采用EBSD方法研究高纯Al溅射靶材的微观结构

高纯Al溅射靶材在电子信息产品制造业有着广泛应用。微观结构与组织的均匀性、晶粒尺寸和取向分布对高纯Al溅射靶材的性能有很大的影响。本文采用EBSD技术对高纯Al溅射靶材的晶粒取向分布进行了分析,探索了晶粒取向与溅射速率关系,并采用EBSD大面积扫描对高纯Al溅射靶材的晶粒尺寸及微观结构与组织均匀性进行了研究。     

超高纯Al-0.5%Cu合金溅射靶材微观组织与织构的EBSD分析

用EBSD技术对超高纯（99.9995%以上）Al-0.5%Cu合金靶材冷轧及退火过程中的微观组织、织构及取向差进行了表征,分析了合金靶材多向冷轧、退火过程中微观组织、织构及取向差等的演变规律。     

高纯钽交叉轧制过程中微观结构和织构梯度的演变

高纯钽板在交叉轧制过程中,通过控制轧制的道次,得到了70％,82％和87％变形量的样品.应用X-射线衍射(XRD)技术测量了轧制样品1/8厚度层,1/4厚度层和中间层的宏观织构,并对样品沿厚度方向上的变形组织与微织构进行电子背散射衍射(EBSD)表征.结果表明,随着交叉轧制变形量的增加,{111} 和{100}取向晶粒的取向分裂程度增加,并且{111}取向的晶粒分裂程度高于{100}取向的晶粒.变形量为70％时,高纯钽板沿厚度方向存在强烈的微观组织和织构梯度,中间层具有强烈的{111}取向晶粒,而1/8厚度层主要为{100} 取向.随着变形量增加,高纯钽板沿厚度方向的微观组织和织构均匀性得到改善.当变形量达到87％时,表面和中心的{100} 和{111} 取向晶粒都为长条状且交互分布在一起,使得钽板沿厚度方向织构梯度得到减弱,同时获得均一的晶粒尺寸.     

高纯钽板中晶粒生长的取向相关性研究

钽溅射靶材主要用于集成电路中导线的扩散阻挡层,其溅射性能受微观组织影响较大。本文采用电子背散射衍射( EBSD)技术,结合Extend Cahn-Hagel模型对周向轧制钽板的再结晶行为进行分析。并侧重于钽板再结晶初、中期与取向相关的晶粒生长速率的研究。结果表明,{111}?uvw?(?111?//ND)晶粒具有生长优势,初始阶段生长速率约为同期{001}?uvw?(?100?//ND)晶粒的1?6倍。     

半导体用高利用率长寿命溅射靶材的研制

半导体制造工艺中使用的高纯金属溅射靶材的利用率直接关系到靶材自身的使用寿命和芯片制作的成本,在靶材研制中需要重点关注。以晶圆制造中广泛应用的高纯铝、铜等靶材为例,介绍了溅射靶材的发展演变,并以靶材使用前后轮廓测量为基础,研究了100~300 mm晶圆制造用靶材的利用率。结果表明,常规靶材随着尺寸增加和溅射工艺的严格控制,靶材利用率减小(30%)。制备高利用率的大尺寸长寿命靶材,需对靶材的溅射面形貌和靶材厚度等方面进行结构优化设计,经优化设计后的靶材利用率最大可达到50%以上,使用寿命亦显著延长。     

EBSD技术在形变Zr合金组织与织构研究中的应用

本文采用配备在扫描电镜中的EBSD系统及相应的取向分析和组织重构技术,对形变状态和退火状态下Zr合金的微观组织及织构演变规律进行了初步研究。结果表明,形变样品中晶粒细碎且不均匀,具有较为明显的形变带特征;织构主要为基面平行于轧面（（0002）／／Z）取向织构,同时还存在较多的{0001}（1010）和{0001}（1150）织构及{1104}（1102）织构。退火样品中晶粒均匀,基本为等轴晶,几种主要基面织构变化不大,但{1104}（1102）织构含量与形变样品相比提高了一倍以上。     

放电等离子体烧结镍的形变组织研究(英文)

利用放电等离子体烧结(SPS)技术制备了粗晶(13μm)和细晶(2μm)两种镍样品。EBSD分析表明,两种烧结样都没有织构,且它们的晶粒都为完全再结晶组织。对此烧结样进行单轴压缩,研究晶粒尺寸对形变中微观组织演变的影响。在样品坐标系中,用每个像素点相对于平均取向的旋转轴来构图,结果显示在一些大晶粒中有扩展的平直界面。滑移迹线和Schmid因子分析表明,这些界面平行于{111}迹线的晶粒,其取向与前人研究的有相同微观组织的大晶粒取向相同。对于SPS烧结的粗晶样和细晶样,几乎每个晶粒内部都发生了一定程度的晶粒分裂。     

金属膜电阻器用高阻靶材制备工艺研究

金属膜电阻器用的靶材是影响膜质量和电阻器性能的重要因素之一,晶粒细化是炼制致密性靶材的关键.晶粒细化不仅有利于Cr-Si靶材内部组织均匀化,且能降低其韧脆转变温度,从而使炼制的靶材强度和硬度高、塑性好,提高靶材的成品率.分析了晶粒细化提高靶材综合性能的原因,并介绍了研究中所采用的Ti细化剂、磁力搅拌等晶粒细化措施.实验表明,在RJ24生产线上溅射的1 MΩ金属膜电阻器具有较好的性能,且电阻温度系数均小于20×10-6/℃.     

气氛热处理对无取向硅钢组织及织构的影响

本文以鞍钢生产的50AW 600牌号的无取向硅钢为研究对象,进行常规热处理和气氛热处理试验。根据冷轧无取向硅钢退火工艺的特点,研究了退火温度和保温时间对冷轧无取向硅钢晶粒组织和织构演变的影响;同时,也研究了不同的热处理气氛对无取向硅钢织构的影响。结果表明,气氛热处理条件下的无取向硅钢的晶粒要比常态下及常规热处理条件下的晶粒粗大,且比较均匀;气氛热处理形成了有利织构,提高了其磁性能;同全氢气氛相比较,氨分解气氛更有利于50AW 600无取向硅钢有利织构的形成。     

高硅钢温轧过程压下率及中间退火对组织、织构的影响

传统轧制法制备6．5wt．％高硅钢过程中温轧工艺具有显著不同于3wt．％Si的电工钢的特点及组织织构特征,是开发新型基于织构优化的高硅钢的关键环节。采用EBSD技术对通过热轧、温轧、冷轧及退火工艺制备0．3mm厚的6．5wt．％Si电工钢板的组织和织构进行分析,重点研究温轧过程中的中间退火和大、小压下率组合以控制织构。结果表明,在热轧退火板是部分再结晶组织的情况下,一次性温轧或先小形变量、中间退火后再大形变量的工艺可得到更多的Goss晶粒;经过最终退火后Goss取向会发生偏转,形成部分黄铜取向,而{111}（112）取向的晶粒内形核生成近Goss取向的再结晶晶粒;大压下量轧制是最终组织中{111}取向晶粒较多的主要原因。     

Correlating discrete orientation and grain size to the sputter deposition properties of tantalum

Recent findings indicate that the erosion behavior of tantalum sputtering targets varies across regions of different discrete crystal orientation. Specifically, bands of sharp, localized (100) texture amid the microstructure and aligned parallel to the sputtering surface of planar tantalum targets have been shown to resist erosion. Referencing theoretical models and characterization studies of wrought tantalum, this paper explores the relationship between discrete crystallographic texture and grain size of tantalum with respect to the physical erosion behavior of tantalum sputtering targets. The findings demonstrate that both grain size and preferred orientation contribute to the deposition behavior of tantalum. Also, controlling both the microstructural and textural homogeneity are key to assuring the reliability of Ta targets and the subsequent integrity of the sputter-deposited thin films.     

Zr掺杂TaOx薄膜离子导体性能的研究

采用射频反应磁控溅射工艺,以纯钽、锆为靶材,在WO3/ITO/玻璃基材上制备TaOx:Zr薄膜。研究锆掺入量、掺杂方式、溅射功率等制备工艺参数对TaOx薄膜性能的影响。用三位电极法和透射光谱等方法检测薄膜的离子导电性能。结果表明:TaOx:Zr薄膜主要为非晶态,在150 W的掺杂溅射功率和10 min的相对掺杂时间的实验条件下,所制备的TaOx:Zr薄膜有良好的离子导电性能,透光率约为90%。     

Dual Process Dielectric Formation for Decoupling Capacitors on Flexible Substrates

Large area, high density integrated capacitors within printed wiring boards can provide a substantial decoupling capacitance with very low parasitic inductance. Tantalum pentoxide (Ta₂O₅) is an excellent dielectric for this application due to the relatively high dielectric constant (~ 22-24), however the difficulty of fabricating large, defect-free capacitors has thus far prevented the realization of practical applications. This work demonstrates high performance capacitors with Ta₂O₅ dielectric developed with a two step oxidation scheme consisting of reactive sputtering followed by anodization. Thin films of Ta₂O₅ were deposited by reactive sputtering on silicon and also on Upilex^reg covered glass wafers using dc magnetron sputtering with a gas flow ratio of 10/90 O₂/Ar. In the two-step oxidation scheme, anodization is performed after reactively sputtering tantalum oxide films to obtain a densifled oxide structure. The electrical and physical properties of these two step sputtered/ anodized tantalum oxide films are shown to be superior to those of tantalum oxide films prepared by either anodization or sputtering alone. This work has shown that Ta₂O₅ is a potential dielectric for integrated capacitors that could be used in advanced packaging applications.     

钽薄膜淀积速率与阻挡效果的研究

在硅衬底上用不同淀积速率溅射得到了 60 nm厚钽薄膜作为铜布线工艺中的扩散阻挡层。样品在退火前后 ,用二次离子质谱仪 (SIMS)对钽膜的阻挡效果进行鉴定 ,原子力显微镜 (AFM)分析了钽薄膜的形貌结构。研究发现不同淀积速率制作的钽膜由于其结构的差异对铜硅互扩散有着不同的阻挡效果 ,并提出样品在退火时 ,薄膜晶粒的重结晶过程是导致阻挡层失效的重要因素之一     

Tantalum-film technology

In tantalum film circuitry, capacitors, resistors, and rudimentary interconnections are all produced in a single pattern of tantalum. Important processes are discussed in detail including 1) sputtering, by which tantalum films are produced, 2) pattern generation, and 3) anodization, by which capacitor dielectrics are formed and by which resistors are protected and adjusted to value. Predominantly the discussion is based on developments and practices of Bell Telephone Laboratories. Capacitors withstand stresses of several million volts/cm, have low leakages, a temperature coefficient of +200 to +250 ppm/°C, and a dissipation factor at 1 kc of 1 per cent maximum. Resistors of outstanding quality can be made from tantalum nitride produced by reactive sputtering. These resistors have high electrical stability and low temperature coefficients and can be fabricated to initial tolerances as low as 0.01 per cent. Because of the versatility of tantalum technology, a wide variety of circuit types can be fabricated. Tantalum technology is particularly valuable in the fabrication of thin-film integrated circuits with severe precision requirements as in the precise tuning of thin-film notch filters, and for distributed parameter networks.     

微波电路用共面电极TaNx薄膜片式电阻器

采用反应溅射方法制作TaNx电阻薄膜,并通过溅射Ni、Au形成双层共面电极。研究了溅射条件对电阻薄膜组分的影响以及此类电阻器的微波特性。结果显示,溅射工作真空度小于0.5Pa,氮气体积分数大于5%时,可以得到阻值稳定的六方晶体结构TaNx电阻薄膜,其共面电极的电阻器使用频率上限大于20GHz。     

Hafnium tantalum nitride resistive sea for the silicon diode-array camera tube target

A new material has been developed as a resistive sea for the silicon diode-array camera tube target. The material is prepared by reactive sputtering of a hafnium tantalum cathode in a nitrogen atmosphere. By adjusting the relative amounts of hafnium and tantalum in the cathode or by changing the sputtering parameters, the resistivity of the hafnium tantalum nitride sea may be optimized. The nitride may be heated to 350°C during camera tube bakeout with no degradation in performance. By controlling the film deposition conditions, electrostatic focus camera tubes have been made with excellent aging, dark current, lag, and resolution characteristics.     

High-performance tantalum oxide capacitors fabricated by a novelreoxidation scheme

High-performance tantalum oxide capacitors with excellent reliability that were developed by a two-step oxidation scheme are discussed. An anodic reoxidation process is applied to the reactively sputter-deposited tantalum oxide films to make the densified oxide structure. The electrical and physical properties as well as the reliability of these two-step oxidized sputtered/anodized tantalum oxide films are shown to be much superior to those of conventional tantalum oxide films prepared by either anodization or sputtering alone. Capacitors made of the sputtered/anodized tantalum oxide film have greatly improved electrical properties and better reliability than anodized or sputtered tantalum oxide capacitors and are very useful for applications to high-capacity storage capacitors in future high-density VLSI memories