柔性衬底上使用等离子增强原子层沉积制备的氮化镓薄膜物性分析

采用等离子增强原子层沉积技术（PE-ALD）在350℃温度下,在KAPTON柔性衬底上直接生长出多晶GaN薄膜。利用低角度掠入射X射线衍射仪、AFM、SEM、TEM、XPS对薄膜的晶体结构、表面形貌及薄膜成分进行了表征和分析。结果表明,薄膜呈多晶态,且具有良好的均匀性;薄膜中的N元素全部以N-Ga键形式存在;大部分Ga元素以Ga-N键形式构成GaN;少量的Ga元素分别以Ga-Ga键和Ga-O键形式构成金属镓以及Ga2O3。研究发现,虽然KAPTON具有较好的耐高温性,但GaN会反向扩散进入KAPTON衬底,形成具有一定厚度的GaN扩散层。     

衬底表面处理对原子层沉积法生长GaN薄膜的影响

采用等离子增强原子层沉积技术于蓝宝石衬底上生长GaN薄膜,研究氮等离子体预处理衬底对薄膜结晶性能的影响.利用X射线衍射仪、扫描电子显微镜、原子力显微镜、X射线光电子能谱仪等手段对薄膜的晶体结构、表面形貌及薄膜成分进行表征和分析.结果表明,经预处理的蓝宝石衬底上生长的GaN薄膜晶体质量明显提高,沿c轴高度择优取向生长;光学带隙约为3.48 eV;薄膜呈n型导电特性,电阻率为2.551×10-2 Ω·cm,载流子浓度高达1.876×1019 cm-3,迁移率为13.04 cm2·V-1·s-1;薄膜中Ga元素主要与N元素以Ga-N键生成GaN.     

玻璃衬底上低温沉积GaN薄膜研究

采用电子回旋共振.等离子体增强金属有机物化学气相沉积(ECR-PEMOCVD)方法在康宁7101型普通玻璃衬底上沉积了GaN薄膜,利用反射高能电子衍射(RHEED)、X射线衍射(XRD)、原子力显微镜(AFM)和霍尔测量系统对样品进行了检测,研究了其结晶性和电学特性随沉积温度的变化.结果表明,当沉积温度为250-430℃时,得到的GaN薄膜都呈现高度的C轴择优取向,结晶性较好;薄膜表面形貌较为平整且呈n型导电.     

等离子体增强原子层沉积制备压电AlN薄膜

采用等离子体增强原子层沉积(PEALD)技术在单晶硅衬底上成功制备了具有(002)晶面择优取向的氮化铝(AlN)晶态薄膜,为设计新型压电功能器件提供了思路.利用椭圆偏振光谱仪(SE)、原子力显微镜(AFM)、X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)对.样品的生长速率、表面形貌、晶体结构、薄膜成分进行了表征和分析.结果 表明,在250℃沉积温度下,以N2H2和Ar的混合气体的等离子体作为共反应物,在相同工艺条件下仅增加前驱体三甲基铝(TMA)脉冲注入之后的氮气吹扫时间(tp1),制备的AlN薄膜的(002)晶面择优取向趋于显著,说明tp1的增加可以促进Al和N原子的有序排列,并促进(002)晶面择优取向形成.实验中,tp1为30 s且循环次数为1150时,PEALD制备的AlN薄膜表面平整光滑,均方根表面粗糙度为0.885 nm,(002)晶面衍射峰最明显,薄膜中氧原子数分数为11.04％,氧原子在AlN薄膜中形成氧缺陷并形成一种稳定的基于八面体配位铝的新型氧缺陷相,XPS结果证明了N-O-Al键的形成.     

立方GaAs(100)衬底上制备单相六方GaN薄膜

立方 Ga As (10 0 )衬底上制备的 Ga N薄膜多为立方结构且立方相为亚稳相 ,采用水平常压 MOCVD方法在立方 Ga As (10 0 )衬底上制备出了 Ga N薄膜 . XRD测试表明 ,薄膜具有单一的相 .结合对工艺条件的分析 ,认为薄膜具有六方结构 .最后 ,通过 Raman光谱测试 ,证实在立方 Ga As衬底上制备出了单相六方 Ga N薄膜 .还对立方 Ga As衬底上制备出六方 Ga N薄膜的原因进行了讨论     

立方GaAs（100）衬底上制备单相六方GaN薄膜

立方GaAs（100）衬底上制备的GaN薄膜多为立方结构且立方相为亚稳相,采用水平常压MOCVD方法在立方GaAs（100）衬底上制备出了GaN薄膜．XRD测试表明,薄膜具有单一的相．结合对工艺条件的分析,认为薄膜具有六方结构．最后,通过Raman光谱测试,证实在立方GaAs衬底上制备出了单相六方GaN薄膜．还对立方GaAs衬底上制备出六方GaN薄膜的原因进行了讨论．     

(001)GaAs衬底上异质外延的立方GaN薄膜与界面

用电子回旋共振微波等离子体辅助金属有机化学气相沉积（ＥＣＲ－ＰＡＭＯＣＶＤ）法，在低温条件下，在（００１）ＧａＡｓ衬底上异质外延，生长了立方晶ＧａＮ薄膜．高分辩电镜（ＨＲＥＭ）观测与Ｘ射线衍射（ＸＲＤ）测量结果表明：ＧａＮ薄膜具有典型的闪锌矿结构；三种方法测得其晶格常数为０．４５１～０．４５７ｎｍ；在ＧａＮ／ＧａＡｓ界面处的生长模式为异质外延；ＧａＮ薄膜中的位错主要为堆垛层错与刃形位错；随着远离界面，ＧａＮ中位错密度与镶嵌组织迅速减少．     

氮气流量对玻璃衬底上低温沉积GaN薄膜结晶性的影响

采用电子回旋共振-等离子体增强金属有机物化学气相沉积(ECR-PEMOCVD)技术,在康宁7101型普通玻璃衬底上沉积了高度C轴择优取向的多晶GaN薄膜.利用反射高能电子衍射(RHEED),X射线衍射(XRD)对样晶进行检测,研究了在低温(430℃)沉积中氮气流量对GaN薄膜结品性的影响.并且利用原子力显微镜(AFM)和室温光敏发光(PL)谱研究了薄膜的表面形貌和发光特性,发现薄膜表面形貌较为平整,其发光峰由较强的紫外近带边发光峰和极其微弱的绿光发光峰组成.     

氮气流量对玻璃衬底上低温沉积GaN薄膜结晶性的影响

采用电子回旋共振-等离子体增强金属有机物化学气相沉积（ECR-PEMOCVD）技术,在康宁7101型普通玻璃衬底上沉积了高度c轴择优取向的多晶GaN薄膜. 利用反射高能电子衍射（RHEED) , X射线衍射 (XRD) 对样品进行检测,研究了在低温（430℃）沉积中氮气流量对GaN薄膜结晶性的影响. 并且利用原子力显微镜 (AFM) 和室温光致发光 (PL) 谱研究了薄膜的表面形貌和发光特性,发现薄膜表面形貌较为平整,其发光峰由较强的紫外近带边发光峰和极其微弱的绿光发光峰组成.     

热原子层沉积技术制备TiAlCN薄膜的特性

在Si和SiO2基底上,采用热原子层沉积技术,以四(二甲基氨基)钛(Ti(N (CH3)2)4)和三甲基铝(Al (CH3)3)为前驱体,制备TiAlCN薄膜.测试结果表明,随着基底温度的升高,膜层的沉积速率升高,电阻率降低,光学带隙由3.45 eV降低到2.00 eV,并在基底温度为300和350℃时出现了双吸收边;基底温度为350℃时,Al (CH3)3分解,使Al进入膜层与TiN和TiC形成TiAlN和TiAlC;膜层中TiN和TiC的形成,可以有效抑制膜层的自然氧化;基底温度为250和300℃时,薄膜为无定型结构,当基底温度为350℃时,有TiN晶体产生;膜层的表面粗糙度随着基底温度的升高先降低后升高,表面粗糙度的升高可能是因为在基底温度为350℃时前驱体材料的分解,使C-H键进入膜层所导致的.     

Low Temperature Stabilization of Nanoscale Epitaxial Spinel Ferrite Thin Films by Atomic Layer Deposition

In this work heteroepitaxial stabilization with nanoscale control of the magnetic Co₂FeO₄ phase at 250 °C is reported. Ultrasmooth and pure Co₂FeO₄ thin films (5–25 nm) with no phase segregation are obtained on perovskite SrTiO₃ single crystal (100) and (110) oriented substrates by atomic layer deposition (ALD). High resolution structural and chemical analyses confirm the formation of the Co‐rich spinel metastable phase. The magneto‐crystalline anisotropy of the Co₂FeO₄ phase is not modified by stress anisotropy because the films are fully relaxed. Additionally, high coervice fields, 15 kOe, and high saturation of magnetization, 3.3 μ_B per formula unit (at 10 K), are preserved down to 10 nm. Therefore, the properties of the ALD‐Co₂FeO₄ films offer many possibilities for future applications in sensors, actuators, microelectronics, and spintronics. In addition, these results are promising for the use of ALD compared to the existing thin‐film deposition techniques to stabilize epitaxial multicomponent materials with nanoscale control on a wide variety of substrates for which the processing temperature is a major drawback.     

硫化锌薄膜的原子层沉积生长及表征

为满足硫化锌(ZnS)薄膜在光学薄膜领域进一步应用的要求,基于原子层沉积(Atomic Layer Deposition, ALD)技术在130℃温度下以二乙基锌(DEZ)和硫化氢(H2S)为反应源,在砷化镓(GaAs)衬底表面沉积了ZnS薄膜。用扫描电子显微镜(Scanning Electron Microscope, SEM)分析了样品的表面形貌和膜界面特性,用X射线衍射仪(X-ray Diffraction, XRD)分析了薄膜的结构特性,并通过X射线光电子能谱(X-ray Photoelectron Spectroscopy, XPS)分析了薄膜的化学成分。研究了厚度对薄膜结构和形貌的影响。结果表明,得到的ZnS薄膜为多晶结构,薄膜的厚度随循环数线性增加,速率为1.45 ?/cycle。对在75℃温度下烘烤48 h后的薄膜进行了XPS分析,得出的Zn/S比为1.07:1,表明烘烤除去了薄膜中残存的H2S。以较短生长时间得到的较薄的薄膜具有更好的表面平整度和更致密的结构。     

Atomic and Molecular Layer Deposition of Hybrid Mo–Thiolate Thin Films with Enhanced Catalytic Activity

A synthetic route toward hybrid MoS₂‐based materials that combines the 2D bonding of MoS₂ with 3D networking of aliphatic carbon chains is devised, leading to a film with enhanced electrocatalytic activity. The hybrid inorganic–organic thin films are synthesized by combining atomic layer deposition (ALD) with molecular layer deposition (MLD) using the precursors molybdenum hexacarbonyl and 1,2‐ethanedithiol and characterized by in situ Fourier transform infrared spectroscopy, and the resultant material properties are probed by X‐ray photoelectron spectroscopy, Raman spectroscopy, and grazing incidence X‐ray diffraction. The process exhibits a growth rate of 1.3 Å per cycle, with an ALD/MLD temperature window of 155–175 °C. The hybrid films are moderately stable for about a week in ambient conditions, smooth (σ_RMS ≈ 5 Å for films 60 Å thick) and uniform, with densities ranging from 2.2–2.5 g cm^?3. The material is both optically transparent and catalytically active for the hydrogen evolution reaction (HER), with an overpotential (294 mV at ?10 mA cm^?2) superior to that of planar MoS₂. The enhancement in catalytic activity is attributed to the incorporation of organic chains into MoS₂, which induces a morphological change during electrochemical testing that increases surface area and yields high activity HER catalysts without the need for deliberate nanostructuring.     

原子层沉积低温生长α-MoO3薄膜

以六羰基钼和氧气为前驱体,通过等离子增强原子层沉积技术（PE-ALD）在硅基片上实现了α-MoO₃薄膜的低温制备。利用X射线衍射仪、扫描电子显微镜、原子力显微镜、X射线光电子能谱仪等手段对薄膜的晶体结构、表面形貌及薄膜成分进行表征和分析。研究发现衬底温度和氧源脉冲时间对MoO₃薄膜的晶体结构和表面形貌变化起关键作用。当衬底温度为170℃及以上时所制备的薄膜为α-MoO₃;适当延长ALD单循环中的氧源脉冲时间有利于低温沉积沿（0k0）高度择优取向的MoO₃薄膜。根据对不同厚度MoO₃薄膜表面的原子力显微图片分析,MoO₃薄膜为岛状生长模式。     

Inherently Area-Selective Atomic Layer Deposition of SiO2 Thin Films to Confer Oxide Versus Nitride Selectivity

Area-selective atomic layer deposition (AS-ALD) offers tremendous advantages in comparison with conventional top-down patterning processes that atomic-level selective deposition can achieve in a bottom-up fashion on pre-defined areas in multi-dimensional structures. In this work, a method for exploiting substrate-dependent selectivity of aminosilane precursors for oxides versus nitrides through chemo-selective adsorption is reported. For this purpose, AS-ALD of SiO₂ thin films on SiO₂ substrates rather than on SiN substrates are investigated. Theoretical screening using density functional theory (DFT) calculations are performed to identify Si precursors that maximize adsorption selectivity; results indicate that di(isopropylamino)silane (DIPAS) has the potential to function as a highly chemo-selective precursor. Application of this precursor to SiN and SiO₂ substrates result in inherent deposition selectivity of ≈4 nm without the aid of surface inhibitors. Furthermore, deposition selectivity is enhanced using an ALD-etch supercycle in which an etching step inserts periodically after a certain number of ALD SiO₂ cycles. Thereby, enlarged deposition selectivity greater than ≈10 nm is successfully achieved on both blanket- and SiO₂/SiN-patterned substrates. Finally, area-selective SiO₂ thin films over 4–5 nm are demonstrated inside 3D nanostructure. This approach for performing inherent AS-ALD expands the potential utility of bottom-up nanofabrication techniques for next-generation nanoelectronic applications.