In situ time-resolved optical measurements of a-Si thin films during excimer laser crystallization

An in situ time-resolved optical reflection and transmission (TRORT) monitoring system combining two He-Ne probe lasers, a digital oscilloscope and three fast photodetectors is developed to investigate the crystallization processes of Si thin films during excimer laser crystallization (ELC). The physical meaning of optical spectra obtained by TRORT measurements has been interpreted in detail. The melt duration and transient phase transformation dynamics of Si thin films can be determined and interpreted immediately. A high efficiency and non-destructive evaluation approach is proposed for determining the grain size of polycrystalline Si after ELC directly and immediacy under appropriate experimental conditions.     

Fabrication of large-grain polycrystalline Ge films using absorptive films

Amorphous germanium (a-Ge) films in samples with or without an absorptive film are crystallized by short-pulse XeF excimer laser crystallization (ELC). An in situ time-resolved optical reflection and transmission (TRORT) monitoring system combining a cw He-Ne probe laser, a digital oscilloscope and two photodetectors is developed to investigate the melting and resolidification dynamics of Ge films during ELC. TRORT measurements reveal that the longest melt duration is prolonged from 250 to 1000 ns by adding absorptive films in the samples. Absorptive films are shown to be effective in improving the melt duration of the molten state and the grain size of polycrystalline Ge films. The grain size with a diameter of approximately 12 μm can be fabricated in the superlateral growth regime for 90-nm-thick a-Ge films at room temperature in air by single-shot ELC.     

Fabrication of large-grain polycrystalline silicon for solar cells

The rapid recrystallization of a-Si films utilizing excimer laser crystallization (ELC) is investigated. The melt duration of liquid silicon (liquid Si) is measured by in-situ time-resolved optical measurements during ELC. The grain size of crystallized poly-Si films are characterized by FE-SEM. The substrate temperature as a function of the longest melt duration of liquid Si for different Si film thicknesses are presented. In-situ timeresolved optical measurements reveal that the longest melt duration of 400-nm-thick a-Si thin films at a substrate temperature of 500 °C is 1714 ns. The diameter of the disk grain as large as 4.7 μm is produced by ELC, which can be applied to solar cells with a high conversion efficiency and reliability.     

Rapid determination of surface roughness of polycrystalline silicon following frontside and backside excimer laser irradiation

Excimer-laser crystallization (ELC) is the most commonly employed technology for fabricating low-temperature polycrystalline silicon (LTPS). Investigations on the surface roughness of polycrystalline silicon (poly-Si) thin films have become an important issue because the surface roughness of poly-Si thin films is widely believed to be related to its electrical characteristics. In this study, we develop a simple optical measurement system for rapid surface roughness measurements of poly-Si thin films fabricated by frontside ELC and backside ELC. We find that the incident angle of 20° is a good candidate for measuring the surface roughness of poly-Si thin films. The surface roughness of polycrystalline silicon thin films can be determined rapidly from the reflected peak power density measured by the optical system developed using the prediction equation. The maximum measurement error rate of the optical measurement system developed is less than 9.71%. The savings in measurement time of the surface roughness of poly-Si thin films is up to 83%. The method of backside ELC is suggested for batch production of low-temperature polycrystalline silicon thin-film transistors due to the lower surface roughness of poly-Si films and higher laser-beam utilization efficiency.     

Solidification velocity in liquid silicon during excimer laser crystallization

Excimer laser crystallization (ELC) is commonly employed to fabricate low-temperature polycrystalline silicon. A time-resolved in-situ optical system with nanosecond response time is developed to monitor and record the phase transformation process during ELC. The average solidification velocity of liquid silicon (liquid Si) is investigated from the optical spectra recorded by a fast oscilloscope. It is found that the average solidification velocities of liquid Si in the partial-melting and complete-melting regimes are fundamentally different. In the partial-melting regime, the average solidification velocity decreases with increasing excimer laser energy density; while in the complete-melting regime, it increases abruptly due to the presence of deeply supercooled liquid Si.     

Characterization of polycrystalline Ge thin films fabricated by short-pulse XeF excimer laser crystallization

XeF excimer laser-induced melting and recrystallization dynamics of amorphous germanium are investigated using time-resolved optical reflection and transmission measurements with a nanosecond time resolution, field-emission scanning electron microscopy, and micro-Raman spectroscopy. It is found that the disc-shaped grain with a diameter of approximately 0.8 μm is located in the complete melting regime with a melt phase duration of approximately 141–200 ns. The significant change of transmissivity is a key phenomenon revealing the excessive excimer laser fluence during excimer laser crystallization by in-situ optical measurements. Differences between the melting and recrystallization phenomenon for Si and Ge thin films are also discussed.     

非晶态Se薄膜的自发晶化研究

利用真空热蒸镀的方法制备了非晶Se薄膜,测试了稳定的非晶Se薄膜,不稳定的非晶Se薄膜和初始自发晶化的非晶Se薄膜的透射率光谱和拉曼光谱,对透射率光谱曲线进行了拟合,计算了薄膜的厚度和折射率随波长的变化关系。在自我晶化过程中,Se薄膜折射率逐渐增大;随波长增大,折射率则减小,初始自发晶体的Se薄膜中,出现标志Se8环和链的结构,不完整的环和链结构在自发晶化过程中得到了增强。     

Studies of thin smectic C films by X-ray reflectivity

The smectic order in thin and ultra thin films (150–600Å) of the chiral ferroelectric liquid crystal mixture ZLI-3654 is studied using the X-ray reflectivity technique. The spin cast films on various substrates (float glass, Si wafer, polymer coated glass, etc.) order spontaneously with smectic layering parallel to the substrate surface. A simple model which assumes a sinusoidal density modulation can describe well the experimental reflectivity profiles. The X-ray reflectivity provides a method to evaluate the phases of the structure factor. We demonstrate, for the first time, that is possible to extract the molecular tilt angle, , in ferroelectric liquid crystals from X-ray reflectivity measurements of ultra thin films. The temperature dependence of the tilt angle in the smectic C^* phase are almost independent of the film thickness (down to 200 Å) and are similar to those in the bulk.     

热致晶化高反射率SbOx薄膜的结构分析和光学性质

利用直流磁控反应溅射法制备了SbOx薄膜,利用X射线衍射分析仪和光谱仪分别研究了这种薄膜热致晶化的微观结构和光学性质的变化,并通过非晶态薄膜粉末的示差扫描量热实验测出不同加热速度条件下结晶峰温度,研究了这种薄膜的结晶动力学。发现沉积态SbOx薄膜为非晶态,非晶态SbOx薄膜在热致晶化过程中发生了两种变化,分别对应为较低温度下Sb晶体和较高温度下立方Sb2O3相的生成。退火后晶态薄膜中出现了单质Sb和Sb2O3,300℃退火后Sb2O3相含量最大。晶态薄膜的反射率均高于沉积态,在晶态薄膜中200℃退火的薄膜反射率最大。     

Non-destructive measurements on recrystallization and grain-size characterization of polycrystalline silicon

Excimer-laser annealing is a widely used technique for producing polycrystalline silicon thin films. We develop an optical inspection system with simple optical arrangements for rapid measurement of recrystallization and grain-size characterization of poly-Si thin films. The recrystallization characterization of the sample after excimer-laser annealing can be easily manifested directly by the profile of peak-power density distribution. We investigate the relation between the maximum grain size of poly-Si thin films and transmission of the optical measurements and find that it coincides with those obtained by field-emission scanning electron microscopy.     

Photoacoustic spectroscopy of thin SiO2 films grown on (100) crystalline Si substrates

Photoacoustic Spectroscopy (PAS) has been used to measure the thickness of thin SiO₂ films grown on (100) Si wafers. The data are in reasonable agreement with a simple theoretical model. It suggests that photoacoustic Spectroscopy is complementary to optical interferometry, in that it is capable of giving quantitative estimates of thin transparent films on opaque substrates of low reflectivity via the transmitted fraction of the optical energy incident on the sample. Both theoretical and experimental results indicate that PAS can be very useful in the measurement of thin films on substrates of low reflectivity.     

Chemical and structural analysis of low-temperature excimer-laser annealing in indium-tin oxide sol-gel films

We investigated the influence of excimer-laser annealing (ELA) on the electrical, chemical, and structural properties of indium–tin oxide (ITO) films prepared by a solution process. The ITO film was prepared by the sol-gel method and annealed by excimer-laser pulses with an energy density up to 240?mJ/cm². Hall measurements showed that the ELA substantially enhanced the electrical properties of the ITO films, including their resistivity, carrier density, and mobility, as increasing the laser energy density. In-depth x-ray photoelectron spectroscopy analysis of the chemical states in the film surface showed that the ELA reduced carbon species and promoted both an oxidation and crystallization. These changes were consistent with results of x-ray diffraction and transmission electron microscopy measurements, where expansions in the microcrystal growth were observed for higher laser energy density. We comprehensively understand that the chemical rearrangement and concomitant crystallization are the main factors for achieving the electrical properties during the ELA. These results suggest the potential of the ELA-treated sol-gel films for providing high-quality ITO films at low temperatures toward the flexible device applications.     

退火对Ge诱导晶化多晶Si薄膜结晶特性的影响

本文采用磁控溅射法, 衬底温度500 ℃下在硅衬底上分别制备具有Ge填埋层的a-Si/Ge 薄膜和a-Si薄膜, 并进行后续退火, 采用Raman光谱、X射线衍射、原子力显微镜及场发射扫描电镜等对所制薄膜样品进行结构表征. 结果表明, Ge有诱导非晶硅晶化的作用, 并得出以下重要结论: 衬底温度为500 ℃时生长的a-Si/Ge薄膜, 经600 ℃退火5 h Ge诱导非晶硅薄膜的晶化率为44%, 在相同的退火时间下退火温度提高到700 ℃, 晶化率达54%. 相同条件下, 无Ge填埋层的a-Si薄膜经800 ℃退火5 h薄膜实现晶化, 晶化率为46%. 通过Ge填埋层诱导晶化可使在相同的条件下生长的非晶硅晶薄膜的晶化温度降低约200 ℃. Ge诱导晶化多晶Si薄膜在Si(200)方向具有高度择优取向, 且在此方向对应的晶粒尺寸约为76 nm. 通过Ge诱导晶化制备多晶Si薄膜有望成为制备高质量多晶Si薄膜的一条有效途径.     

Nanosecond laser pulse induced vertical movement of thin gold films on silicon determined by a modified Michelson interferometer

The vertical movement of a 40 nm thin Au film on a silicon substrate during intense nanosecond (ns) laser irradiation is determined on the nm vertical and ns time scales using an optimized Michelson interferometer. The balanced setup with two detectors uses the inverse interference signal and accounts for transient reflectivity changes during irradiation. We show that a change in phase shift upon reflection must be taken into account to gain quantitative results. Three distinct fluence regimes can be distinguished, characterized by transient reflectivity behavior, dewetting processes and film detachment. Maximum displacement velocities are determined to be 0.6 m/s and 1.9 m/s below and above the melting threshold of the metal, respectively. Flight velocities of detaching liquid films are found to be between 30 and 70 m/s for many nanoseconds.     

Ge2 Sb2 Te5相变薄膜光学及擦除性能研究

利用蓝绿激光对非晶态Ge2Sb2Te5 相变薄膜进行擦除性能的研究,分别用1000 ns,500 ns,100 ns,60 ns脉宽的蓝绿激光进行实验.结果表明,一定脉宽下,反射率对比度随擦除功率的增加而增大.并且,在1000 ns,500 ns,100 ns,60 ns的激光作用时间范围内,非晶态薄膜均可转变成晶态.对于脉宽为60 ns的蓝绿激光,擦除功率大于4.49 mW以后,薄膜的反射率对比度高于15％,这表明Ge2Sb2Te5相变薄膜在短脉宽、低擦除功率条件下,可具有较高的晶化速度.同时,分析了非晶态和晶态Ge2Sb2Te5相变薄膜的光谱特性,对比研究了780 nm,650 nm,514 nm和405 nm波长处的反射率和反射率对比度,提出了Ge2Sb2Te5相变薄膜用于蓝光光盘的改进方法.     

SbOx Thin Films Used for Write-Once Blue Laser Recording

SbOx thin films are deposited by reactive dc-magnetron sputtering from an antimony metal target in Ar＋O2 with the relative O2 content 7%. It is found that the as-deposited films can represent a two-component system comprising amorphous Sb and amorphous Sb2 O3. The crystallization of Sb is responsible for the changes of optical properties of the films. The results of the static test show that the SbOx thin films have good writing sensitivity for blue laser beams and the recording marks are very clear and circular. High reflectivity contrast of about 41% is obtained at a writing power 6mW and writing pulse width 300ns. In addition, the films show a good stability after reading 10000 times.     

干涉法测量多层透明膜系反射率

应用干涉法实现透明膜系反射率的测量。将待测膜系镀在两薄玻璃片，并构成F-P干涉仪，根据透射光谱的自由谱宽和干涉峰的半宽值，计算出膜系反射率，避免了光源波动对测量结果的影响。在实验所用膜系的反射率小于98％时，测量误差小于0．09％。     

Nickel-disilicide-assisted excimer laser crystallization of amorphous silicon

Polycrystalline silicon (poly-Si) thin film has been prepared by means of nickel-disilicide (NiSi多晶硅 受激准分子激光器结晶 结晶化 界面晶粒生长polycrystalline silicon, excimer laser crystallization,Ni-disilicide, Ni-metal-induced lateral crystallization, two-interface grain growthProject supported by the National High Technology Development Program of China (Grant No 2002AA303250) and by the National Natural Science Foundation of China (Grant No 60576056).9/7/2005 12:00:00 AM3/6/2006 12:00:00 AMPolycrystalline silicon （poly-Si） thin film has been prepared by means of nickel-disilicide （NiSi2） assisted excimer laser crystallization （ELC）. The process to prepare a sample includes two steps. One step consists of the formation of NiSi2 precipitates by heat-treating the dehydrogenated amorphous silicon （a-Si） coated with a thin layer of Ni. And the other step consists of the formation of poly-Si grains by means of ELC. According to the test results of scanning electron microscopy （SEM）, another grain growth model named two-interface grain growth has been proposed to contrast with the conventional Ni-metal-induced lateral crystallization （Ni-MILC） model and the ELC model. That is, an additional grain growth interface other than that in conventional ELC is formed, which consists of NiSi2 precipitates and a-Si. The processes for grain growth according to various excimer laser energy densities delivered to the a-Si film have been discussed. It is discovered that grains with needle shape and most of a uniform orientation are formed which grow up with NiSi2 precipitates as seeds. The reason for the formation of such grains which are different from that of Ni-MILC without migration of Ni atoms is not clear. Our model and analysis point out a method to prepare grains with needle shape and mostly of a uniform orientation. If such grains are utilized to make thin-film transistor, its characteristics may be improved.     

激光晶化形成纳米硅材料的场电子发射性质研究

利用KrF准分子激光退火超薄非晶硅膜,并结合热退火技术制备了单层纳米硅薄膜并研究了薄膜的场电子发射性质.在晶化形成的纳米硅薄膜中可以观测到稳定的场电子发射现象,其开启电场从原始淀积的非晶硅薄膜的17V/μm降低到8.5V/μm,而场发射电流密度可以达到0.1mA/cm².激光晶化后形成的纳米硅材料的场电子发射特性的改善可以从薄膜表面形貌的改变以及高密度纳米硅的形成所导致的内部电场增强作用来解释. 关键词： 纳米硅 场发射 激光晶化