Journal of Crystal Growth最新文献_第3页

The effect of annealing process and seed layer control on the crystallization characteristics and optoelectronic properties of β-Ga2O3 films fabricated by ALD 退火工艺和种层控制对ALD法制备β-Ga2O3薄膜结晶特性和光电性能的影响

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-22 DOI: 10.1016/j.jcrysgro.2025.128427

Ziyu Yang , Zihua Ma , Jianghai He , Chufeng Hou , Qi Liu , Shihao Xia , Kongli Ran , Qiang Wang , Yuefei Zhang , Fei Chen

This study utilizes Atomic Layer Deposition (ALD) technology, employing Trimethylgallium (TMG) and Ozone (O₃) as precursors to fabricate Ga₂O₃ thin films. To enhance the crystallinity of the films, the effects of seed layers and annealing processes on the Ga₂O₃ thin films were investigated. High-quality β-Ga₂O₃ thin films were successfully grown on sapphire substrates. Experimental results indicate that directly depositing Ga₂O₃ on sapphire substrates did not yield satisfactory β-Ga₂O₃ films. To improve the crystallinity, a Ga₂O₃ seed layer was prepared on the sapphire substrate, and high-temperature annealing was employed to promote crystallization of the Ga₂O₃ seed layer, providing artificial nucleation sites for subsequent thin film deposition. The influence of the annealing temperature and seed layer thickness on the quality of the secondary Ga₂O₃ films was also studied. It was found that a seed layer with a thickness of 16.5 nm, followed by annealing at 1000 °C, resulted in Ga₂O₃ films with optimal crystallinity. After the deposition of the thin film, post-deposition annealing was performed to investigate the effects of annealing temperature on the structural and optical properties of the Ga₂O₃ films. The results show that with increasing annealing temperature, the optical band gap of the films enlarged, the proportion of high-valence gallium increased, and the crystallinity improved. Thus, it can be concluded that optimized annealing conditions lead to higher quality Ga₂O₃ films. The optical band gap of the Ga₂O₃ film treated with 30 min of annealing reached its maximum value of approximately 5.24 eV. Under a 5 V bias, the photocurrent was 1.9 × 10⁻⁴ A, the dark current was 4.9 × 10⁻⁷ A, and the photo-dark ratio was 388, which showed significant improvement compared to the as-deposited sample. At a 10 V bias, the device’s response time (τ_x) was 0.3 s, and its decay time (τd) was 0.28 s.

本研究采用原子层沉积（ALD）技术，以三甲基镓（TMG）和臭氧（O3）为前驱体制备Ga2O3薄膜。为了提高薄膜的结晶度，研究了种子层和退火工艺对薄膜结晶度的影响。在蓝宝石衬底上成功生长出高质量的β-Ga2O3薄膜。实验结果表明，在蓝宝石衬底上直接沉积Ga2O3不能得到满意的β-Ga2O3薄膜。为了提高结晶度，在蓝宝石衬底上制备了Ga2O3种子层，并采用高温退火方法促进Ga2O3种子层的结晶，为后续的薄膜沉积提供人工成核位点。研究了退火温度和种层厚度对二次Ga2O3薄膜质量的影响。结果表明，采用16.5 nm的种子层，在1000℃下退火，可以得到结晶度最佳的Ga2O3薄膜。薄膜沉积后，进行沉积后退火，研究退火温度对薄膜结构和光学性能的影响。结果表明：随着退火温度的升高，薄膜的光学带隙增大，高价镓的比例增加，结晶度提高；因此，优化的退火条件可以获得更高质量的Ga2O3薄膜。经30 min退火处理的Ga2O3薄膜的光学带隙达到最大值，约为5.24 eV。在5 V偏置下，光电流为1.9 × 10−4 a，暗电流为4.9 × 10−7 a，光暗比为388，与沉积样品相比有明显改善。在10v偏置下，器件的响应时间τx为0.3 s，衰减时间τd为0.28 s。

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引用次数: 0

Epitaxial columnar growth of strain-free antiferromagnetic Weyl semimetal Mn3Sn on wurtzite c-plane GaN/Al2O3(0001) 无应变反铁磁性Weyl半金属Mn3Sn在纤锌矿c-平面GaN/Al2O3上的外延柱状生长（0001）

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-21 DOI: 10.1016/j.jcrysgro.2025.128426

Hannah Hall, Sunil Timilsina, Sneha Upadhyay, Tyler Erickson, Cherie D’Mello, David C. Ingram, Arthur R. Smith

Weyl semimetal thin films with excellent crystalline quality are of great interest for antiferromagnetic spintronics. Mn

_{3}

Sn is one Weyl semimetal with great properties and promise for exciting science and applications. It has proven very challenging, however, to grow Mn

_{3}

Sn thin films with smooth surfaces, negligible strain, and excellent crystallinity. In this work, we discuss the successful preparation of epitaxial Mn

_{3}

Sn (0001)-oriented thin films via molecular beam epitaxial growth on

c

-plane wurtzite GaN which was grown by MBE on Al

_{2}

O

_{3}

(0001). We present the reflection high energy electron diffraction analysis along with x-ray diffraction in order to demonstrate the crystalline quality of the film, and we give atomic models to explain the epitaxial orientation relationships between the crystal lattices of the substrate, GaN layer, and Mn

_{3}

Sn layer. Importantly, we discuss the film lattice parameters as compared to expected values, demonstrating negligible strain both in-plane and out-of-plane. Atomic force microscopy reveals an epitaxial columnar growth mode characterized by flat-top-mesa islands, while scanning tunneling microscopy shows the atomically smooth surfaces of the mesa-top structures. Finally, Rutherford backscattering informs the stoichiometry of the film as well as the layer thicknesses.

具有优异晶体质量的Weyl半金属薄膜是反铁磁自旋电子学研究的热点。Mn3Sn是一种Weyl半金属，具有良好的性能和令人兴奋的科学和应用前景。然而，制备表面光滑、应变可忽略不计、结晶度优异的Mn3Sn薄膜已被证明是非常具有挑战性的。在这项工作中，我们讨论了在Al2O3（0001）上MBE生长的c面纤锌矿GaN上通过分子束外延生长成功制备外延Mn3Sn（0001）取向薄膜。为了证明薄膜的晶体质量，我们提出了反射高能电子衍射分析和x射线衍射分析，并给出了原子模型来解释衬底、GaN层和Mn3Sn层晶格之间的外延取向关系。重要的是，我们讨论了薄膜晶格参数与期望值的比较，证明了面内和面外的应变可以忽略不计。原子力显微镜观察到外延柱状生长模式为平顶台地岛，而扫描隧道显微镜观察到台地结构的原子光滑表面。最后，卢瑟福后向散射告知薄膜的化学计量以及层厚度。

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引用次数: 0

Role of directly grown multiwalled carbon nanotube as intermediate layers for GaN on c-plane sapphire 直接生长的多壁碳纳米管作为c-平面蓝宝石上氮化镓中间层的作用

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-20 DOI: 10.1016/j.jcrysgro.2025.128425

Gulnaz Gahramanova , Rasim Jabbarov , Oliver Rettig , Imamaddin Amiraslanov , Irada Mammadova , Ferdinand Scholz

This work investigates the role of directly synthesized multiwalled carbon nanotube (MWCNT) as an intermediate layer for the growth of gallium nitride (GaN) on c-plane sapphire. MWCNTs forests were grown on c-plane sapphire using aerosol-assisted chemical vapor deposition (A-CVD), and the structural and crystalline characteristics of these MWCNT templates were confirmed by Raman spectroscopy and powder X-ray diffraction (PXRD). Subsequently, GaN layers were grown via Metal-Organic Vapor Phase Epitaxy (MOVPE) on both bare c-sapphire and MWCNT/c-sapphire templates.

Structural and optical analyses (SEM, HRXRD, and low-temperature PL) reveal that GaN grown on MWCNTs is polycrystalline and exhibits reduced crystalline quality compared to GaN/sapphire, confirming a fundamentally different growth mode. Despite this, the hybrid GaN/MWCNT architecture exhibits significantly enhanced electrical conductivity. At 3 MHz, the AC conductivity of GaN/MWCNT/sapphire reaches ∼7 × 10³ µS, compared to ∼4.5 × 10² µS for GaN/sapphire. Under DC bias, the current at 20 V increases from ∼10⁻⁸ A (GaN/sapphire) to the milliamp range (10⁻³ A) for GaN/MWCNT/sapphire. These results demonstrate that MWCNT forests do not serve as a replacement for high-quality epitaxial GaN but instead enable a non-conventional GaN growth platform—porous, conductive, and weakly bonded to the substrate—opening pathways for GaN architectures relevant to sensing, catalytic interfaces, UV detection, and future transferable/lift-off GaN films.

本文研究了直接合成的多壁碳纳米管（MWCNT）作为c面蓝宝石上氮化镓（GaN）生长的中间层的作用。采用气溶胶辅助化学气相沉积（A-CVD）技术在c平面蓝宝石上制备了MWCNT模板，并通过拉曼光谱和粉末x射线衍射（PXRD）对模板的结构和晶体特征进行了验证。随后，通过金属有机气相外延（MOVPE）在裸露的c-蓝宝石和MWCNT/c-蓝宝石模板上生长GaN层。结构和光学分析（SEM， HRXRD和低温PL）表明，生长在MWCNTs上的GaN是多晶的，与GaN/蓝宝石相比，其晶体质量降低，证实了一种根本不同的生长方式。尽管如此，GaN/MWCNT混合结构表现出显著增强的导电性。在3 MHz时，GaN/MWCNT/蓝宝石的交流电导率达到~ 7 × 103µS，而GaN/蓝宝石的交流电导率为~ 4.5 × 102µS。在直流偏置下，20 V电流从GaN/蓝宝石的10−8 A增加到GaN/MWCNT/蓝宝石的10−3 A毫安范围。这些结果表明，MWCNT森林不能作为高质量外延GaN的替代品，而是提供了一个非传统的GaN生长平台——多孔、导电、与衬底弱键合——用于GaN结构的开放途径，这些途径与传感、催化界面、紫外线检测和未来可转移/可提升的GaN薄膜有关。

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引用次数: 0

Effect of Fe in structural and electrical properties in GaSb grown by TVDS technique Fe对TVDS法生长的GaSb结构和电性能的影响

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-19 DOI: 10.1016/j.jcrysgro.2025.128423

Gayatree Tripathy, Diana Pradhan, Sushanta Kumar Kamilla

Gallium Antimonide (GaSb) proves to be a suitable substrate material in mid-infrared optoelectronic, spintronic and high speed electronic devices due to its lattice compatibility with the other compound semiconductors. Bandgap tuning, magnetic behaviour as well as tailoring the defects that directly impact the carrier mobility and conductivity can be done with doping transition metals. The present work involves growth of Fe doped GaSb by customized in-house horizontal “Thermo-Vertical Directional Solidification” (TVDS) apparatus. This compound semiconductor processing apparatus facilitates both the synthesis of the melt and the crystal growth process under precise thermal control of 1⁰C/min accuracy. Phase formation was confirmed by room temperature X-ray Diffraction (XRD) pattern which shows little lattice expansion with Fe doping at Ga site. Morphological study using Scanning Electron Microscopy (SEM) images reported average etch pit density of 2.1 × 10⁵ cm⁻² on the surface. The crystallite size from XRD and sub-grain size from SEM are nearly similar in dimension. Hall effect measurement results showed increase in mobility and carrier concentration while the resistivity value decreases. Similar changes in electrical parameters were further confirmed by the Dielectric Spectroscopy that give insights to different kinds of polarization mechanisms due to dopant-induced additional p-type carriers.

锑化镓（GaSb）由于其与其他化合物半导体的晶格相容性，被证明是中红外光电、自旋电子和高速电子器件中合适的衬底材料。带隙调谐，磁性行为以及剪裁直接影响载流子迁移率和电导率的缺陷可以通过掺杂过渡金属来完成。目前的工作是利用自制的卧式“热垂直定向凝固”（TVDS）装置生长Fe掺杂的GaSb。这种化合物半导体加工装置有助于在1⁰C/min精度的精确热控制下合成熔体和晶体生长过程。通过室温x射线衍射（XRD）证实，在Ga位点掺杂Fe后，相的晶格扩展很小。利用扫描电子显微镜（SEM）图像进行形态学研究，发现表面的平均蚀刻坑密度为2.1 × 105 cm−2。XRD分析得到的晶粒尺寸与SEM分析得到的亚晶粒尺寸基本一致。霍尔效应测量结果表明，电导率和载流子浓度增加，而电阻率值降低。电介质光谱进一步证实了类似的电参数变化，这为掺杂剂诱导的额外p型载流子的不同极化机制提供了见解。

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引用次数: 0

Structural and optical characterization of highly homogeneous lithium niobate tantalate single-crystal solid solutions 高均相铌酸锂钽酸盐单晶固溶体的结构和光学特性

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-19 DOI: 10.1016/j.jcrysgro.2025.128422

Umar Bashir , Saud Bin Anooz , Martin Schmidbauer , Lukas M. Eng , Matthias Bickermann , Steffen Ganschow

The compositional homogeneity of nominally LiNb_1−xTa_xO₃ (x = 0.45) single crystals is studied using micro-X-ray fluorescence and high-resolution X-ray diffraction. Highly homogeneous regions are reported with less than 1 % Ta variation over areas as large as 4 × 4 mm² in z-cut specimens. To our knowledge, this represents the most detailed study of homogeneity in lithium niobate tantalate (LNT) solid solutions to date, establishing a quantitative benchmark for future studies. Spectroscopic ellipsometry shows a decreasing refractive index and blue-shift in optical absorption with increasing Ta content, while the dielectric response remains structurally consistent. These investigations establish a quantitative benchmark for selecting compositionally homogeneous LNT crystals suitable for applications such as second-harmonic generation, Raman spectroscopy, piezoresponse force microscopy, and domain wall conductivity.

利用微x射线荧光和高分辨率x射线衍射研究了名义LiNb1−xTaxO3 （x = 0.45）单晶的成分均匀性。据报道，在z形切割的样品中，高度均匀的区域在4 × 4 mm2的面积上Ta变化小于1%。据我们所知，这是迄今为止对铌酸锂钽酸盐（LNT）固溶体均匀性最详细的研究，为未来的研究建立了定量基准。椭偏光谱分析表明，随着Ta含量的增加，材料的折射率和光吸收蓝移减小，而介电响应在结构上保持一致。这些研究为选择适合二次谐波产生、拉曼光谱、压电响应力显微镜和畴壁电导率等应用的组成均匀的LNT晶体建立了定量基准。

引用次数: 0

A reitveld refinement in WPPF analysis for crystallographic behavior study of nanocrystal anatase TiO2 synthesized by ultrasonic-assisted sol–gel method and its photocatalytic activity 超声辅助溶胶-凝胶法合成纳米锐钛矿TiO2晶体行为及其光催化活性的WPPF分析reitveld改进

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-19 DOI: 10.1016/j.jcrysgro.2025.128424

Mirza Nusrat Sweety , Shariful Islam

A novel crystallographic study has been conducted on a simplified synthesis of anatase TiO₂ nanocrystals derived from a sol–gel process, utilizing TTIP as the precursor at a pH of 2, assisted by ultrasonic means. The Reitveld refinement analysis performed using whole powder pattern fitting (WPPF) confirmed the complete formation of the TiO₂ anatase, verifying its tetragonal structure [α = β = γ = 90.0°; a = b = 3.7877 Å, c = 9.5090 Å]. Peak profiling indicated that the highest preferred orientation occurred along the (1 0 1) plane at 2θ = 25.357°, with a d-spacing of 0.35096 nm and an intensity of 6913 cps. The computed unit cell volume was 136.424 Å³, and additional measurements indicated a dislocation density of 0.00615 nm⁻², lattice strain of 0.58 %, microstrain of 0.00815, crystallinity of 63.279 %, and a crystallinity index of 1.37, all suggesting lattice expansion and a significant capacity for defect tolerance, crucial for applications in electronics and catalysis. According to the Scherrer equation, the average crystallite size was determined to be 12.75 nm; using the Monshi-Scherrer model, it was calculated at 12.17 nm; the Williamson-Hall model yielded 27.57 nm; the LSLM of the Scherrer equation resulted in 13.57 nm; the Size-Strain plot model estimated it to be 6.48 nm; and the Halder-Wagner model provided a size of 7.20 nm. Energy dispersive spectroscopy (EDS) analysis confirmed the elemental purity, showing 34.89 % Ti and 65.11 % O, while scanning electron microscopy (SEM) revealed a uniform distribution of non-clumped nanoparticles. The UV study show cased that a blue-shifted intense absorption peak of T_A (3.31 eV) compared to the bulk material reported in the literature (3.2 eV). The maximum photo-degradation efficiency under the dosage 30 mg, initial dye concentration 10 ppm, degradation time 60 min were found to be 98.8 %. By integrating a straightforward synthesis approach with comprehensive refinement, this detailed analysis of structural, optical and surface morphology along with photo-catalytic activity provides a reliable foundation for the production of pure anatase phase TiO₂ nanocrystals.

以TTIP为前驱体，在pH = 2的条件下，超声辅助下，对溶胶-凝胶法制备锐钛矿型TiO2纳米晶进行了新的晶体学研究。采用全粉末模式拟合（WPPF）进行Reitveld细化分析，证实了TiO2锐钛矿的完全形成，验证了其四方结构[α = β = γ = 90.0°；A = b = 3.7877 Å， c = 9.5090 Å]。峰谱分析表明，在2θ = 25.357°的（1 0 1）平面上，光强为6913 cps， d-间距为0.35096 nm。计算得到的晶胞体积为136.424 Å3，额外的测量表明位错密度为0.00615 nm - 2，晶格应变为0.58%，微应变为0.00815，结晶度为63.279 %，结晶度指数为1.37，所有这些都表明晶格膨胀和显著的缺陷容忍能力，这对电子和催化的应用至关重要。根据Scherrer方程，确定晶粒的平均尺寸为12.75 nm；采用Monshi-Scherrer模型，在12.17 nm处计算；Williamson-Hall模型的波长为27.57 nm；Scherrer方程的LSLM为13.57 nm；尺寸-应变图模型估计为6.48 nm；Halder-Wagner模型提供的尺寸为7.20 nm。能谱分析（EDS）证实了元素纯度，Ti为34.89%，O为65.11%，扫描电镜（SEM）显示纳米颗粒均匀分布，无团块。紫外光研究表明，与文献报道的大块材料（3.2 eV）相比，TA的蓝移强吸收峰（3.31 eV）。在投加量为30 mg、初始染料浓度为10 ppm、降解时间为60 min的条件下，最大光降解效率为98.8%。通过将简单的合成方法与全面的细化相结合，对结构、光学和表面形貌以及光催化活性进行了详细的分析，为生产纯锐钛矿相TiO2纳米晶体提供了可靠的基础。

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引用次数: 0

Quasi-discrete modeling of step-flow dynamics: capturing bunching and debunching in sic solution growth 阶梯流动动力学的准离散建模：捕获碳化硅溶液生长中的聚束和脱束

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-17 DOI: 10.1016/j.jcrysgro.2025.128420

C.W. Lan

Step-flow dynamics during SiC solution growth critically shape surface morphology and defect formation, yet conventional models often average step densities or encounter front-tracking singularities, missing transient bunching and debunching. We introduce a quasi-discrete 2D/3D model that couples advection–diffusion transport with Gaussian-regularized Robin boundary conditions, representing macrosteps as localized, integral-matched sinks. Each macrostep is resolved by a few Gaussian-weighted nodes while solute transport is computed on a fine finite-element mesh, ensuring stability and mass conservation. Simulations reveal that parallel flow drives strong bunching, producing wide terraces with amplified supersaturation; bunched steps advance more slowly due to solute depletion, while high-supersaturation pockets accelerate leading steps and trigger debunching. Conversely, anti-parallel flow advects depletion upstream and preserves uniform step spacing, with no bunching across tested conditions. In three dimensions, parallel flow yields stripe coalescence, while anti-parallel flow stabilizes step trains. By quantifying terrace supersaturation’s link to polytype nucleation, this robust, efficient model offers a predictive tool for optimizing step morphology and minimizing defects in high-quality SiC crystal growth.

SiC溶液生长过程中的阶梯流动动力学对表面形貌和缺陷形成至关重要，然而传统模型通常平均阶梯密度或遇到前跟踪奇点，而忽略了瞬态聚束和脱束。我们引入了一个准离散的二维/三维模型，该模型将平流-扩散输运与高斯正则化Robin边界条件耦合在一起，将宏步骤表示为局部积分匹配的汇。每个宏步由几个高斯加权节点解析，而溶质迁移是在精细的有限元网格上计算的，确保了稳定性和质量守恒。模拟结果表明，平行流驱动强聚束，形成过饱和度增大的宽阶地；由于溶质耗竭，聚束步骤的推进速度较慢，而高过饱和口袋加速了领先步骤并触发了脱溶。相反，反平行流在上游平流耗尽，并保持均匀的步距，在测试条件下没有聚束。在三维空间中，平行流动产生条形聚并，而反平行流动使阶跃序列稳定。通过量化台阶过饱和与多型成核的联系，这个稳健、高效的模型为优化台阶形貌和最小化高质量SiC晶体生长中的缺陷提供了预测工具。

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引用次数: 0

Particle swarm optimization-optimized long short-term memory prediction and Model-Free Adaptive Control for Czochralski silicon crystal growth Czochralski硅晶体生长的粒子群优化长短期记忆预测与无模型自适应控制

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-16 DOI: 10.1016/j.jcrysgro.2025.128421

Lin Hou , Dedong Gao , Shan Wang , Wenyong Zhang , Haixin Lin , Yan An , Xin Liu

In the manufacturing of Czochralski-grown silicon single crystals, production control mainly relies on operator experience and conventional feedback strategies, which are often insufficient for addressing the nonlinear, time-varying nature and sensitivity to disturbances of the process. Consequently, real-time tracking of key parameter dynamics remains challenging, resulting in adjustment delays and limiting improvements in product quality and production efficiency. To overcome these challenges, this study proposes a hybrid framework that integrates a Particle Swarm Optimization (PSO)-based Long Short-Term Memory (LSTM) prediction model with a Model-Free Adaptive Control (MFAC) method. PSO is employed to optimize the hyperparameters of LSTM and MFAC, thereby improving prediction accuracy and enhancing the responsiveness and stability of diameter regulation. Experimental results demonstrate that the PSO-LSTM prediction model significantly improves prediction accuracy, enabling more effective decision support during crystal growth. Moreover, the combined PSO-MFAC strategy achieves faster diameter control response than traditional PID control. This work integrates predictive modeling and advanced control techniques into the Czochralski silicon crystal growth process, offering a practical approach to enhancing production reliability and efficiency.

在czochralski生长硅单晶的制造中，生产控制主要依赖于操作员经验和传统的反馈策略，这些策略往往不足以解决过程的非线性、时变性质和对干扰的敏感性。因此，关键参数动态的实时跟踪仍然具有挑战性，导致调整延迟，限制了产品质量和生产效率的提高。为了克服这些挑战，本研究提出了一种混合框架，该框架将基于粒子群优化（PSO）的长短期记忆（LSTM）预测模型与无模型自适应控制（MFAC）方法相结合。利用粒子群算法对LSTM和MFAC的超参数进行优化，提高了预测精度，增强了直径调节的响应性和稳定性。实验结果表明，PSO-LSTM预测模型显著提高了预测精度，为晶体生长过程提供了更有效的决策支持。此外，组合PSO-MFAC策略比传统PID控制实现了更快的直径控制响应。这项工作将预测建模和先进的控制技术集成到Czochralski硅晶体生长过程中，为提高生产可靠性和效率提供了一种实用的方法。

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引用次数: 0

Porous silicon prepared by magnesiothermic reduction of silica extracted from a barley straw: Effect of silica crystallization 用镁热还原法从大麦秸秆中提取二氧化硅制备多孔硅：二氧化硅结晶的影响

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-13 DOI: 10.1016/j.jcrysgro.2025.128418

M. Naddaf

In this report, amorphous silica powder was extracted from an open atmosphere burned wild barley (Hordeum murinum ssp. leporinum) straw using the alkali leaching method. Nitrogen adsorption–desorption measurements, energy dispersive X-ray spectroscopy (EDS) and Fourier transform infrared spectroscopy (FTIR) results, and analysis reveal that the as-extracted amorphous silica is mesoporous with a large surface area (357 m²/g) and somewhat high content of carbon. X-ray diffraction (XRD) patterns showed that the extracted silica crystallized into the cristobalite phase, on heating it in an air atmosphere for 90 min at 1000 ˚C. The effect of the crystallization process on morphological and structural properties of porous silicon (PSi) produced from the extracted silica by magnesiothermic reduction has been investigated. The reduction process of the amorphous extracted silica resulted in the formation of a mixed phase of cubic Si and silicon carbide (SiC), which has a crystallinity index of 52 %, meso/micropores embedded in macro-size voids, average size of Si crystallites of ∼ 70 nm, and specific surface area of ∼ 160 m²/g. In comparison, the PSi produced from the crystallized silica exhibited a single cubic silicon nanocrystalline phase, higher purity, better crystallinity and a smaller average size of Si nano-crystallites. These suggest that the pre-crystallization of agriculture-derived silica precursor can be used as an effective way to produce high-quality PSi. The present work contributes to the previous reported literature on HF-free synthesis of PSi, a promising material for a wide range of applications.

本文从露天燃烧的野大麦中提取了无定形二氧化硅粉末。秸秆采用碱浸法。氮的吸附-解吸、能谱（EDS）和傅立叶变换红外光谱（FTIR）分析结果表明，萃取的无定形二氧化硅具有较大的比表面积（357 m2/g）和较高的碳含量的介孔结构。x射线衍射（XRD）表明，在1000℃的空气中加热90 min后，提取的二氧化硅结晶为方石石相。研究了晶化工艺对硅萃取物镁热还原法制备多孔硅（PSi）形貌和结构性能的影响。无定形萃取二氧化硅的还原过程形成了立方硅和碳化硅（SiC）的混合相，其结晶度指数为52%，中孔/微孔嵌入在大尺寸的孔洞中，Si晶体的平均尺寸为~ 70 nm，比表面积为~ 160 m2/g。相比之下，由二氧化硅结晶制备的PSi具有单立方硅纳米晶相、更高的纯度、更好的结晶度和更小的Si纳米晶的平均尺寸。这表明农业硅前驱体的预结晶可以作为生产高质量PSi的有效途径。本文对前人报道的无hf合成PSi材料的研究工作进行了补充，该材料具有广泛的应用前景。

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引用次数: 0

Sea urchin-like ZnO nanostructures from a zinc commercial primer for removal of methylene blue dye 一种用于去除亚甲基蓝染料的锌商业底漆制备的海胆状ZnO纳米结构

IF 2 4区材料科学 Q3 CRYSTALLOGRAPHY

Journal of Crystal Growth

Pub Date : 2025-11-13 DOI: 10.1016/j.jcrysgro.2025.128417

J. Nava-Martínez , M. Ballesteros-Balbuena , O.F. Olea-Mejía , A.R. Vilchis-Néstor , V.H. Castrejón-Sánchez , S. Camacho-López , M. Camacho-López

In the present work commercial zinc primer was used for the synthesis of sea urchin-like zinc oxide nanostructures. Zn primer was deposited on ceramic square plates followed by drying at ambient conditions. Using a tubular furnace, these samples were subjected to thermal oxidation at 420 °C in air for different treatment times in the range from 20 to 360 min. This allowed us to follow the growth of sea urchin-like nanostructures by scanning electron microscopy (SEM), where we found that the length of the needles of the sea urchin-like nanostructures becomes longer as the thermal oxidation time increases. A series of samples synthesized at 420 °C for 100, 180, and 360 min were prepared to be characterized by Raman spectroscopy, X-Ray diffraction, and scanning electron microscopy (SEM). The Raman spectra indicate the formation of nanometric ZnO in all prepared samples. The X-ray diffractograms gave evidence of a mixture of Zn and ZnO in all samples. Once properly characterized, these samples were used to perform adsorption tests of the model molecule Methylene Blue (MB). All three samples proved effective for MB removal at 78 % efficiency. The results presented in this work, show that the simple and low cost method of using a commercially available primer on ceramic substrates, and its thermal treatment in a conventional furnace, presents a simple and reproducible approach to obtaining sea urchin-like ZnO nanostructures with excellent adsorption retention features of MB dye.

本研究利用工业锌底漆合成了类海胆氧化锌纳米结构。将锌底漆沉积在方形陶瓷板上，然后在常温条件下干燥。使用管状炉，这些样品在420℃的空气中进行热氧化，在20到360分钟的范围内进行不同的处理时间。这使我们能够通过扫描电子显微镜（SEM）跟踪海胆样纳米结构的生长，我们发现随着热氧化时间的增加，海胆样纳米结构的针的长度变得更长。制备了一系列在420℃、100、180和360 min下合成的样品，用拉曼光谱、x射线衍射和扫描电子显微镜（SEM）对其进行了表征。拉曼光谱表明，在所制备的样品中均形成了纳米氧化锌。x射线衍射图证明所有样品中都有锌和氧化锌的混合物。一旦正确表征，这些样品被用来进行模型分子亚甲基蓝（MB）的吸附测试。所有三种样品都证明了对MB的去除效率为78%。本研究结果表明，在陶瓷衬底上使用一种简单、低成本的市售底漆，并在传统炉中进行热处理，是一种简单、可重复的方法，可以获得具有优异吸附保留MB染料特性的海胆状ZnO纳米结构。

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