such as low growth rate, high defects density, low yield and high cost hinders the development of SiC epitaxy material and devices. To overcome all these problems, quality parameters of SiC epilayer must be obtained frequently, so as to improve the epitaxy process technologically.
Being one of the popular optical nondestructive characterization techniques, Fourier transformation infrared spectroscopy(FTIR) pertains the features of low cost and nondestructive, and can be used in online testing occasions. In SiC, long-wavelength optical phonons resonate only with intermediate infrared photons, so according to the infrared response dielectric function and multi-layer reflection theory, the infrared specular reflection spectroscopy can be simulated and analyzed, from which the quality parameters of SiC epilayer and substrate system can be acquired.
In this thesis, different techniques such as FTIR(attenuation total refection mode and specular reflection mode), x-ray photoelectronic spectroscopy(XPS)(in-situ wide scanning and narrow scanning modes),Raman scattering spectra(back scattering mode),x-ray diffraction pattern(θ-2θmode, thin film refection mode andωscanning mode), spectra and cross-section scanning electron microscopy(SEM) were used to characterize SiC epilayer, and the following results were obtained:
(1) By the analysis of the attenuation total refection spectroscopies and the wide scanning XPS, the influences of peak number, peak types and backgrounds on the fitting results of narrow scanning XPS were studied in detail. Based on that, the optimum fitting parameters of narrow scanning spectroscopies of C1s, Si2p and O1s were determined to be ten Gaussian peaks with unpredictable locations, FWHM and peak areas and Shirley background. The chemical states and core-level electrons bonding energies on the surface of SiC epilayer were further determined to be: Si(CH_2)_4 (BE_(C1s)=282.50eV, BE_(Si2p)=99.86eV), SiO(CH_2)_3 (BE_(C1s)=283.18eV, BE_(Si2p) =100.41eV, BE_(O1s)=532.34eV), SiO_2(CH_2)_2/SiO_2(CH_3)_2 (BE_(C1s)=284.99eV, BE_(Si2p)=101.44eV, BE_(O1s)=532.95eV), SiO_3(CH_3) (BE_(C1s)=286.36eV, BE_(Si2p)=102.43eV, BE_(O1s)= 533.55eV), Si-Si(BE_(Si2p)=99.23eV), H_2O(BE_(O1s)=529.7eV), OH associate complex (BE_(O1s)=530.96eV),Si-OH(BE_(O1s)=531.70eV), interstitral O atom (BE_(O1s)= 533.96eV), O_2(BE_(O1s)= 541.50eV).
(2) According to the infrared response dielectric function , energy loss function and interaction theory of the infrared photons with long optical phonons in SiC crystal, the frequencies of the transverse and longitudinal optical phonons in SiC epilayer were decided to be 796.4cm~(-1) and 963.5cm~(-1), respectively. And the composition of SiC epilayer was further determined to be SiC and Si-OH bonds, with surface normal line perpendicular to crystal axis. The high frequency relative permittivity of SiC epilayer was determined to be 6.56.
(3) A semi-infinite bulk structural model and a semi-infinite bulk plus single layer structural model were built for the single side polished SiC substrate, based on which the influence of each parameter on the infrared specular reflection spectroscopy were investigated. And further the infrared specular reflection spectroscopy of the two model systems were simulated. Results indicated that the semi-infinite buck structural model was unsuitable for SiC substrate, while the semi-infinite bulk plus single layer structural model fitted the SiC substrate structrue very well, and there were a thin amorphous SiC layer on top of the substrate.
(4) Besides the above mentioned two models, a semi-infinite bulk plus three-layer structural model was built for SiC epi-layer and substrate system, and by which the influences of the parameters on the infrared specular reflection spectroscopy of the system were investigated. The infrared specular reflection spectroscopy simulations based on the three models showed that, the SiC epilayer and substrate system ought to be described by the semi-infinite bulk plus three-layer structural model. There were a thin amorphous SiC layer on top of the epi-layer, and a interface layer with plasmons between the epilayer and substrate.
(5) The interpretations of both the infrared specular reflection spectroscopy and other common used charaterization techniques showed that the infrared specular reflection spectroscopy could provide all the quality parameters obtainable by other techniques with equivalent precisions, while pertains features of low cost, nondestructive, without sample preparation and online testing at the same time.
光学无损表征是目前表征技术发展的新潮流。傅立叶变换红外反射谱(FTIR)不但费用低廉,而且具有无损和可在线测试的优点。由于在中红外区的13～10μm波段,SiC中的长波光学声子与红外光谐振产生剩余射线带,在该波段以外的区域,长波光学声子不与红外光谐振,因此在碳化硅中可传播较长的距离,因此根据红外响应介电函数和多层膜反射理论对红外镜面反射谱进行模拟和解析,可获得外延层与衬底系统的质量特性参数。
本文重点研究了用近垂直入射的红外镜面反射谱对SiC外延材料的无损表征,并将其解析结果与其它的表征技术如X射线光电子能谱(XPS)(原位宽扫描和窄扫描模式)、傅立叶变换红外衰减全反射谱、拉曼散射谱(RSS)(背散射模式)、X射线衍射(XRD)(θ-2θ模式、薄膜反射模式和ω扫描模式)和横截面扫描电子显微镜(SEM)等的所有解析结果进行了比较,获得了以下结果:
1)解析了SiC外延层表面的红外衰减全反射谱和XPS宽扫描谱,研究了拟合峰数目、峰型和背底对XPS窄扫描谱拟合结果的影响,确定的C1s、Si2p和O1s窄扫描谱的最优拟合参数为:位置、半高宽和峰面积不固定的10个高斯峰和Shirley背底;确定的SiC外延层表面化学态结构及其原子的芯电子束缚能分别为: Si(CH_2)_4(BE_(C1s)=282.50eV,BE_(Si2p)= 99.86eV),SiO(CH_2)_3(BE_(C1s)=283.18eV, BE_(Si2p)=100.41eV,BE_(O1s)=532.34eV),SiO_2(CH_2)_2/SiO_2(CH_3)_2(BE_(C1s)=284.99eV,BE_(Si2p)= 101.44eV,BE_(O1s)=532.95eV),SiO_3(CH_3)(BE_(C1s)=286.36eV,BE_(Si2p)=102.43eV),BE_(O1s)= 533.55eV),Si-Si(BE_(Si2p)=99.23eV),H_2O(BE_(O1s)=529.76eV),缔合OH(BE_(O1s)=530.96 eV),Si-OH(BE_(O1s)= 531.70eV),填隙O(BE_(O1s)= 533.96eV),O_2(BE_(O1s)= 541.50eV);
2)根据红外响应介电函数、能量损失函数和红外光与SiC外延层-衬度系统作用等对SiC外延层-衬底系统的测试红外镜面反射谱进行解析,得到的SiC外延层的ωT O和ωLO频率分别为796.4cm~(-1)和963.5cm~(-1),组分为SiC和Si-OH键,表面法线与光轴(c轴)夹角为90°,晶轴与表面法线垂直,高频介电常数为6.56;
3)构建了单面抛光SiC衬底的半无限体结构模型和半无限衬底上单层膜结构模型,根据菲涅耳公式和多层膜转移矩阵理论计算了模型系统的反射率,研究了其各个参数对系统红外镜面反射谱的影响,并用模型系统对衬底的测试红外镜面反射谱谱进行了模拟,结果表明半无限体结构模型不适合描述该SiC衬底结构,半无限衬底上单层膜结构模型非常适合描述其结构,衬底表面存在光学声子衰减常数远大于体材料光学声子衰减常数,等离子体频率大于体材料等离子体频率,等离子衰减常数小于体材料衰减常数的薄的非晶层。
4)除了构建外延层-衬底系统的半无限衬底上单层膜结构模型外,本文还构建了外延层-衬底系统的半无限衬底上双层膜和半无限衬底上三层膜结构模型,用红外响应介电函数和多层膜转移矩阵理论分别计算了其反射率,研究了其各参数对模型系统红外镜面反射谱的影响,并用模型系统分别对三个测试的谱形差异较大的外延层-衬底系统的红外镜面反射谱进行模拟,结果表明SiC外延层-衬底系统应用半无限衬底上三层膜结构模型来描述,外延层表层存在与前面衬底表层类似的薄非晶层,外延层与衬底间存在等离子体非零的界面层。
5)对比了SiC外延层样品红外镜面反射谱的解析结果与RSS谱、XRD、XPS和横截面SEM图的解析结果发现,红外镜面反射谱的解析结果,不但包含了其它表征技术提供的凄凉参数信息,而且其结果吻合地非常好。加之,红外镜面反射谱具有测试费用低、无需样品制备、无损及可在线检测的优点,由此作者指出,傅立叶变换红外镜面反射谱是一种新的SiC外延材料质量评估技术。
The fact such as low growth rate, high defects density, low yield and high cost hinders the development of SiC epitaxy material and devices. To overcome all these problems, quality parameters of SiC epilayer must be obtained frequently, so as to improve the epitaxy process technologically.
Being one of the popular optical nondestructive characterization techniques, Fourier transformation infrared spectroscopy(FTIR) pertains the features of low cost and nondestructive, and can be used in online testing occasions. In SiC, long-wavelength optical phonons resonate only with intermediate infrared photons, so according to the infrared response dielectric function and multi-layer reflection theory, the infrared specular reflection spectroscopy can be simulated and analyzed, from which the quality parameters of SiC epilayer and substrate system can be acquired.
In this thesis, different techniques such as FTIR(attenuation total refection mode and specular reflection mode), x-ray photoelectronic spectroscopy(XPS)(in-situ wide scanning and narrow scanning modes),Raman scattering spectra(back scattering mode),x-ray diffraction pattern(θ-2θmode, thin film refection mode andωscanning mode), spectra and cross-section scanning electron microscopy(SEM) were used to characterize SiC epilayer, and the following results were obtained:
(1) By the analysis of the attenuation total refection spectroscopies and the wide scanning XPS, the influences of peak number, peak types and backgrounds on the fitting results of narrow scanning XPS were studied in detail. Based on that, the optimum fitting parameters of narrow scanning spectroscopies of C1s, Si2p and O1s were determined to be ten Gaussian peaks with unpredictable locations, FWHM and peak areas and Shirley background. The chemical states and core-level electrons bonding energies on the surface of SiC epilayer were further determined to be: Si(CH_2)_4 (BE_(C1s)=282.50eV, BE_(Si2p)=99.86eV), SiO(CH_2)_3 (BE_(C1s)=283.18eV, BE_(Si2p) =100.41eV, BE_(O1s)=532.34eV), SiO_2(CH_2)_2/SiO_2(CH_3)_2 (BE_(C1s)=284.99eV, BE_(Si2p)=101.44eV, BE_(O1s)=532.95eV), SiO_3(CH_3) (BE_(C1s)=286.36eV, BE_(Si2p)=102.43eV, BE_(O1s)= 533.55eV), Si-Si(BE_(Si2p)=99.23eV), H_2O(BE_(O1s)=529.7eV), OH associate complex (BE_(O1s)=530.96eV),Si-OH(BE_(O1s)=531.70eV), interstitral O atom (BE_(O1s)= 533.96eV), O_2(BE_(O1s)= 541.50eV).
(2) According to the infrared response dielectric function , energy loss function and interaction theory of the infrared photons with long optical phonons in SiC crystal, the frequencies of the transverse and longitudinal optical phonons in SiC epilayer were decided to be 796.4cm~(-1) and 963.5cm~(-1), respectively. And the composition of SiC epilayer was further determined to be SiC and Si-OH bonds, with surface normal line perpendicular to crystal axis. The high frequency relative permittivity of SiC epilayer was determined to be 6.56.
(3) A semi-infinite bulk structural model and a semi-infinite bulk plus single layer structural model were built for the single side polished SiC substrate, based on which the influence of each parameter on the infrared specular reflection spectroscopy were investigated. And further the infrared specular reflection spectroscopy of the two model systems were simulated. Results indicated that the semi-infinite buck structural model was unsuitable for SiC substrate, while the semi-infinite bulk plus single layer structural model fitted the SiC substrate structrue very well, and there were a thin amorphous SiC layer on top of the substrate.
(4) Besides the above mentioned two models, a semi-infinite bulk plus three-layer structural model was built for SiC epi-layer and substrate system, and by which the influences of the parameters on the infrared specular reflection spectroscopy of the system were investigated. The infrared specular reflection spectroscopy simulations based on the three models showed that, the SiC epilayer and substrate system ought to be described by the semi-infinite bulk plus three-layer structural model. There were a thin amorphous SiC layer on top of the epi-layer, and a interface layer with plasmons between the epilayer and substrate.
(5) The interpretations of both the infrared specular reflection spectroscopy and other common used charaterization techniques showed that the infrared specular reflection spectroscopy could provide all the quality parameters obtainable by other techniques with equivalent precisions, while pertains features of low cost, nondestructive, without sample preparation and online testing at the same time.
引文
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