MOCVD

MOCVD
  • 文章类型: Journal Article
    二维(2D)材料的热膨胀系数(TEC)的当前报告显示出跨越数量级的大差异。由于涉及原子薄且光学透明的样品的间接测量的方法,确定任何2D材料的TEC仍然是困难的。我们展示了一种解决这种差异的方法,并使用四维扫描透射电子显微镜(4D-STEM)直接测量标称单层外延WSe2的TEC。实验上,使用桶式加热样品架将来自金属有机化学气相沉积(MOCVD)的WSe2加热至18-564°C的温度范围,以观察温度引起的结构变化,而不会对样品造成额外的改变或破坏。通过将4D-STEM测量与定量结构分析相结合,对于平面内和平面外TEC,标称单层多晶外延2DWSe2的热膨胀系数确定为(3.5±0.9)×10-6K-1和(5.7±2)×10-5K-1,分别,晶胞体积TEC为(3.6±0.2)×10-5K-1,与历史上确定的块状晶体值非常吻合。
    Current reports of thermal expansion coefficients (TEC) of two-dimensional (2D) materials show large discrepancies that span orders of magnitude. Determining the TEC of any 2D material remains difficult due to approaches involving indirect measurement of samples that are atomically thin and optically transparent. We demonstrate a methodology to address this discrepancy and directly measure TEC of nominally monolayer epitaxial WSe2 using four-dimensional scanning transmission electron microscopy (4D-STEM). Experimentally, WSe2 from metal-organic chemical vapor deposition (MOCVD) was heated through a temperature range of 18-564 °C using a barrel-style heating sample holder to observe temperature-induced structural changes without additional alterations or destruction of the sample. By combining 4D-STEM measurements with quantitative structural analysis, the thermal expansion coefficient of nominally monolayer polycrystalline epitaxial 2D WSe2 was determined to be (3.5 ± 0.9) × 10-6 K-1 and (5.7 ± 2) × 10-5 K-1 for the in- and out-of-plane TEC, respectively, and (3.6 ± 0.2) × 10-5 K-1 for the unit cell volume TEC, in good agreement with historically determined values for bulk crystals.
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  • 文章类型: Journal Article
    生长表面的粗糙形态导致铟成分的不均匀分布,有意或无意掺杂杂质,从而影响GaN基光电和垂直功率电子器件的性能。我们观察了通过MOCVD同质外延生长的无意掺杂GaN的形貌,并确定了粗糙表面与衬底的斜切角度和方向之间的关系。研究了Ehrlich-Schwoebel屏障作用下的生长动力学,发现具有较大斜切角的样品或在高温下生长的样品中的不对称步进运动是步进聚束的原因。对于具有宽梯田或偏离[11'00]m方向的台阶,弯曲的台阶被认为是由表面自由能最小化引起的。
    The rough morphology at the growth surface results in the non-uniform distribution of indium composition, intentionally or unintentionally doped impurity, and thus impacts the performance of GaN-based optoelectronic and vertical power electronic devices. We observed the morphologies of unintentionally doped GaN homo-epitaxially grown via MOCVD and identified the relations between rough surfaces and the miscut angle and direction of the substrate. The growth kinetics under the effect of the Ehrlich-Schwoebel barrier were studied, and it was found that asymmetric step motions in samples with a large miscut angle or those grown at high temperature were the causes of step-bunching. Meandering steps were believed to be caused by surface free energy minimization for steps with wide terraces or deviating from the [11¯00] m-direction.
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  • 文章类型: Journal Article
    基于激光感应横向电压(LITV)效应的光热探测器因其快速而宽的光谱响应而引起了人们的极大兴趣。在这项研究中,我们使用我们设计的金属有机化学气相沉积系统在12°倾斜的单晶LaAlO3(LAO)(100)衬底上制备了La掺杂的SrTiO3(STO)外延薄膜。在248nm激光的照射下,观察到LaxSr1-xTiO3薄膜的LITV信号,并显示出对La掺杂水平的依赖性,这可以用光吸收系数的变化来解释,热导率,和光学穿透深度。在1.0mJmm-2的激光功率密度下,观察到优化的LITV信号的峰值电压为23.25V,衰减时间为106ns。LaxSr1-xTiO3的高峰值电压和快速响应时间在光热检测领域显示出巨大的潜力。
    Light and thermal detectors based on the laser-induced transverse voltage (LITV) effect have garnered significant interest for their rapid and broad spectral response. In this study, we prepared the La-doped SrTiO3(STO) epitaxial thin films on the 12° inclined single crystal LaAlO3(LAO) (100) substrates using our home-designed metal-organic chemical vapor deposition system. Under the illumination of a 248 nm laser, the LITV signals of LaxSr1-xTiO3films were observed and showed dependence on the La doping level, which can be explained by the changes in the light absorption coefficient, thermal conductivity, and optical penetration depth. The optimized LITV signal was observed with a peak voltage of 23.25 V and a decay time of 106 ns under the laser power density of 1.0 mJ mm-2. The high peak voltage and fast response time of LaxSr1-xTiO3show great potential in the field of light and thermal detection.
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  • 文章类型: Journal Article
    尽管AlGaN基紫外-B发光二极管(UV-BLED)在光疗等各种应用中具有相当大的潜力,UV固化,植物生长,和分析技术,由于发光效率低,它们的发展仍在进行中。在这项研究中,我们引入了一种新颖的外延生长机制,以有效地控制AlGaN多阱(MWs)上AlGaN纳米棒结构的高度和厚度使用水平反应器基金属有机化学气相沉积(MOCVD)。通过调节H2载气流量,我们可以控制生长边界层的厚度,成功地将AlGaN阱和p-AlGaN层与衬底分离。阴极发光(CL)测量证实了核-壳AlGaN量子阱作为高度稳定的非极化结构的稳定性,在各种注入电流下,波长峰值几乎保持不变。此外,透射电子显微镜(TEM)提供了明确的分化证据,突出了275nmAlGaN核和295nmAlGaN壳结构的不同形成。开发的AlGaNMW结构,以这些矫正特征为特征,与传统的核-壳AlGaN结构相比,不仅显示出显着改善的电致发光(EL)峰强度,而且还显示出低得多的泄漏电流。新提出的生长机制和先进的非极化核-壳AlGaN结构有望成为显著提高下一代高效UVLED效率的优秀替代品。
    Despite the considerable potential of AlGaN-based ultraviolet-B light-emitting diodes (UV-B LEDs) in various applications such as phototherapy, UV curing, plant growth, and analytical technology, their development is still ongoing due to low luminescence efficiency. In this study, we introduced a novel epitaxial growth mechanism to effectively control the height and thickness of AlGaN multiple wells (MWs) on AlGaN nanorod structures using horizontal reactor-based metal-organic chemical vapor deposition (MOCVD). By adjusting the H2 carrier gas flow rate, we could control the growth boundary layer\'s thickness, successfully separating the AlGaN well and p-AlGaN layer from the substrate. Cathodoluminescence (CL) measurements confirmed the stability of the core-shell AlGaN quantum wells as a highly stable nonpolarized structure, with the wavelength peak remaining almost unchanged under various injection currents. Furthermore, transmission electron microscopy (TEM) provided clear evidence of differentiation, highlighting the distinct formation of the 275 nm AlGaN core and the 295 nm AlGaN shell structure. The developed AlGaN MW structure, characterized by these rectification features, not only demonstrated a significantly improved electroluminescence (EL) peak intensity but also exhibited a much lower leakage current compared to the conventional core-shell AlGaN structure. The newly proposed growth mechanism and advanced nonpolarized core-shell AlGaN structure are expected to serve as excellent alternatives for substantially enhancing the efficiency of the next generation of high-efficiency UV LEDs.
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  • 文章类型: Journal Article
    在这项工作中,我们研究了MOCVD条件以合成具有六方P63cmh-LuMnO3相作为潜在的低带隙铁电材料的薄膜。研究的主要参数是有机金属原料的比例,衬底温度,和退火效应。研究中使用了两种不同的基材:熔融石英(SiO2)玻璃和镀铂硅(Pt\\Ti\\SiO2\\Si(100))。为了研究已开发阶段的热力学稳定性和质量,详细的晶体结构分析,微观结构,形态学,用X射线衍射仪测量薄膜的粗糙度,扫描电子显微镜(SEM),能量色散光谱法(EDS),拉曼光谱,和压电式力显微镜(PFM)。发现膜中在0.93<|Lu|/|Mn|<1.33范围内的摩尔组成适合于获得单相h-LuMnO3。通过在700°C下沉积获得最好的薄膜,然后在800°C下进行长达12小时的长时间热处理。这些薄膜表现出高度结晶的六方单相,具有相对较窄的直接带隙,大约1.5eV,这在h-LuMnO3系统的预期值内。
    In this work, we investigated the MOCVD conditions to synthesize thin films with the hexagonal P63cm h-LuMnO3 phase as a potential low-band gap ferroelectric material. The main parameters investigated were the ratio of organometallic starting materials, substrate temperature, and annealing effect. Two different substrates were used in the study: fused silica (SiO2) glass and platinized silicon (Pt\\Ti\\SiO2\\Si(100)). In order to investigate the thermodynamic stability and quality of the developed phases, a detailed analysis of the crystal structure, microstructure, morphology, and roughness of the films was performed by X-ray diffractometer, scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), Raman spectroscopy, and piezoelectric force microscopy (PFM). Molar compositions in the film within 0.93 < |Lu|/|Mn| < 1.33 were found to be suitable for obtaining a single-phase h-LuMnO3. The best films were obtained by depositions at 700 °C, followed by thermal treatments at 800 °C for long periods of up to 12 h. These films exhibited a highly crystalline hexagonal single phase with a relatively narrow direct band gap, around 1.5 eV, which is within the expected values for the h-LuMnO3 system.
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  • 文章类型: Journal Article
    使用二维(2D)材料生产独立式膜通常涉及诸如范德华(vdW)外延,准vdW外延,和远程外延。然而,当尝试通过使用这些2D材料辅助生长技术来制造独立式GaN时,出现了挑战。问题在于确保稳定,金属有机化学气相沉积(MOCVD)下的高温生长条件可能由于衬底的GaN分解而对2D材料造成损害。即使使用这种方法成功生长了GaN,对2D材料的损坏导致与基板的直接接合,使生长的GaN的剥离几乎不可能。本研究介绍了一种在2D材料/GaN模板上生长和剥离GaN的方法。首先,将石墨烯和六方氮化硼(h-BN)转移到GaN模板上,在MOCVD中的高温和各种气体下创造稳定的条件。GaN在750和900°C下以两步法生长,确保在二维材料保持完整的情况下剥离。本质上,虽然仅使用MOCVD在2D材料/GaN上生长GaN具有挑战性,这项研究表明,在有效保护二维材料的情况下,生长的GaN可以承受高温,并且仍然会剥落。此外,这些结果支持vdW外延和远程外延原理不仅可以使用特定设备,而且可以普遍应用。
    The production of freestanding membranes using two-dimensional (2D) materials often involves techniques such as van der Waals (vdW) epitaxy, quasi-vdW epitaxy, and remote epitaxy. However, a challenge arises when attempting to manufacture freestanding GaN by using these 2D-material-assisted growth techniques. The issue lies in securing stability, as high-temperature growth conditions under metal-organic chemical vapor deposition (MOCVD) can cause damage to the 2D materials due to GaN decomposition of the substrate. Even when GaN is successfully grown using this method, damage to the 2D material leads to direct bonding with the substrate, making the exfoliation of the grown GaN nearly impossible. This study introduces an approach for GaN growth and exfoliation on 2D material/GaN templates. First, graphene and hexagonal boron nitride (h-BN) were transferred onto the GaN template, creating stable conditions under high temperatures and various gases in MOCVD. GaN was grown in a two-step process at 750 and 900 °C, ensuring exfoliation in cases where the 2D materials remained intact. Essentially, while it is challenging to grow GaN on 2D material/GaN using only MOCVD, this study demonstrates that with effective protection of the 2D material, the grown GaN can endure high temperatures and still be exfoliated. Furthermore, these results support that vdW epitaxy and remote epitaxy principle are not only possible with specific equipment but also applicable generally.
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  • 文章类型: Journal Article
    获得均匀且可再现的晶片级过渡金属二硫属化物(TMDC)薄膜对于现代电子学至关重要。金属有机化学气相沉积(MOCVD)为可扩展的生产和大面积集成提供了一种有前途的方法。然而,在MOCVD合成过程中,由于有机硫前体热解导致的外来碳掺入是一个持续的问题,无意的碳掺入的作用仍然难以捉摸。这里,我们报道了二硫化钼(MoS2)薄膜的大规模合成,伴随着无定形碳层的形成。使用拉曼,光致发光(PL)光谱,和透射电子显微镜(TEM),我们确认多晶MoS2如何与外来无定形碳层结合。此外,通过使用碳掺入的MoS2薄膜制造场效应晶体管(FET),我们发现传统的n型MoS2可以转化为p型半导体由于碳的掺入,在TMDC材料中很少发生。这种意想不到的行为扩展了我们对TMDC特性的理解,并为探索新颖的设备应用开辟了新的途径。
    Acquiring homogeneous and reproducible wafer-scale transition metal dichalcogenide (TMDC) films is crucial for modern electronics. Metal-organic chemical vapor deposition (MOCVD) offers a promising approach for scalable production and large-area integration. However, during MOCVD synthesis, extraneous carbon incorporation due to organosulfur precursor pyrolysis is a persistent concern, and the role of unintentional carbon incorporation remains elusive. Here, we report the large-scale synthesis of molybdenum disulfide (MoS2) thin films, accompanied by the formation of amorphous carbon layers. Using Raman, photoluminescence (PL) spectroscopy, and transmission electron microscopy (TEM), we confirm how polycrystalline MoS2 combines with extraneous amorphous carbon layers. Furthermore, by fabricating field-effect transistors (FETs) using the carbon-incorporated MoS2 films, we find that traditional n-type MoS2 can transform into p-type semiconductors owing to the incorporation of carbon, a rare occurrence among TMDC materials. This unexpected behavior expands our understanding of TMDC properties and opens up new avenues for exploring novel device applications.
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  • 文章类型: Journal Article
    正确调整拓扑绝缘体中的费米能级位置对于调整其自旋极化电子传输并提高基于它们的任何功能器件的效率至关重要。这里,我们报告了完整的原位金属有机化学气相沉积(MOCVD),并在大面积(4“)Si(111)衬底上研究了高度结晶的Bi2Te3/Sb2Te3拓扑绝缘体异质结构。底部的Sb2Te3层是理想的种子层,用于在顶部生长高度结晶的Bi2Te3,也引起费米能级的显着变化,使其非常接近狄拉克点,通过角度分辨光发射光谱法可视化。为了利用这种理想的拓扑保护表面状态,我们制造了简单的自旋电荷转换器Si(111)/Sb2Te3/Bi2Te3/Au/Co/Au,并通过自旋泵浦铁磁共振来探测自旋电荷转换(SCC)。在室温下测量大的SCC,并在逆Edelstein效应中解释,从而导致λIEEE~0.44nm的转换效率。我们的结果表明,当使用完全原位MOCVD工艺在Sb2Te3顶部生长时,Bi2Te3的表面费米能级得到了成功的调整,鉴于其未来的技术转让,这是非常有趣的。
    Properly tuning the Fermi level position in topological insulators is of vital importance to tailor their spin-polarized electronic transport and to improve the efficiency of any functional device based on them. Here, we report the full in situ metal organic chemical vapor deposition (MOCVD) and study of a highly crystalline Bi2Te3/Sb2Te3 topological insulator heterostructure on top of large area (4″) Si(111) substrates. The bottom Sb2Te3 layer serves as an ideal seed layer for the growth of highly crystalline Bi2Te3 on top, also inducing a remarkable shift of the Fermi level to place it very close to the Dirac point, as visualized by angle-resolved photoemission spectroscopy. To exploit such ideal topologically protected surface states, we fabricate the simple spin-charge converter Si(111)/Sb2Te3/Bi2Te3/Au/Co/Au and probe the spin-charge conversion (SCC) by spin pumping ferromagnetic resonance. A large SCC is measured at room temperature and is interpreted within the inverse Edelstein effect, thus resulting in a conversion efficiency of λIEEE ∼ 0.44 nm. Our results demonstrate the successful tuning of the surface Fermi level of Bi2Te3 when grown on top of Sb2Te3 with a full in situ MOCVD process, which is highly interesting in view of its future technology transfer.
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  • 文章类型: Journal Article
    金属-有机CVD方法(MOCVD)允许将电子质量的超薄2D过渡金属二硫属化合物(TMD)膜沉积到晶片级基板上。在这项工作中,温度对结构的影响,化学状态,研究了MOCVDMoS2薄膜的电子质量。结果表明,在650°C至950°C范围内的温度升高导致非单调平均微晶尺寸变化。原子力显微镜(AFM),透射电子显微镜(TEM),和拉曼光谱研究表明,在该范围内,薄膜晶体结构随着温度的升高而改善。同时,X射线光电子能谱(XPS)方法可以揭示非化学计量相分数的增加,对应于从大约0.9at增加的硫空位(VS)浓度。%至3.6at。%.晶畴尺寸和VS浓度之间建立的依赖性表明这些空位主要在晶界处形成。结果表明,薄膜电阻率从4kΩ·cm增加到39kΩ·cm的主要原因是增加的Vs浓度和在晶粒边界处散射的电荷载流子增强。
    Metal-Organic CVD method (MOCVD) allows for deposition of ultrathin 2D transition metal dichalcogenides (TMD) films of electronic quality onto wafer-scale substrates. In this work, the effect of temperature on structure, chemical states, and electronic qualities of the MOCVD MoS2 films were investigated. The results demonstrate that the temperature increase in the range of 650 °C to 950 °C results in non-monotonic average crystallite size variation. Atomic force microscopy (AFM), transmission electron microscopy (TEM), and Raman spectroscopy investigation has established the film crystal structure improvement with temperature increase in this range. At the same time, X-Ray photoelectron spectroscopy (XPS) method allowed to reveal non-stoichiometric phase fraction increase, corresponding to increased sulfur vacancies (VS) concentration from approximately 0.9 at.% to 3.6 at.%. Established dependency between the crystallite domains size and VS concentration suggests that these vacancies are form predominantly at the grain boundaries. The results suggest that an increased Vs concentration and enhanced charge carriers scattering at the grains\' boundaries should be the primary reasons of films\' resistivity increase from 4 kΩ·cm to 39 kΩ·cm.
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  • 文章类型: Journal Article
    在半导体金属氧化物中,这是一类重要的传感材料,二氧化钛(TiO2)薄膜因其在恶劣环境中的高化学和机械稳定性而被广泛用作传感器。无毒性,生态相容性,和光催化性能。基于TiO2的化学需氧量(COD)传感器利用TiO2的光催化性能诱导有机化合物氧化为CO2。在这项工作中,我们讨论了通过低压金属有机化学气相沉积(MOCVD)在金属AISI316网格上生长的纳米结构TiO2薄膜。要增加表面感应面积,已经开发了不同的无机酸基化学蚀刻方案,确定适当的基板粗糙度的最佳实验条件。通过扫描电子显微镜(SEM)研究了化学蚀刻的原始网格和MOCVD涂层的网格,X射线衍射(XRD)能量色散X射线(EDX)微区分析,和X射线光电子能谱(XPS)。我们证明了在55°C下通过HCl/H2SO4蚀刻提供了最合适的表面形态。为了研究开发的高表面积TiO2薄膜作为COD传感器的行为,基于ISO10678:2010对功能模型污染物的光催化降解进行了测试,显示出最佳性能的酸蚀刻网涂有多晶TiO2的活性增加了60%,每小时每平方米降低66μmolMB。
    Among semiconductor metal oxides, that are an important class of sensing materials, titanium dioxide (TiO2) thin films are widely employed as sensors because of their high chemical and mechanical stability in harsh environments, non-toxicity, eco-compatibility, and photocatalytic properties. TiO2-based chemical oxygen demand (COD) sensors exploit the photocatalytic properties of TiO2 in inducing the oxidation of organic compounds to CO2. In this work, we discuss nanostructured TiO2 thin films grown via low-pressure metal organic chemical vapor deposition (MOCVD) on metallic AISI 316 mesh. To increase the surface sensing area, different inorganic acid-based chemical etching protocols have been developed, determining the optimal experimental conditions for adequate substrate roughness. Both chemically etched pristine meshes and the MOCVD-coated ones have been studied by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive X-ray (EDX) microanalysis, and X-ray photoelectron spectroscopy (XPS). We demonstrate that etching by HCl/H2SO4 at 55 °C provides the most suitable surface morphology. To investigate the behavior of the developed high surface area TiO2 thin films as COD sensors, photocatalytic degradation of functional model pollutants based on ISO 10678:2010 has been tested, showing for the best performing acid-etched mesh coated with polycrystalline TiO2 an increase of 60% in activity, and degrading 66 µmol of MB per square meter per hour.
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