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Key melt properties for controlled synthesis of glass beads by aerodynamic levitation coupled to laser heating 气动悬浮-激光加热控制合成玻璃珠的关键熔体特性
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-02-23 DOI: 10.1111/ijag.16627
Jan Baborák, Maureen Yembele, Petr Vařák, Sandra Ory, Emmanuel Véron, Michael J. Pitcher, Mathieu Allix, Pavla Nekvindová, Alessio Zandonà

Binary alkali silicate glasses were synthesized as beads by aerodynamic levitation coupled to laser heating to test the applicability of the method to this compositional range. While bubble-free lithium disilicate beads could be easily obtained, sodium and potassium silicates proved more challenging to melt without significant alkali evaporation: the final samples contained bubbles and exhibited compositional drifts compared to the starting stoichiometry, especially at high SiO2 content. The risk of volatilization from the melts was evaluated empirically: the volatility of each oxide component scaled to the ratio between its melting temperature Tm and the Tm of the target composition (revap), while the difference between such ratios (Δevap) provided a qualitative estimation of the risk of differential evaporation. The formulated approach enables to evaluate the suitability of aerodynamic levitation synthesis for a given target glass composition: while low melting temperature and low liquidus viscosity (η < 100 Pa s) represent the primary optimal conditions, more viscous materials can still be prepared without major compositional drifts using a more careful melting procedure, especially if revap and Δevap are minimized.

采用气动悬浮耦合激光加热的方法合成了二元碱硅酸盐玻璃微珠,验证了该方法在该成分范围内的适用性。虽然可以很容易地获得无气泡的二硅酸锂微珠,但事实证明,在没有明显碱蒸发的情况下熔化硅酸钠和硅酸钾更具挑战性:与开始的化学计量相比,最终样品含有气泡,并表现出成分漂移,特别是在高SiO2含量时。对熔体挥发的风险进行了经验评估:将每种氧化物成分的挥发性按比例计算为其熔化温度Tm与目标成分Tm之间的比值(revap),而这些比值之间的差值(Δevap)提供了对差异蒸发风险的定性估计。制定的方法能够评估空气动力学悬浮合成对给定目标玻璃成分的适用性:当低熔融温度和低液相粘度(η <100 Pa s)代表主要的最佳条件,使用更仔细的熔化程序仍然可以制备更粘稠的材料,而不会产生主要的成分漂移,特别是如果revap和Δevap最小化。
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引用次数: 2
An optical technique based on silicate glass sintering for temperature mapping 基于硅酸盐玻璃烧结的温度映射光学技术
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-01-21 DOI: 10.1111/ijag.16625
Noah Burke, Panagiotis Panoutsopoulos, Otto J. Gregory

Thermal paints have been used for decades by the gas turbine engine community to map surface temperature with low resolution. A novel thermal paint based on the sintering of a lead-silicate glass powder was developed that can map maximum temperature with high resolution (±5°C) over a 60°C range beginning at the glass transition temperature (Tg${T}_g$). The paint exhibited excellent adhesion to nickel-based superalloy components due to similar coefficients of thermal expansion between the superalloy and glassy ceramic coating. An optical transition was qualitatively and quantitatively observed using scanning electron microscopy, ultraviolet-visible (UV-VIS) reflectance spectroscopy, and visual inspection. UV-VIS reflectance spectroscopy was used to confirm the optical transition observed by the naked eye and quantitatively assess the transition of the thermal paint with high resolution. This technique for obtaining high resolution experimental temperature maps can aid the performance, efficiency, and reliability of gas turbine engines.

几十年来,燃气涡轮发动机社区一直使用热漆来绘制低分辨率的表面温度图。一种基于铅硅酸盐玻璃粉烧结的新型热涂料可以在玻璃化转变温度(T g$ {T}_g$)开始的60°C范围内以高分辨率绘制最高温度(±5°C)。由于高温合金和玻璃陶瓷涂层之间的热膨胀系数相似,该涂料与镍基高温合金组分具有良好的附着力。通过扫描电子显微镜、紫外-可见(UV-VIS)反射光谱和目视检查,定性和定量地观察到光学转变。采用UV-VIS反射光谱法对肉眼观察到的光学跃迁进行了确认,并对热涂料的跃迁进行了高分辨率的定量评价。这种获得高分辨率实验温度图的技术有助于提高燃气涡轮发动机的性能、效率和可靠性。
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引用次数: 1
Structure and redox ratio of soda-lime-silica glasses with high iron oxide concentrations 高氧化铁浓度钠钙硅玻璃的结构和氧化还原率
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-01-20 DOI: 10.1111/ijag.16626
Tina Tasheva, Ruzha Harizanova, Irena Mihailova, Zara Cherkezova-Zheleva, Daniela Paneva, Milena Nedkova, Christian Rüssel

The high temperature synthesis of glasses in the system (100-x)(0.16Na2O/0.10CaO/0.74SiO2)/xFe2O3, x = 5 ÷ 20 mol% is reported. For Fe2O3 concentrations ≤15 mol%, glasses are formed while the sample with 20 mol% crystallizes during cooling the melt. X-ray diffraction shows the crystallization of magnetite. The microstructure of the glass-crystalline sample is investigated by optical microscopy and scanning electron microscopy and two types of iron-rich crystals corresponding to magnetite and hematite are detected. The refractive indices as determined by the Becke line method are in the 1.567 - 1.639 range and. increase with increasing Fe2O3 concentration. The structure is characterized using Infra-red spectroscopy. The presence of symmetric stretching, asymmetric stretching and bending vibrations of Si-O-Si is detected and attributed to the occurrence of SiO4 tetrahedral units with varying numbers of nonbridging oxygens. Also, the increasing Fe2O3 concentration results in occurrence of Fe-O-Si bonds indicating the glass network depolymerization due to Fe2O3 addition. In all samples, the presence of Fe3+ and Fe2+ and the existence of iron ions in tetrahedral and octahedral coordination, as well as a very small amount of Fe0 and the precipitation of hematite and magnetite in the glass-crystalline sample is revealed by Mössbauer spectroscopy.

报道了在(100-x)(0.16Na2O/0.10CaO/0.74SiO2)/xFe2O3体系中高温合成玻璃,x = 5 ÷ 20 mol%。当Fe2O3浓度≤15 mol%时,玻璃形成,而当Fe2O3浓度为20 mol%时,熔体在冷却过程中结晶。x射线衍射显示了磁铁矿的结晶。利用光学显微镜和扫描电镜对玻璃晶样品的微观结构进行了研究,检测到磁铁矿和赤铁矿两种富铁晶体。贝克线法测定的折射率在1.567 ~ 1.639之间。随Fe2O3浓度的增加而增加。利用红外光谱对其结构进行了表征。Si-O-Si的对称拉伸、不对称拉伸和弯曲振动的存在被检测到,并归因于具有不同数量的非桥接氧的SiO4四面体单元的出现。此外,Fe2O3浓度的增加导致Fe-O-Si键的出现,表明由于Fe2O3的加入导致玻璃网络解聚。Mössbauer光谱分析表明,在所有样品中均存在Fe3+和Fe2+,铁离子以四面体和八面体配位存在,以及极少量的Fe0和玻璃晶样品中赤铁矿和磁铁矿的析出。
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引用次数: 4
Study on gas trapping during precision glass molding of microlens array in a nitrogen atmosphere 氮气氛下微透镜阵列精密玻璃成型过程中的气体捕获研究
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-01-19 DOI: 10.1111/ijag.16624
Tianfeng Zhou, Zihao Zeng, Qian Yu, Jia Zhou, Peng Liu, Xibin Wang

Microlens arrays will suffer from filling defects due to trapped gas when molded in a nitrogen atmosphere by precision glass molding (PGM). In this paper, a multistep molding method is proposed to avoid gas trapping and improve the accuracy of a microlens array. The defect formation mechanism of the microlens array caused by the trapped gas is investigated, and the effect of the molding pressure on the defect formation is analyzed. A numerical model of the mold-nitrogen-glass interface at high temperature is established to evaluate the defect evolution, and the minimum number of PGM steps required to greatly reduce defects caused by the trapped gas is predicted. The numerical model is validated by a multistep PGM experiment of D-K59 glass material. The results show that a three-step PGM process significantly reduced the height of the defect. The difference between the height of the microlens unit and the depth of the mold is less than 0.4%. The molded microlens array has a peak-to-valley value of 0.38 μm and a surface roughness Ra of 3.5 nm. This work is instructive for the fabrication of high-precision glass microlens arrays.

微透镜阵列在氮气环境中采用精密玻璃模压成型(PGM)时,会因困住气体而产生填充缺陷。本文提出了一种多步成型方法,以避免气体捕获,提高微透镜阵列的精度。研究了困气对微透镜阵列缺陷形成的机理,分析了成型压力对缺陷形成的影响。建立了高温下模具-氮-玻璃界面的数值模型,对缺陷演化过程进行了评价,并预测了能大大减少被捕获气体引起的缺陷所需的最小PGM步骤数。通过D-K59玻璃材料的多步PGM实验验证了数值模型的有效性。结果表明,三步PGM工艺显著降低了缺陷的高度。微透镜单元高度与模具深度的差值小于0.4%。模制微透镜阵列的峰谷值为0.38 μm,表面粗糙度Ra为3.5 nm。该工作对高精度玻璃微透镜阵列的制作具有指导意义。
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引用次数: 3
Effect of draw temperature and flame polishing on birefringence of silica glass fiber 拉伸温度和火焰抛光对硅玻璃纤维双折射性能的影响
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-01-15 DOI: 10.1111/ijag.16623
Bronson D. Hausmann, Thomas W. Hawkins, John Ballato, Minoru Tomozawa

Recently developed methods for high resolution birefringence measurement have been applied to distinguish between the surface and interior birefringence of silica glass fibers as a function of drawing temperature and initial surface condition for two types of silica glass with different water contents. Fibers were drawn in a water-free argon environment using graphite heating elements. It was found that fibers drawn at lower temperatures resulted in greater, interior birefringence, in agreement with previous reports. Additionally, it was found that in the case of low-water silica glass, flame polishing via oxygen–hydrogen mixture and drawn into fibers at lower temperature resulted in significant surface compressive stress upon drawing. This compressive stress may be the result of surface stress relaxation in silica glass that occurs in the presence of water during fiber drawing. In silica glass that contains greater internal hydroxyl impurity concentrations, the interior birefringence as well as the surface stress relaxation was significantly reduced under the same fiber drawing conditions. Characterization of such stress responses provides insight into the effects of common processing techniques as well as impresses the significance of preform processing for consistent fiber production.

应用近年来发展的高分辨率双折射测量方法,对两种不同含水量的硅玻璃纤维进行了表面和内部双折射的区分,并将其作为拉伸温度和初始表面条件的函数。使用石墨加热元件在无水氩气环境中拉伸纤维。研究发现,在较低温度下拉伸的纤维产生了更大的内部双折射,这与之前的报道一致。此外,在低水二氧化硅玻璃的情况下,通过氧氢混合物进行火焰抛光并在较低温度下拉伸到纤维中,在拉伸时产生显着的表面压应力。这种压应力可能是二氧化硅玻璃表面应力松弛的结果,这种应力松弛发生在纤维拉伸过程中存在水的情况下。在内部羟基杂质浓度较大的硅玻璃中,在相同的纤维拉伸条件下,内部双折射和表面应力松弛明显降低。这种应力响应的表征提供了对常见加工技术的影响的深入了解,以及对一致纤维生产的预成型加工的重要性的深刻印象。
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引用次数: 0
Case II diffusion of water in Na2O–3SiO2 glass: Constant tensile stress gradient at the diffusion interface 案例II水在Na2 O‐3SiO2玻璃中的扩散:扩散界面处的恒定拉伸应力梯度
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2023-01-13 DOI: 10.1111/ijag.16622
Bronson D. Hausmann, Minoru Tomozawa

Some polymers and oxide glasses exhibit unusual diffusion of liquid or gas, with the depth of diffusion exhibiting a linear increase with time, instead of normal square root of time dependence. There have been many models, but very few experimental data that can help clarify the cause of the phenomenon's existence in glass. Residual stress in sodium trisilicate glass (Na2O–3SiO2) samples was characterized following Case II water diffusion at 80°C in a saturated water vapor environment. The surface-swelled layer of the glass was removed by dissolving it in water, and birefringence of the newly revealed surface layer was measured. The presence of a constant negative tensile stress gradient was revealed by indicating that Case II diffusion in sodium trisilicate glass originates from this stress gradient, which overwhelms the more typical Fick's law concentration-dependent flux.

一些聚合物和氧化物玻璃表现出不寻常的液体或气体扩散,扩散深度随时间线性增加,而不是正常的时间依赖的平方根。有很多模型,但很少有实验数据,可以帮助澄清现象的原因存在于玻璃。在饱和水蒸气环境下,在80°C条件下,用Case II水扩散表征了三硅酸钠玻璃(na20 - 3sio2)样品的残余应力。通过将玻璃溶解在水中去除表面膨胀层,并测量新露出的表面层的双折射。在三硅酸钠玻璃中,存在一个恒定的负拉伸应力梯度,表明情况II扩散源于这个应力梯度,这压倒了更典型的菲克定律浓度依赖性通量。
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引用次数: 0
Structural, spectroscopic, and radiation shielding properties of Pb2+-doped borate and phosphate glasses 掺pb2 +硼酸盐和磷酸盐玻璃的结构、光谱和辐射屏蔽性能
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2022-12-22 DOI: 10.1111/ijag.16621
Hosam Othman, Brian Topper, Hagar Elkholy, Doris Möncke

Lead-containing alkali/alkaline-earth borate and barium lead phosphate glasses were prepared by melt-quenching for a detailed investigation of the Pb2+ ions’ optical properties. UV–Vis absorption and photoluminescence spectroscopy reveal variations in the s–p transition of Pb2+, which are shown to correlate with the optical basicity of the host glass in both borates and phosphates. Pb2+ emission differs significantly for borate and phosphate glasses, as the nature of the charged sites available to accommodate Pb2+ cations vary. Optical basicity values were determined from the composition (Λth) and the measured refractive index (Λn). The UV-cutoff shifts toward higher wavelengths with increasing optical basicity and lead content. In borate glasses, the frequency of the stretching modes due to nonbridging oxygen atoms of trigonal metaborate species is identified to be inversely proportional to the excitation wavelength (directly proportional to the excitation energy) of Pb2+. Lead-containing alkali and alkaline-earth borate glasses show additional correlations between the Pb2+ emission wavelength and the weighted average of the field strength of the modifier(s). Complementary to the investigation of optical properties, radiation and neutron shielding parameters were calculated, suggesting the potential utility of some of the studied compositions for radiation shielding applications.

采用熔融淬火法制备了含铅碱/碱土硼酸盐和磷酸铅钡玻璃,并对Pb2+离子的光学性质进行了详细的研究。紫外-可见吸收光谱和光致发光光谱揭示了Pb2+ s-p跃迁的变化,这与硼酸盐和磷酸盐中主体玻璃的光学碱度有关。硼酸盐和磷酸盐玻璃的Pb2+发射明显不同,因为可容纳Pb2+阳离子的带电位点的性质不同。光学碱度值由组成(Λth)和测量的折射率(Λn)确定。随着光学碱度和铅含量的增加,紫外截止向更高波长偏移。在硼酸盐玻璃中,由三角偏硼酸盐非桥接氧原子引起的拉伸模式的频率与Pb2+的激发波长成反比(与激发能成正比)。含铅碱硼酸盐玻璃和碱土硼酸盐玻璃显示出Pb2+发射波长与改性剂场强加权平均值之间的额外相关性。除了光学性质的研究外,还计算了辐射和中子屏蔽参数,表明所研究的一些成分在辐射屏蔽应用中的潜在效用。
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引用次数: 0
Structural, thermal and DC conductivity properties of WO 3 –P 2 O 5 glasses doped with B 2 O 3 掺b2o3的wo3 - p2o5玻璃的结构、热性能和直流电导率
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2022-11-30 DOI: 10.1111/ijag.16620
Pershina Svetlana
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引用次数: 0
Structural, thermal, and DC conductivity properties of WO3–P2O5 glasses doped with B2O3 掺杂B2O3的WO3–P2O5玻璃的结构、热和直流导电性能
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2022-11-30 DOI: 10.1111/ijag.16620
Svetlana V. Pershina

In this study, glasses in composition 70WO3–(30 − х)P2O5хB2O3 (0 ≤ х ≤ 20 mol%) were prepared by melt quenching method. The glass formation, structure, and thermal and electrical properties are discussed. Homogeneous glasses were obtained at x = 0–10 mol% B2O3, whereas glasses with x = 15 and 20 contain microinclusions of WO3. The glass transition temperature decreases from 709 to 531.6°C with increasing B2O3 content, as well as the crystallization temperature and the thermal stability. The structure of the glasses was studied by Raman spectroscopy and infrared spectroscopy. The Raman spectra are characterized by a band near 995 cm−1, a broad band at 788–800 cm−1, and a band near 675 cm−1 ascribed to vibrations of W–O–P, W–O–W, and P–O–B bonds, respectively. The Fourier-transform infrared spectra show vibrational bands due to characteristic phosphate and borate groups. Tetrahedral BO4 units prevail in the structural network. The electrical conductivity of the glasses decreased with x content due to the growth of WO3-deficient regions.

在本研究中,通过熔融淬火方法制备了成分为70WO3–(30−х)P2O5–хB2O3(0≤х≤20 mol%)的玻璃。讨论了玻璃的形成、结构、热性能和电学性能。在x=0–10 mol%的B2O3下获得了均匀的玻璃,而x=15和20的玻璃含有WO3的微团簇。随着B2O3含量、结晶温度和热稳定性的增加,玻璃化转变温度从709℃降至531.6℃。通过拉曼光谱和红外光谱研究了玻璃的结构。拉曼光谱的特征是995 cm−1附近的一条带,788–800 cm−1处的一条宽带,以及675 cm−2附近的一个带,分别归因于W–O–P、W–O-W和P–O–B键的振动。傅立叶变换红外光谱显示了由于特征性的磷酸盐和硼酸盐基团而产生的振动带。四面体BO4单元在结构网络中占主导地位。由于WO3缺陷区域的生长,玻璃的电导率随着x含量的增加而降低。
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引用次数: 0
Evaluation of nuclear transmutation effects due to beta decay on borosilicate glasses 硼硅酸盐玻璃β衰变核嬗变效应的评价
IF 2.1 3区 材料科学 Q2 Materials Science Pub Date : 2022-11-20 DOI: 10.1111/ijag.16619
Fan Yang, Shikun Zhu, Xu Chen, Jiangjiang Mao, Peng Lv, Haibo Peng, Tieshan Wang

In the study of deep geological disposal of high-level radioactive waste (HLW), beta decay has been widely studied, whereas the nuclear transmutation effects due to beta decay on vitrification are generally neglected. In this work, a series of sodium borosilicate glasses doped with cesium was fabricated. The nuclear transmutation due to beta decay evolving with the deposited time was simulated by substituting for cesium with barium. The macroscopic properties of the glasses, including density, hardness, and Young's modulus, were measured using the Archimedes (buoyancy) method and nanoindentation, respectively. The microscopic structures of the glasses were characterized by grazing incident X-ray diffraction, infrared spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, and Raman spectroscopy. The nuclear transmutation effects were significant. With the substitution of barium for cesium, the density, hardness, and modulus of the glasses increased and eventually tended to saturation. A decrease of [BO3] units and an increase of [BO4] units were observed in the infrared spectra and NMR spectra. In addition, the results were systematically compared to previous strontium-doping work in order to evaluate nuclear transmutation effects due to beta decay on vitrification in HLW comprehensively. The comparison demonstrated that the nuclear transmutation effect of cesium is completely opposite to that of strontium. The research is expected to contribute to a deeper understanding on the nuclear transmutation effects due to beta decay in HLW on vitrification.

在高放废物的深层地质处置研究中,β衰变得到了广泛的研究,而β衰变对玻璃化的核嬗变效应通常被忽视。在本工作中,制备了一系列掺铯硼硅酸钠玻璃。用钡代替铯,模拟了β衰变随沉积时间演变的核嬗变。分别用阿基米德(浮力)法和纳米压痕法测量了玻璃的宏观性能,包括密度、硬度和杨氏模量。用掠入射x射线衍射、红外光谱、核磁共振光谱和拉曼光谱对玻璃的微观结构进行了表征。核嬗变效应显著。随着钡取代铯,玻璃的密度、硬度和模量增加,最终趋于饱和。红外光谱和核磁共振光谱显示[BO3]单位减少,[BO4]单位增加。此外,为了全面评价β衰变对高浓缩铀玻璃化的核嬗变影响,将结果与以往的锶掺杂工作进行了系统的比较。对比表明,铯的核嬗变效应与锶的完全相反。本研究将有助于更深入地了解高浓缩铀中β衰变对玻璃化的核嬗变效应。
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引用次数: 0
期刊
International Journal of Applied Glass Science
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