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Wet bulk micromachining of Borofloat glass towards the fabrication of through-holes in different concentrations of hydrofluoric acid 在不同浓度氢氟酸中制备通孔的硼浮法玻璃湿体微加工
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-07-22 DOI: 10.1111/ijag.70004
Vishal Sahu, Robbi Vivek Vardhan, Priyanka Dewangan, Yogesh Kumar Srivastava, Prem Pal

Glass through-holes are essential for wafer-level packaging of microelectromechanical systems (MEMS) devices and are often fabricated through wet bulk micromachining. For efficient through-hole fabrication, there is a need for the development of cost-effective masking layers and faster etching processes. This work presents an economical method for fabricating through-holes of various dimensions in 500 µm-thick Borofloat glass wafers with a relatively high etch rate using wet bulk micromachining. The process employs wet isotropic etching in 25% and 30% hydrofluoric acid (HF), utilizing a masking layer of sputter-deposited Cr thin film and spin-coated positive photoresist. The masking layer revealed strong adhesion to the wafers during the entire etching process, enabling the fabrication of through-holes with sharp edges. Additionally, the masking layer delivered excellent resistance to both HF concentrations, establishing effective protection, and subsequently resulting in minimal defects on the wafer surface. Through-holes are fabricated in 190 min using 25% HF and in 150 min using 30% HF, with the latter facilitating comparatively faster fabrication due to its higher HF concentration. The present work demonstrates the best output in terms of faster etching time for through-holes fabrication in glass wafers using a Cr thin film combined with a photoresist as a masking layer.

玻璃通孔对于微电子机械系统(MEMS)器件的晶圆级封装是必不可少的,通常通过湿体微加工来制造。为了实现高效的通孔制造,需要开发具有成本效益的掩蔽层和更快的蚀刻工艺。本研究提出了一种经济的方法,可以在500微米厚的硼浮法玻璃晶圆上制造各种尺寸的通孔,并具有相对较高的蚀刻速率。该工艺采用湿法各向同性蚀刻,在25%和30%的氢氟酸(HF)中,利用溅射沉积的Cr薄膜和自旋涂层的正光刻胶掩盖层。在整个蚀刻过程中,掩蔽层显示出与晶圆的强附着力,使得制造具有锋利边缘的通孔成为可能。此外,掩蔽层对两种HF浓度都具有优异的抵抗力,建立了有效的保护,并随后在晶圆表面产生最小的缺陷。用25%的HF在190分钟内制造通孔,用30%的HF在150分钟内制造通孔,后者由于其较高的HF浓度而有利于相对更快的制造。目前的工作表明,在使用铬薄膜和光阻剂作为掩蔽层在玻璃晶圆中制造通孔时,在更快的蚀刻时间方面的最佳输出。
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引用次数: 0
Experimental investigation of fifth oxide effects on calcium–magnesium–aluminosilicate glass properties 第五氧化物对钙镁铝硅酸盐玻璃性能影响的实验研究
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-07-16 DOI: 10.1111/ijag.70003
Clark A. Luckhardt, Elizabeth J. Opila

Molten calcium–magnesium–aluminosilicate (CMAS) containing debris is a leading threat to hot-section components in air-ingesting turbine engines. This study investigated common natural-forming and coating-derived oxide additions to CMXAS glasses—where X denotes a fifth oxide constituent. Glass property relationships are elucidated by cation size effects and allow inferences to glass structure to be made. Iron oxide content, Group IV metal, and rare-earth metal cations—including one dual cation addition (Y3+ and Yb3+)—effects on CMAS viscosity, coefficient of thermal expansion (CTE), softening temperature, and glass transition temperature were explored. The baseline material, nominally a 33 CaO–9 MgO–13 AlO1.5–45 SiO2 (single cation oxide mol%) CMAS, was synthesized from constituent oxide powders. Natural-forming additions consistently operated as network modifiers. However, coating-derived additions behaving as network modifiers in the molten liquid state were found to behave as network formers in the condensed amorphous state. Fe3+ additions were shown to have the greatest effect of all additions on glass properties, exhibiting the greatest propensity for CMAS attack. Trends observed between dilatometric CMXAS glass properties allow for CMXAS properties to be inferred should one property (CTE, Td, Tg) be known. Coating performance should consider the effect of coating constituent on CMAS viscosity and CTE, dissolution, and precipitation behaviors.

含碎片的熔融钙镁铝硅酸盐(CMAS)是进气涡轮发动机热截面部件的主要威胁。本研究调查了常见的自然形成和涂层衍生的氧化物添加到CMXAS玻璃中,其中X表示第五种氧化物成分。通过阳离子尺寸效应阐明了玻璃的性质关系,并对玻璃结构进行了推断。探讨了氧化铁含量、IV族金属和稀土金属阳离子(包括一个双阳离子添加(Y3+和Yb3+))对CMAS粘度、热膨胀系数(CTE)、软化温度和玻璃化转变温度的影响。以组成氧化物粉末为原料,合成了标称为33 CaO-9 MgO-13 AlO1.5-45 SiO2(单阳离子氧化物摩尔%)CMAS的基准材料。自然形成的添加剂始终作为网络调节剂。然而,涂层衍生的添加剂在熔融液体状态下表现为网络改性剂,在凝聚非晶状态下表现为网络形成剂。在所有添加物中,Fe3+对玻璃性能的影响最大,表现出最大的CMAS攻击倾向。观察到的膨胀CMXAS玻璃性质之间的趋势允许推断CMXAS性质,如果一个性质(CTE, Td, Tg)是已知的。涂层性能应考虑涂层成分对CMAS粘度和CTE、溶解和沉淀行为的影响。
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引用次数: 0
The development and application of the stirred-reactor coupon analysis (SRCA) test method 搅拌反应器剩余物分析(SRCA)试验方法的开发与应用
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-07-15 DOI: 10.1111/ijag.16707
Joelle T. Reiser, James J. Neeway, Scott K. Cooley, Benjamin Parruzot, Alejandro Heredia-Langner, Stéphane Gin, Manon Thomas, Nicholas J. Smith, Jonathan P. Icenhower, Nicholas Stone-Weiss, Yuta Takahashi, Hajime Iwata, Seiichiro Mitsui, Junya Sato, Christoph Lenting, Yaohiro Inagaki, Mike T. Harrison, Jincheng Du, Wenqing Xie, Karine Ferrand, Clare L. Thorpe, Ramya Ravikumar, Claire L. Corkhill, John S. McCloy, Michelle M. V. Snyder, Amanda R. Lawter, Gary L. Smith, R. Matthew Asmussen, Joseph V. Ryan

A new technique, termed the stirred-reactor coupon analysis (SRCA) method, has been developed to measure the rate of glass dissolution in forward-rate conditions. Monolithic glass coupons are partially masked with an inert material before placement in a large volume of well-mixed solution with known chemistry and temperature for a predetermined duration. After the test, the mask is removed, and the difference in step height between the protected area and the exposed corroded portions of the sample coupon is measured to determine the extent of glass dissolution. The step height is converted to a rate measurement using the test duration and glass density. Test parameters such as sample surface preparation and test duration were evaluated to determine their effects on the measured rates. Additionally, results from an interlaboratory study (ILS) consisting of 12 laboratories from 11 different institutions are presented, where each laboratory performed 12 independent tests. When removing experimental outlier data, the 95% reproducibility limits for the SRCA method has no statistical difference with previously published standardized test methods used to determine the forward rate of glass dissolution. Overall, this paper describes steps necessary to perform the test method and provides the statistical calculations to evaluate test accuracy.

一种新的技术,被称为搅拌反应器联用分析(SRCA)方法,已经开发了测量玻璃溶解速率在正速率条件下。单片玻璃片片在放置在已知化学性质和温度的大量混合溶液中预先确定的时间之前,用惰性材料部分掩盖。测试结束后,取下面罩,测量受保护区域与样品片暴露腐蚀部分之间的阶高差,以确定玻璃溶解的程度。使用测试持续时间和玻璃密度将台阶高度转换为速率测量。测试参数,如样品表面制备和测试持续时间进行评估,以确定其对测量速率的影响。此外,还介绍了由来自11个不同机构的12个实验室组成的实验室间研究(ILS)的结果,其中每个实验室进行了12项独立测试。在去除实验异常值数据后,SRCA方法95%的重现性限与先前发表的用于确定玻璃向前溶出速率的标准化测试方法没有统计学差异。总体而言,本文描述了执行测试方法所需的步骤,并提供了评估测试准确性的统计计算。
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引用次数: 0
Mechanical effects of ion-implanted gold nanoparticles on the surface properties of silica glass 离子注入金纳米粒子对二氧化硅玻璃表面性能的力学影响
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-06-16 DOI: 10.1111/ijag.70002
José R. Pérez-Higareda, Jesús A. Torres, César Leyva-Porras, Oscar O. Solís-Canto, Carlos Torres-Torres, Alicia Oliver, David Torres-Torres

Silica glass (SG) is a highly versatile material used in optics, electronics, construction, and medicine due to its transparency and mechanical properties. However, enhancing its performance poses scientific challenges, especially in reinforcing it while preserving these properties and understanding its deformation under stress. This study investigates the effect of gold nanoparticles (AuNPs) on the mechanical response of SG material. AuNPs were nucleated into high-purity SG using a 3MV Tandem Accelerator Pelletron, followed by thermal annealing at 600°C in an H2 + N2 atmosphere. High-resolution transmission electron microscopy (HRTEM) revealed a Gaussian distribution of AuNPs at a depth of ∼450 nm. Nanoindentation tests indicated minor variations in hardness (1.5%) and reduced elastic modulus (4.4%) with AuNP incorporation. Scratch tests demonstrated that the mechanical integrity of the AuNPs/SG sample was preserved when deformation remained below the determined fracture load of SG, although it exhibited a slightly higher coefficient of friction. Finite element analysis provided insights into the strain behavior within the AuNP zone, confirming how AuNPs distribute stress within the SG matrix.

二氧化硅玻璃(SG)是一种高度通用的材料,由于其透明度和机械性能,用于光学,电子,建筑和医学。然而,提高其性能带来了科学挑战,特别是在保持这些特性的同时加强它,并了解其在应力下的变形。研究了金纳米颗粒对SG材料力学响应的影响。使用3MV串联加速器Pelletron将AuNPs核成高纯度的SG,然后在H2 + N2气氛中在600℃下进行热退火。高分辨率透射电子显微镜(HRTEM)显示,AuNPs在深度约450 nm处呈高斯分布。纳米压痕试验表明,掺入AuNP后,硬度变化较小(1.5%),弹性模量降低(4.4%)。划痕试验表明,当变形低于SG的确定断裂载荷时,AuNPs/SG样品的力学完整性得以保留,尽管它表现出略高的摩擦系数。有限元分析揭示了AuNP区域内的应变行为,确认了AuNP如何在SG矩阵内分布应力。
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引用次数: 0
Er3+–Yb3+-codoped LaF3 glass–ceramic optical fiber Er3+ -Yb3 +-共掺LaF3玻璃陶瓷光纤
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-06-10 DOI: 10.1111/ijag.70001
M. Sedano, M. Kochanowicz, D. Dorosz, A. Durán, J. Fernández, R. Balda, M. J. Pascual

This paper reports the preparation and characterization of LaF3-based glass–ceramic (GC) optical fibers codoped with Er3+ and Yb3+ ions, using the rod-in-tube method with Duran glass as cladding. Structural analysis, including x-ray diffraction and transmission electron microscopy, confirmed the presence of LaF3 nanocrystals in the core, with sizes ranging from 8 to 10 nm, slightly smaller than those observed in bulk samples due to the higher cooling rate during fiber drawing. Optical measurements showed transmission losses of 13 dB/m for the GC fibers after heat treatment at 660°C for 40 h. Upconversion (UC) emissions were observed in the green (2H11/2, 4S3/24I15/2), red (4F9/24I15/2), and blue (2H9/24I15/2) regions upon excitation at 980 nm. The dependence of UC emission on pump power showed a near linear dependence, which can be explained by saturation effects in the intermediate energy states and indicates that the UC process is driven by energy transfer from Yb3+ to Er3+ ions. These results demonstrate the potential of these fibers for advanced optical applications, including telecommunication, sensors and laser technologies.

本文报道了以Duran玻璃为包层,采用管中棒法制备Er3+和Yb3+离子共掺杂的laf3基玻璃陶瓷(GC)光纤,并对其性能进行了表征。结构分析,包括x射线衍射和透射电子显微镜,证实了核心中存在LaF3纳米晶体,尺寸在8到10 nm之间,由于纤维拉伸过程中的冷却速率较高,比在体样品中观察到的尺寸略小。光学测量表明,在660°C热处理40小时后,GC光纤的传输损耗为13 dB/m。在980 nm激发时,在绿色(2H11/2、4S3/2→4I15/2)、红色(4F9/2→4I15/2)和蓝色(2H9/2→4I15/2)区域观察到上转换(UC)发射。UC发射对泵浦功率的依赖表现为近线性关系,这可以用中间能态的饱和效应来解释,表明UC过程是由Yb3+离子向Er3+离子的能量转移驱动的。这些结果证明了这些光纤在先进光学应用方面的潜力,包括电信、传感器和激光技术。
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引用次数: 0
Topological constraint model of alkaline earth vanadate glasses 碱土钒酸盐玻璃的拓扑约束模型
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-06-04 DOI: 10.1111/ijag.70000
Adam Shearer, John C. Mauro

Topological constraint theory has enabled the successful prediction of glass properties over a wide range of compositions. In this study, a topological constraint model is constructed for alkaline earth vanadate glasses based on experimental data. The change in vanadate structural units from VO5 to VO4 was modeled as a function of alkaline earth content and related to thermal and mechanical properties. The model covers both high- and low-temperature properties to probe the temperature dependence of constraint rigidity for each constituent of the glass network. The model is changed to describe anomalies in magnesium sites potentially implying that magnesium can form locally rigid structures. Furthermore, the traditional understanding of vanadate glass structure is compared to recent results concluding that the terminal oxygen must exist as a part of the VO4 units. Results for the model explain that bridging oxygen constraints are the main contributors to network rigidity in both low- and high-temperature regimes. Vanadate glass networks are highly connected even with the introduction of modifier species, which introduce their own bond constraints. Corroboration between experimental data and the topological constraint model illustrates the role of alkaline earth oxides in the glass network.

拓扑约束理论已经成功地预测了玻璃在各种成分上的性能。本文基于实验数据,建立了碱土钒酸盐玻璃的拓扑约束模型。钒酸盐结构单元从VO5到VO4的变化是碱土含量的函数,并与热力学性能有关。该模型涵盖了高温和低温性能,以探索玻璃网络每个组成部分的约束刚度对温度的依赖关系。该模型被改变为描述镁位点的异常,这可能意味着镁可以形成局部刚性结构。此外,对钒酸盐玻璃结构的传统理解与最近的研究结果进行了比较,得出了终端氧必须作为VO4单元的一部分存在的结论。该模型的结果解释了桥接氧约束是低温和高温条件下网络刚性的主要贡献者。钒酸盐玻璃网络是高度连接的,即使引入了改性剂种类,引入了自己的键约束。实验数据与拓扑约束模型之间的印证说明了碱土氧化物在玻璃网络中的作用。
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引用次数: 0
Femtosecond laser crystallization of YAG in yttrium aluminosilicate glasses 钇铝硅酸盐玻璃中YAG的飞秒激光结晶
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-05-28 DOI: 10.1111/ijag.16710
Collin Barker, Brian Knorr, Monika Michálková, Marzieh Ghadamyari, Milan Parchoviansky, Daniel Drdlík, Dušan Galusek, Himanshu Jain, Volkmar Dierolf

This work demonstrates the capability to crystallize YAG via femtosecond pulsed laser. Challenges in using melt-quench glass are shown to restrict glass composition and have not yielded YAG via femtosecond laser crystallization. An alternative glass-making technique was used to fabricate a range of compositions not otherwise possible. Glasses of YAG with added silica in the range of 0–20 mol% were tested under the laser to explore the allowable deviation from stoichiometric YAG. Raman spectroscopy and Electron backscatter diffraction indicated successful fabrication of YAG, and usage of combined excitation emission spectroscopy (CEES) allowed probing of erbium doped compositions.

这项工作证明了用飞秒脉冲激光结晶钇铝石榴石的能力。使用熔融淬火玻璃的挑战显示限制了玻璃成分,并且通过飞秒激光结晶无法产生YAG。另一种玻璃制造技术被用来制造一系列不可能的组合物。在激光下对添加了0-20摩尔%二氧化硅的YAG玻璃进行了测试,以探索其与化学计量YAG的允许偏差。拉曼光谱和电子背散射衍射表明YAG的制备成功,使用联合激发发射光谱(CEES)可以探测掺铒成分。
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引用次数: 0
Effect of Al2O3 and Ga2O3 on the photoluminescence of borosilicate glasses embedding CsPbBr3 perovskite nanocrystals Al2O3和Ga2O3对包埋CsPbBr3钙钛矿纳米晶的硼硅酸盐玻璃光致发光的影响
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-05-27 DOI: 10.1111/ijag.16709
Thi Thuy Pham, Jinju Lee, Devarajulu Gelija, Woon Jin Chung

CsPbBr3 perovskite nanocrystals (PNCs) were successfully embedded in a borosilicate glass matrix for a robust green color converter, and its photoluminescence quantum yield (PLQY) was optimized by varying glass composition and heat treatment conditions. A high PLQY of up to 68% was obtained under 450 nm excitation by adjusting ZnO and Al2O3 content and by incorporating Ga2O3. The formation of PNCs was confirmed by X-ray diffraction (XRD) and transmission electron microscope (TEM), while the effect of compositional variation was investigated by nuclear magnetic resonance (NMR), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Time-resolved photo-luminescence (TRPL) also examined the effect of the composition and the heat treatment on the PLQY. Thermal, chemical, and photonic stabilities of the CsPbBr3 PNC embedded glass (PNEG) were examined to show its robustness for practical applications. A white light-emitting device consisting of CsPbBr3 PNEG and commercial red phosphor (K2SiF6:Mn4+) with an InGaN blue LED chip was composed and achieved a wide color gamut reaching up to 131% of the NTSC standard, successfully demonstrating its practical feasibility as a color converter for display applications.

将CsPbBr3钙钛矿纳米晶体(PNCs)成功嵌入到硼硅酸盐玻璃基体中,用于鲁棒绿色转换器,并通过改变玻璃成分和热处理条件来优化其光致发光量子产率(PLQY)。通过调整ZnO和Al2O3的含量以及加入Ga2O3,在450 nm激发下获得了高达68%的高PLQY。通过x射线衍射(XRD)和透射电子显微镜(TEM)证实了pnc的形成,并通过核磁共振(NMR)、拉曼光谱(Raman spectroscopy)和x射线光电子能谱(XPS)研究了组分变化对pnc的影响。时间分辨光致发光(TRPL)也考察了组分和热处理对PLQY的影响。研究了CsPbBr3 PNC嵌入式玻璃(PNEG)的热稳定性、化学稳定性和光子稳定性,证明了其在实际应用中的鲁棒性。由CsPbBr3 PNEG和商用红色荧光粉(K2SiF6:Mn4+)组成的白色发光器件与InGaN蓝色LED芯片组成,实现了高达NTSC标准131%的宽色域,成功地证明了其作为显示应用的颜色转换器的实际可行性。
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引用次数: 0
Impacts of Cr(III) and Cr(VI) concentrations on key high-level waste glass properties Cr(III)和Cr(VI)浓度对高废玻璃关键性能的影响
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-05-15 DOI: 10.1111/ijag.16708
Vivianaluxa Gervasio, Sarah A. Saslow, Jesse B. Lang, Bjorn E. Westman, Derek A. Cutforth, Suzanne M. Baird, Sulaiman E. Sannoh, Renee L. Russell, Jarrod V. Crum, AA Kruger, John D. Vienna

This study investigates the effects of chromium concentration and redox on simulated high-level waste (HLW) borosilicate glass properties for high-chromium Hanford wastes. Thirty glasses with target 1 ≤ Cr2O3 ≤ 2.5 wt% were fabricated and analyzed. The Cr redox ratios were measured using K-edge X-ray absorption near edge structure along with properties of interest to vitrification of Hanford HLW: crystal formation after centerline canister cooling, crystallinity as a function of temperature, viscosity, electrical conductivity, toxic characteristic leaching procedure and product consistency test (PCT) responses, and SO3 solubility. Only Cr(III) and Cr(VI) were identified in the test glasses, and their ratio was found to be largely correlated to optical basicity. Cr redox appeared to have a significant impact on most of the properties, except for PCT. Most properties were affected differently by Cr(III) than by Cr(VI). These effects were quantified and rationalized based on the previously studied bonding nature of the two primary oxidation states.

研究了铬浓度和氧化还原对高铬汉福德废渣模拟高废渣硼硅酸盐玻璃性能的影响。制备了30个靶1≤Cr2O3≤2.5 wt%的玻璃并进行了分析。利用k边x射线吸收近边结构测量了Cr的氧化还原比,以及对汉福德高铁玻璃化感兴趣的特性:中心线罐冷却后的晶体形成,结晶度作为温度、粘度、电导率、毒性特征浸出过程和产品一致性测试(PCT)响应的函数,以及SO3的溶解度。在测试玻璃中只鉴定出Cr(III)和Cr(VI),并且发现它们的比例与光学碱度有很大关系。Cr(III)和Cr(VI)对大多数性质的影响不同,Cr(III)和Cr(VI)对大多数性质的影响不同。这些影响是量化和合理化的基础上,先前研究的键合性质的两个主要氧化态。
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引用次数: 0
Properties, mechanisms, and perspectives of ultrafast laser modifications in silicate glass volume 超快激光修饰硅酸盐玻璃体积的性质、机理和前景
IF 2.5 3区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-05-14 DOI: 10.1111/ijag.16706
Nadezhda Shchedrina, Matilde Sosa, Maxime Cavillon, Matthieu Lancry

Ultrafast laser irradiation of glass enables highly localized structural transformations within the material's bulk, unlocking diverse applications in photonics, data storage, and microfabrication. Here, we provide a concise yet comprehensive overview of the main types of femtosecond laser-induced modifications in silica-based glasses (Types I, II, III, X, and related crystalline transformations), highlighting their distinct features and underlying thermal- and pressure-driven mechanisms. This review offers a current state-of-the-art perspective on various modifications, while also presenting new nanoscale insights through advanced scattering scanning near-field optical microscopy and nano-Fourier transform infrared spectroscopy, discussing the densification mechanisms behind. Finally, we outline broader perspectives, from fundamental research directions to industry developments, to inspire future advances in next-generation optical technologies.

玻璃的超快激光照射可以在材料体内实现高度局部化的结构转换,从而在光子学、数据存储和微制造方面实现多种应用。在这里,我们提供了一个简洁而全面的概述主要类型的飞秒激光诱导改性硅基玻璃(类型I, II, III, X,以及相关的晶体转化),突出其独特的特点和潜在的热和压力驱动的机制。这篇综述提供了当前最先进的各种改性的观点,同时也通过先进的散射扫描近场光学显微镜和纳米傅里叶变换红外光谱提出了新的纳米尺度的见解,讨论了致密化背后的机制。最后,我们概述了更广阔的前景,从基础研究方向到产业发展,以激发下一代光学技术的未来发展。
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引用次数: 0
期刊
International Journal of Applied Glass Science
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