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Linear volumetric additive manufacturing of zirconia from a transparent photopolymerizable ceramic slurry via Xolography 通过 Xolography 从透明的可光聚合陶瓷浆料中线性增材制造氧化锆
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-10 DOI: 10.1016/j.oceram.2024.100655
J.C. Sänger , N.F. König , A. De Marzi , A. Zocca , G. Franchin , R. Bermejo , P. Colombo , J. Günster

Advanced ceramics printed with photon-based additive manufacturing deals with anisotropic mechanical properties from the layer-by-layer manufacturing. Motivated by the success in using highly filled transparent slurries containing nanoparticles for powder-based two-photon-polymerization (2PP) for advanced ceramic printing, this works approach is the transfer to Xolography, a volumetric additive manufacturing technology based on linear two-photon excitation and without recoating steps. This paper reports the results of a preliminary investigation optimizing the photocurable slurry to the requirements of Xolography in terms of transparency, over a significantly larger mean free path, compared to 2PP. A feedstock filled with 70 % weight fraction of ceramic particles (∼30 vol%) exhibiting an exceptionally high degree of transparency in the relevant wavelength range of 400–800 nm was prepared from 5 nm zirconia nanoparticles. The high transparency of the photocurable slurry is attributed to the near-monomodal particle size distribution of the zirconia nanoparticles used.

用基于光子的增材制造技术打印的先进陶瓷,在逐层制造过程中会产生各向异性的机械特性。在基于粉末的双光子聚合(2PP)技术中使用含有纳米颗粒的高填充透明浆料进行先进陶瓷打印取得了成功,受此激励,这种工作方法被转移到了基于线性双光子激发且无需再涂层步骤的体积增材制造技术--Xolography。本文报告了一项初步调查的结果,即优化光固化浆料,以满足 Xolography 在透明度方面的要求,与 2PP 相比,平均自由路径要大得多。从 5 纳米氧化锆纳米颗粒中制备出了一种原料,其中填充了 70% 重量分数的陶瓷颗粒(∼30 vol%),在 400-800 纳米的相关波长范围内具有极高的透明度。光固化浆料的高透明度归功于所使用的氧化锆纳米粒子近似于均一的粒度分布。
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引用次数: 0
Effect of increased intra-bundle spacing on mechanical behaviour of Cf- ZrB2–SiC ultra-high temperature ceramic matrix composites produced by slurry infiltration and hot pressing 增加束内间距对浆渗和热压法生产的 Cf- ZrB2-SiC 超高温陶瓷基复合材料力学性能的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-10 DOI: 10.1016/j.oceram.2024.100656
Adarsha Ranjan Mishra , Vajinder Singh , Manish Patel , Rahul Mitra

A study has been carried out to examine the influence of augmented intra-bundle spacing achieved through innovative pre-treatment (heat treatment or ultrasonication) of carbon fibre (Cf) fabric, on mechanical properties of Cf-ZrB2-SiC composites processed by ZrB2–SiC slurry infiltration and hot pressing. Significantly enhanced Cf fabric intra-bundle spacing has facilitated homogeneous slurry infiltration, but has lowered elastic modulus, flexural strength, and fracture toughness compared to the composite with as-received Cf, because of fibre disorientation introduced during pre-treatment and its partial degradation by formation of interfacial ZrC during sintering. Notably, the composite with heat-treated Cf has shown superior fracture toughness (7.78 ± 0.4 MPa√m) and work of fracture (3043.25 ± 24.2 J/m2) compared to that containing ultra-sonicated Cf by 52.5 % and 95.7 %, respectively. Despite these variations, all the composites have exhibited non-catastrophic fracture behaviour during testing owing to the role of fibre pull-out, crack bridging, and crack deflection operating as toughening mechanisms.

本研究通过对碳纤维(Cf)织物进行创新性预处理(热处理或超声波处理),考察了增强束内间距对采用 ZrB2-SiC 浆料浸润和热压工艺加工的 Cf-ZrB2-SiC 复合材料机械性能的影响。Cf 织物束内间距的显著增加促进了浆料的均匀浸润,但与采用 Cf 的复合材料相比,弹性模量、抗弯强度和断裂韧性都有所降低,原因是纤维在预处理过程中发生了取向紊乱,并在烧结过程中因界面 ZrC 的形成而发生部分降解。值得注意的是,与含超声波 Cf 的复合材料相比,含热处理 Cf 的复合材料的断裂韧性(7.78 ± 0.4 MPa√m)和断裂功(3043.25 ± 24.2 J/m2)分别提高了 52.5% 和 95.7%。尽管存在这些差异,但由于纤维拉出、裂纹桥接和裂纹挠曲等增韧机制的作用,所有复合材料在测试过程中均表现出非灾难性断裂行为。
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引用次数: 0
Preparation and characterization of YAG microspheres doped with Eu2+/Eu3+ for broad band emission 用于宽带发射的掺杂 Eu2+/Eu3+ 的 YAG 微球的制备与表征
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-07 DOI: 10.1016/j.oceram.2024.100654
Marzieh Ghadamyari , Róbert Klement , Hossein Ebrahim Hosseini , Milan Parchovianský , Jozef Kraxner , Dušan Galusek , Sathya Narayanasamy , Erwin Hack , Gurdial Blugan , Monika Michálková

Achieving full-spectrum lighting is a major challenge for phosphor-converted light-emitting diodes (pc-LEDs), which are crucial for solid-state lighting. This study presents the synthesis of polycrystalline Eu-doped Y3Al5O12 (YAG) phosphors through a sol-gel method and flame synthesis process, leading to XRD amorphous microspheres. The amorphous nature of the microspheres allows the reduction of Eu3+ to Eu2+ at a significantly lower temperature (800 °C) than the reduction of crystalline samples described in the literature (1400 °C). The presence of Eu2+ in the YAG lattice was confirmed by X-ray photoelectron spectroscopy (XPS). The X-ray diffraction (XRD) of samples annealed in reducing atmosphere confirmed partial crystallization of pure YAG in all examined samples. The Eu-doped YAG phosphor embedded in residual glass microspheres exhibited a broadband emission spectrum over the wavelength range 450–800 nm peaking at 565 nm, corresponding to the 4f65d1→ 4f7 electron transition within the Eu2+ ions.

实现全光谱照明是荧光粉转换发光二极管(pc-LED)的一大挑战,而荧光粉转换发光二极管对固态照明至关重要。本研究介绍了通过溶胶-凝胶法和火焰合成工艺合成掺 Eu 的 Y3Al5O12 (YAG) 多晶荧光粉,从而得到 XRD 无定形微球。微球的无定形性质使得 Eu3+ 还原成 Eu2+ 的温度(800 °C)大大低于文献中描述的晶体样品的还原温度(1400 °C)。X 射线光电子能谱 (XPS) 证实了 Eu2+ 存在于 YAG 晶格中。在还原气氛中退火的样品的 X 射线衍射 (XRD) 证实了所有检测样品中纯 YAG 的部分结晶。嵌入残留玻璃微球的掺 Eu YAG 荧光粉在 450-800 纳米波长范围内显示出宽带发射光谱,在 565 纳米波长处达到峰值,这与 Eu2+ 离子内的 4f65d1→ 4f7 电子转变相对应。
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引用次数: 0
A comparative assessment of thermal conductivity of functionally graded and equivalent non-graded ZrB2–B4C–SiC–LaB6 ultra-high-temperature ceramic composites 功能分级和等效非分级 ZrB2-B4C-SiC-LaB6 超高温陶瓷复合材料导热性的比较评估
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-06 DOI: 10.1016/j.oceram.2024.100653
Ajit Kumar Naik , Lava Kumar Pillari , Kyle Lessoway , Lukas Bichler , Tapas Laha , Siddhartha Roy

In this study, functionally graded ZrB2–B4C–SiC–LaB6 composite materials (FGMs) with potential applications in hypersonic aircraft thermal protection systems were fabricated using spark plasma sintering. A systematic study of the thermal conductivity of the FGM, the conductivity of respective FGM layers, and the equivalent non-graded composites, was performed from room temperature up to 450 °C. The results suggest that the thermal conductivity of the FGMs (in the through-thickness direction) and their equivalent non-graded composites ranged between 25 and 34.9 W/mK, which was ∼60 % less than ZrB2. While the overall thermal conductivity of the FGM and equivalent non-graded composites were similar, in the FGM, the topmost layer with high ZrB2-content displayed up to 245 % higher thermal conductivity than the bottom layer with high B4C content. A systematic comparison between experimentally determined conductivity and relevant thermal conductivity models was conducted.

本研究采用火花等离子烧结法制造了功能分级 ZrB2-B4C-SiC-LaB6 复合材料 (FGM),有望应用于高超音速飞机热防护系统。从室温到 450 °C,对 FGM 的热导率、各 FGM 层的热导率以及等效的非分级复合材料的热导率进行了系统研究。结果表明,烟气脱硫材料(通厚方向)及其等效无级复合材料的导热系数介于 25 到 34.9 W/mK 之间,比 ZrB2 低 60%。虽然 FGM 和等效无级复合材料的总体热导率相似,但在 FGM 中,ZrB2-含量高的最上层的热导率比 B4C 含量高的最下层高出 245%。实验测定的热导率与相关热导率模型进行了系统比较。
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引用次数: 0
Residues from beneficiation of granite in porcelain stoneware: Effects on technological properties 瓷质炻器中的花岗岩选矿残留物:对工艺性能的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-05 DOI: 10.1016/j.oceram.2024.100651
Chiara Molinari , Andreea Sima , Matteo Cavina , Guia Guarini , Sonia Conte , Stefania Albonetti , Enrique Sanchez , Eugeni Cañas , Michele Dondi , Chiara Zanelli

Granite extraction waste represents an interesting alternative material for porcelain stoneware production, but information on its influence presents several gaps. For this reason, two different wastes were selected: a coarser iron-rich material from magnetic separation and a finer one from conveyance and abatement systems. Both were physically and chemically characterized. Batches were formulated by partial substitution of feldspar and technological behaviour of bodies was assessed by simulating the industrial manufacture at laboratory scale. Tiles were shaped by uniaxial pressure and fired by fast firing in electric roller kiln. The effect of waste addition was evaluated during the whole production process. Fired samples were characterized in terms of technological properties, mineralogical composition and microstructure evolution. The formulation optimization reduces firing temperature getting commercial technological constraints. A further increase of finer waste content affects compaction and mechanical strength. The presence of micaceous particles after the firing process may act as cracks initiation.

花岗岩开采废料是陶瓷炻器生产的一种有趣的替代材料,但有关其影响的信息却存在一些空白。因此,我们选择了两种不同的废料:一种是磁选产生的较粗的富铁材料,另一种是输送和净化系统产生的较细的材料。这两种废料都具有物理和化学特征。通过部分替代长石配制了批次产品,并通过模拟实验室规模的工业生产评估了产品的技术性能。瓷砖通过单轴压力成型,并在电动辊道窑中快速烧制。在整个生产过程中,对添加废料的影响进行了评估。烧制的样品在工艺性能、矿物成分和微观结构演变方面都有特征。配方优化降低了焙烧温度,满足了商业技术要求。进一步增加较细废料的含量会影响压实度和机械强度。焙烧过程后微粒的存在可能会引发裂缝。
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引用次数: 0
Influence of layer thickness and exposure on mechanical properties of additively manufactured polymer-derived SiOC ceramics 层厚度和暴露对添加式制造的聚合物硅OC 陶瓷机械性能的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-08-03 DOI: 10.1016/j.oceram.2024.100652
Jason C. Young , Stephan A. Brinckmann , Ray S. Fertig III , Stephen P. Lynch , Carl P. Frick

One significant hurdle in additively manufacturing polymer-derived ceramics lies in reconciling the lower mechanical properties of additively manufactured parts compared to traditionally manufactured ceramics and PDCs. Here, a methodology is presented for evaluating the influence of layer thickness and exposure on polymer-derived ceramics within the constraints of commercially available software and hardware. Maximizing exposure within printable limitation of DLP processes, produced green bodies with the highest conversion, and resulted in improved pyrolysis outcomes, manufacturability, and most importantly ceramic strengths comparable to traditionally manufactured SiOC PDCs. Decreasing layer thickness and increasing total dwell time had a dramatic impact on mechanical properties, increasing flexural strength by more than 6x from 18 MPa at 100 μm layer thickness to 111 MPa at 10 μm layer thickness. Density of resultant ceramic also increased from 1.62 ± 0.03 g/cc to 2.3 ± 0.05 g/cc. This represented a large increase in mechanical strengths of PDCs produced via DLP in literature.

与传统制造的陶瓷和 PDC 相比,添加式制造的部件机械性能较低,这就给添加式制造聚合物衍生陶瓷带来了很大的障碍。本文介绍了在商用软件和硬件的限制下,评估层厚度和曝光对聚合物衍生陶瓷的影响的方法。在 DLP 工艺的可打印限制范围内最大限度地增加曝光量,可生产出转化率最高的绿色坯体,并改善热解结果和可制造性,最重要的是,陶瓷强度可与传统制造的 SiOC PDC 相媲美。减少层厚度和增加总停留时间对机械性能产生了巨大影响,使抗弯强度提高了 6 倍多,从层厚 100 μm 时的 18 MPa 提高到层厚 10 μm 时的 111 MPa。陶瓷的密度也从 1.62 ± 0.03 g/cc 增加到 2.3 ± 0.05 g/cc。这表明文献中通过 DLP 生产的 PDC 的机械强度大幅提高。
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引用次数: 0
Content of crystalline silica phases in porcelain stoneware 瓷质炻器中结晶二氧化硅相的含量
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-29 DOI: 10.1016/j.oceram.2024.100650
Chiara Molinari, Sonia Conte, Michele Dondi, Chiara Zanelli

Kitchen and bathroom countertop is a demanding application, where high aesthetic standards must combine with durability, ease of maintenance, and resistance to heat, stain, scratch and chipping. The hard materials and composites used for high-end countertops usually contain crystalline silica phases that can be inhaled by workers during drilling and cutting operations. The occurrence of silicosis and other respiratory diseases in machining workers makes it important to know exactly how much crystalline silica is present in countertop materials. This paper collects over 300 quantitative determinations of quartz and cristobalite in porcelain stoneware products and compare these contents with other countertop materials. The sum of crystalline silica phases in porcelain stoneware is on average 21 ± 5 % by weight (mostly quartz). This content is lower than granite (∼30 %) and much lower than engineered stone (∼90 %). Possible ways to reduce the amount of crystalline silica phases in ceramic slabs are overviewed and critically discussed.

厨房和浴室台面是一种要求很高的应用,必须将高美学标准与耐用性、易维护性、耐热性、抗污性、抗划伤性和抗崩角性结合起来。高端台面使用的硬质材料和复合材料通常含有结晶硅相,工人在钻孔和切割操作过程中可能会吸入这些物质。由于机械加工工人会患上矽肺病和其他呼吸道疾病,因此准确了解台面材料中的结晶二氧化硅含量非常重要。本文收集了 300 多份炻瓷产品中石英和菱锰矿的定量测定结果,并将这些含量与其他台面材料进行了比较。按重量计,瓷质炻器中结晶二氧化硅相的总和平均为 21 ± 5%(主要是石英)。这一含量低于花岗岩(∼30%),也远低于人造石(∼90%)。本文概述了减少陶瓷板中结晶二氧化硅相的可能方法,并对其进行了深入讨论。
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引用次数: 0
Investigations on the processing of ceramic materials using Fused Filament Fabrication 利用熔融长丝制造技术加工陶瓷材料的研究
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-29 DOI: 10.1016/j.oceram.2024.100649
Toni Wille , Andreas Hopf , Michel Layher , Jens Bliedtner , Albert Kerber , Lucas Bloß

This paper represents the current status of the investigation into the processing of ceramic components, using Fused Filament Fabrication (“FFF”). The process chain, beginning from the additive manufacturing (“AM”), through the post processing, the debinding and sintering procedure, to the finished part is described. The examined materials are silicon nitride (Si3N4) and silicon carbide (SSiC), prepared by the company SiCeram/Qsil. Furthermore, comprehensive investigations on the materials are done, both in the green and in the sintered state. In addition, sources of occurring problems and defects in the process chain are pointed out and possible solutions are shown. Finally, the current status of investigations, regarding to the transfer into the industry, is discussed.

本文介绍了利用熔融长丝制造技术("FFF")加工陶瓷部件的研究现状。本文介绍了从增材制造("AM")开始,到后处理、排胶和烧结程序,再到成品部件的工艺链。研究的材料是氮化硅(Si3N4)和碳化硅(SSiC),由 SiCeram/Qsil 公司制备。此外,还对材料的生坯和烧结状态进行了全面研究。此外,还指出了工艺链中出现问题和缺陷的根源,并提出了可能的解决方案。最后,还讨论了有关向工业转化的研究现状。
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引用次数: 0
Assessment of geometrical variability in 3D printed ZrO2: Effects of printing and thermal post-processing 评估 3D 打印氧化锆的几何变异性:打印和热后处理的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-26 DOI: 10.1016/j.oceram.2024.100629
Erik Kornfellner , Filip Jelínek , Laszlo Jaksa , Anna Lebhard , Daniel Bomze , Martin Schwentenwein , Francesco Moscato

3D printing is developing rapidly and enables the production of parts manufactured using different materials. These includes zirconium dioxide (ZrO2), which can be of particular interest for bone tissue engineering and implantology. However, highly accurate part-dimensions are a must for these applications, which is why this study addresses geometrical deviations which occur during the printing process and thermal post-processing.

Six sets of test geometries with 50 individual features were 3D printed with two different ZrO2 slurries (3 mol% yttria-stabilized ZrO2) and scanned with a profilometer. After debinding and sintering, the profilometer scan was repeated and the deviations and shrinkage factors were determined.

A notable difference is observed when the same ceramic is processed using two different slurries. For instance, one used ceramic slurry, LithaCon 210, exhibits shrinkage factors of shrXY=21.2±3.4% (n=78) and shrZ=23.6±0.54% (n=24) for protruding structures, while the other ceramic slurry, LithaCon 280, shows shrinkage factors of shrXY=21.7±3.3% (n=78) and shrZ=24.5±0.55% (n=24).

Geometric deviations differed for intruding (like holes and slots) and protruding (like pillars) geometries, being more pronounced in case of intruding geometries, especially where printing overhangs occur.

Although the shrinkage during sintering needs further investigation, these experimental findings are a good starting point to validate and refine simulation models for shrinkage and improve production processes of 3D printed ceramics.

三维打印技术发展迅速,能够生产使用不同材料制造的部件。其中包括二氧化锆(ZrO2),它对骨组织工程学和植入学具有特殊意义。使用两种不同的二氧化锆浆料(3 mol% 的钇稳定二氧化锆)3D 打印了六组测试几何图形,共 50 个独立特征,并使用轮廓仪进行了扫描。去胶和烧结后,重复轮廓仪扫描,并确定偏差和收缩因子。例如,一种使用的陶瓷浆料 LithaCon 210 在突出结构上的收缩因子为 shrXY=21.2±3.4% (n=78)和 shrZ=23.6±0.54% (n=24),而另一种陶瓷浆料 LithaCon 280 的收缩因子为 shrXY=21.7±3.3% (n=78)和 shrZ=24.5±0.55% (n=24)。虽然烧结过程中的收缩率还需要进一步研究,但这些实验结果是验证和完善收缩率模拟模型以及改进 3D 打印陶瓷生产工艺的良好起点。
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引用次数: 0
Solar salt encapsulated into 3D printed activated carbon/alumina supports for thermal energy storage applications 将太阳能盐封装到 3D 打印活性炭/氧化铝支架中,用于热能储存应用
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-26 DOI: 10.1016/j.oceram.2024.100648
Irene Díaz-Herrezuelo , Quentin Falcoz , Audrey Soum-Glaude , Manuel Belmonte

The encapsulation of phase change materials (PCMs) into additive manufactured porous supports is attracting great interest for developing thermal energy storage (TES) materials with improved energy performance. Here, highly porous (86 %) self-supported 3D activated carbon/alumina supports are fabricated by direct ink writing (DIW) and, then, infiltrated with solar salt, a highly corrosive PCM with a melting temperature around 220 °C commonly employed in concentrated solar power plants. This novel, robust, chemically compatible, and lightweight infiltrated 3DTES exhibits good thermal energy storage efficiency (70 %) and thermal stability, high energy storage density (381 J g−1), and avoids the liquid leakage of the molten salt. Besides, the 3D activated carbon/alumina support promotes a better ability to absorb solar energy (79 %) and enhances the thermal conductivity of the solar salt (up to 64 %). These results validate the use of DIW for manufacturing innovative TES with an enhanced energy storage behaviour.

将相变材料(PCM)封装到添加剂制造的多孔支撑物中,对于开发具有更高能量性能的热能储存(TES)材料,正引起人们的极大兴趣。在这里,通过直接墨水写入(DIW)技术制造出了高孔隙率(86%)的自支撑三维活性炭/氧化铝支撑物,然后将太阳盐渗入其中,太阳盐是一种高腐蚀性 PCM,熔化温度约为 220 °C,通常用于聚光太阳能发电厂。这种新型、坚固、化学相容性好且重量轻的浸润式 3DTES 具有良好的热能储存效率(70%)和热稳定性,能量储存密度高(381 J g-1),并避免了熔盐的液体泄漏。此外,三维活性炭/氧化铝支架还提高了吸收太阳能的能力(79%),并增强了太阳能盐的热导率(高达 64%)。这些结果验证了利用 DIW 制造创新型 TES 的可行性,这种 TES 具有更强的储能性能。
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引用次数: 0
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Open Ceramics
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