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Synthesis of titanium carbide (TiC) using recycled precursor for potential scale-up of low-cost MXene 利用再生前驱体合成碳化钛 (TiC),有望扩大低成本 MXene 的规模
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-05 DOI: 10.1016/j.oceram.2024.100637
M.A. Zaed , R. Saidur , K.H. Tan , Jayesh Cherusseri , A.K. Pandey , N. Abdullah , Nurul Atiqah Izzati Md Ishak

In this study, we report the low-cost synthesis of titanium carbide (TiC) from recycled precursors and further used to synthesize MAX phase material, Ti3AlC2. The recycled precursor, carbon extracted from the used tyres using a few processes is used to synthesize TiC with high purity. The use of tyre-derived carbon offers several environmental benefits such as facile synthesis, low cost, environment-friendly, etc. The as-synthesized TiC is further used as a precursor to synthesize low-cost Ti3AlC2. The structure of TiC and Ti3AlC2 are characterized by UV–visible spectroscopy and X-ray diffraction analysis. The microstructure and surface morphology of the samples are examined using scanning electron microscope imaging and energy-dispersive X-ray spectroscopy. The chemical bonding information is analyzed by Fourier transform infrared spectroscopy and the thermal behaviour of the samples are examined using thermogravimetric analysis. The successful cost-effective synthesis of TiC and Ti3AlC2 are confirmed from XRD analysis and the samples show high purity. TiC and Ti3AlC2 show excellent thermal stability which helps in their potential applications in the future. This study proclaims a new strategy to synthesize low-cost Ti3AlC2 MXene for the large-scale production using TiC precursor where the TiC precursor is synthesized using carbon precursor.

在本研究中,我们报告了利用回收前驱体低成本合成碳化钛(TiC),并进一步用于合成 MAX 相材料 Ti3AlC2 的情况。从废旧轮胎中提取的回收前驱体碳只需几道工序就能合成高纯度的 TiC。使用从轮胎中提取的碳具有多种环境优势,如合成简便、成本低廉、环境友好等。合成的 TiC 可进一步用作合成低成本 Ti3AlC2 的前驱体。通过紫外可见光谱和 X 射线衍射分析对 TiC 和 Ti3AlC2 的结构进行了表征。利用扫描电子显微镜成像和能量色散 X 射线光谱分析了样品的微观结构和表面形态。傅立叶变换红外光谱分析了化学键信息,热重分析则检验了样品的热行为。XRD 分析证实了 TiC 和 Ti3AlC2 的成功合成具有成本效益,而且样品纯度很高。TiC 和 Ti3AlC2 表现出卓越的热稳定性,这有助于它们在未来的潜在应用。本研究提出了一种利用 TiC 前驱体合成低成本 Ti3AlC2 MXene 以用于大规模生产的新策略,其中 TiC 前驱体是利用碳前驱体合成的。
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引用次数: 0
Predicting hardness of graphene-added Si3N4 using machine learning: A data-driven approach 利用机器学习预测添加石墨烯的 Si3N4 的硬度:数据驱动法
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-05 DOI: 10.1016/j.oceram.2024.100634
Awais Qadir , Shoaib Ali , Jan Dusza , David Rafaja

This study presents a data-driven framework based on machine learning (ML) using extreme gradient boosting (XGBoost) for predicting the hardness of silicon nitride (Si3N4) ceramics reinforced with graphene. The XGBoost model takes into account various factors such as graphene type and content, characteristics of the raw Si3N4 powder, the parameters of the sintering process (sintering technique, temperature, pressure, holding time), and the characteristics of the sintered samples, i.e., the density, αβ content and Vickers hardness. The parameters that influence the Si3N4 hardness most strongly are identified, with sintering pressure, sintering time and density being the most influential. The addition of graphene content up to a certain threshold (1 wt%) has a positive impact on hardness. However, beyond that it leads to a lower density and a lower mechanical performance. Sintering parameters, particularly the sintering pressure, temperature, holding time and technique, strongly affect the density, final grain size, αβ Si3N4 composition and subsequently the hardness. The study highlights the importance of density and the densification process in achieving high hardness in Si3N4 ceramics. The developed ML model provides a valuable tool for predicting the hardness of Si3N4+graphene ceramics composites and offers insights into selecting suitable graphene type, content, and processing parameters. While the study primarily focuses on Si3N4+graphene composites, this novel approach holds promise for the in-silico design and analysis of diverse ceramic materials.

本研究提出了一种基于机器学习(ML)的数据驱动框架,使用极端梯度提升(XGBoost)技术预测使用石墨烯增强的氮化硅(Si3N4)陶瓷的硬度。XGBoost 模型考虑了各种因素,如石墨烯的类型和含量、Si3N4 原粉的特性、烧结工艺参数(烧结技术、温度、压力、保温时间)以及烧结样品的特性,即密度、αβ 含量和维氏硬度。确定了对 Si3N4 硬度影响最大的参数,其中影响最大的是烧结压力、烧结时间和密度。石墨烯含量达到一定临界值(1 wt%)会对硬度产生积极影响。然而,超过这一限度后,密度会降低,机械性能也会降低。烧结参数,尤其是烧结压力、温度、保温时间和技术,对密度、最终晶粒大小、αβ Si3N4 成分以及随后的硬度都有很大影响。这项研究强调了密度和致密化过程对实现 Si3N4 陶瓷高硬度的重要性。所开发的 ML 模型为预测 Si3N4+ 石墨烯陶瓷复合材料的硬度提供了有价值的工具,并为选择合适的石墨烯类型、含量和加工参数提供了见解。虽然这项研究主要侧重于 Si3N4+ 石墨烯复合材料,但这种新方法有望用于各种陶瓷材料的硅内设计和分析。
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引用次数: 0
Boron induced abnormal grain growth in alumina 硼诱导氧化铝中的异常晶粒生长
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-04 DOI: 10.1016/j.oceram.2024.100636
Christian Bechteler , Hannes Kühl , Richard I. Todd

In this work, hot-pressing of alumina in contact with hexagonal boron nitride or doped with boron carbide was conducted at 1500 °C for 30 min. After hot-pressing, abnormal grain growth induced by boron diffusion from these substances into alumina was detected, as clearly demonstrated with SEM, EDS, EBSD, and Raman spectroscopy. Grain boundary complexion transformations, solute drag, or another mechanism relating to interface-controlled grain boundary mobility are presumed to be the fundamental mechanism responsible for abnormal grain growth observed in this work.

在这项工作中,在 1500 °C 下对接触六方氮化硼或掺杂碳化硼的氧化铝进行了 30 分钟的热压。热压后,检测到硼从这些物质扩散到氧化铝中引起的异常晶粒生长,这一点在 SEM、EDS、EBSD 和拉曼光谱中都有清楚的证明。据推测,晶界复合转化、溶质拖曳或与界面控制晶界流动性有关的其他机制是导致本研究中观察到的异常晶粒生长的基本机制。
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引用次数: 0
Effect of Nb2O5 doping on low-temperature sintering of TiO2-Al2O3 ceramics 掺杂 Nb2O5 对 TiO2-Al2O3 陶瓷低温烧结的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-07-03 DOI: 10.1016/j.oceram.2024.100635
Huei-Jyun Shih , Ying-Chieh Lee , Yu-De Li , Chang-Ting Yang

This study investigates the effects of Nb2O5 as a dopant in TiO2–Al2O3 ceramics to lower sintering temperature and enhance performance, including the physical, mechanical, and dielectric properties of the ceramics at sintering temperatures 1250 °C–1350 °C. Specifically, TiO2–Al2O3 ceramics doped with 1.5 wt% Nb2O5 and sintered at 1350 °C exhibit remarkable density 94 %, compressive strength 1372 MPa, and abrasion resistance 1.36 × 10−4 mm3/N·m, surpassing those of pure alumina ceramics. This improvement is attributed to enhanced grain boundary diffusion and strain energy resulting from Nb5+ cation substitution. The incorporation of Nb2O5 in TiO2–Al2O3 ceramics reduce sintering temperatures by 150–200 °C. The dielectric constant of TiO2–Al2O3 ceramics doped with 1.5 wt% Nb2O5 sintered at 1350 °C is found to be 13.4, with a dielectric loss of 2.56 × 10−2 and insulation resistance 7.3 × 1012 Ω. Nb2O5 is an effective additive for reducing sintering temperatures in Al2O3 based ceramic.

本研究探讨了在 TiO2-Al2O3 陶瓷中掺杂 Nb2O5 对降低烧结温度和提高性能的影响,包括烧结温度为 1250 °C-1350 °C 时陶瓷的物理、机械和介电性质。具体来说,掺杂了 1.5 wt% Nb2O5 并在 1350 °C 下烧结的 TiO2-Al2O3 陶瓷显示出显著的密度 94 %、抗压强度 1372 MPa 和耐磨性 1.36 × 10-4 mm3/N-m,超过了纯氧化铝陶瓷。这种改善归因于 Nb5+ 阳离子替代增强了晶界扩散和应变能。在 TiO2-Al2O3 陶瓷中加入 Nb2O5 可使烧结温度降低 150-200 ℃。在 1350 ℃ 下烧结的掺有 1.5 wt% Nb2O5 的 TiO2-Al2O3 陶瓷的介电常数为 13.4,介电损耗为 2.56 × 10-2,绝缘电阻为 7.3 × 1012 Ω。
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引用次数: 0
“Hexacelsian slurry development for 2D woven alumina fiber impregnation in CMC fabrication” "用于 CMC 制造中二维编织氧化铝纤维浸渍的六元浆料开发"
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-29 DOI: 10.1016/j.oceram.2024.100633
Arnaud Saintonge , William Krikorian , James Braun , Alexandre Allemand , Thierry Piquero , Sophie Beaudet-Savignat , Yann Lepetitcorps

The rheological properties of BAS (BaAl2Si2O8) slurries are investigated in order to optimize the impregnation of an alumina preform to manufacture oxide/oxide composite materials. The fiber preform morphology has been deeply investigated, especially the fiber to fiber gap within tows and compared to the grain size of the matrix powder. The slurry viscosity is measured as a function of powder and organic additives concentration to find the best combination. The optimal combination is evaluated by different measurements including: zeta potential, sedimentation and wettability to verify the slurry behavior for the fibers infiltration. An aqueous slurry containing 20–25 vol% of BAS with 1 wt% of dispersing agent (Darvan 821-A™) improved the rheological properties for fibers infiltration. Finally, characterizations of the composite show a good infiltration in the fiber tows spaces and indicate a mean porosity of 37 vol%, including 9 vol% of macroporosity.

研究 BAS(BaAl2Si2O8)浆料的流变特性是为了优化氧化铝预型件的浸渍,以制造氧化物/氧化物复合材料。深入研究了纤维预型件的形态,特别是纤维束内纤维与纤维之间的间隙,并与基体粉末的粒度进行了比较。为找到最佳组合,测量了浆液粘度与粉末和有机添加剂浓度的函数关系。最佳组合通过不同的测量方法进行评估,包括:ZETA 电位、沉降和润湿性,以验证纤维渗透的浆液行为。含有 20-25 Vol% 的 BAS 和 1 wt% 的分散剂(Darvan 821-A™)的水性浆料改善了纤维浸润的流变特性。最后,复合材料的特性表明纤维束空间的浸润性良好,平均孔隙率为 37%,其中大孔隙率为 9%。
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引用次数: 0
Ceramic fused filament fabrication (CF3) of alumina: Influence of powder particle morphology on processing and microstructure 氧化铝陶瓷熔丝制造(CF3):粉末颗粒形态对加工和微观结构的影响
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-27 DOI: 10.1016/j.oceram.2024.100631
Kameswara Pavan Kumar Ajjarapu, Srimanta Barui, Kavish Sudan, Saleh Khanjar, Kunal Kate

This study investigates ceramic fused filament fabrication (CF3) 3D printing of alumina with an emphasis on the impact of particle morphology on feedstock preparation and printability. Spherical powder displayed superior flow with higher apparent density, tap density, and powder packing fraction compared to irregular powder. A 55 vol % powder loading was chosen to ensure good flowability during printing. Irregular powder-based feedstocks had 40X higher viscosity than spherical powder feedstocks at 400 s−1 shear rate, posing potential printing challenges. Slow printing speed maintained low feed-rates for consistent material flow. The debinding and sintering process produced macroscopically defect-free alumina components with relative densities above 89 % for both powder morphologies. The focus of the work is on comparing two different powder particle morphologies influencing feedstock behavior, printing fidelity, and sintered part properties.

本研究调查了氧化铝的陶瓷熔融长丝制造(CF3)三维打印技术,重点是颗粒形态对原料制备和可打印性的影响。与不规则粉末相比,球形粉末的流动性更好,表观密度、敲击密度和粉末堆积分数更高。为确保印刷过程中良好的流动性,选择了 55 Vol % 的粉末装载量。在 400 s-1 的剪切速率下,不规则粉末原料的粘度比球形粉末原料高 40 倍,这给印刷带来了潜在的挑战。低速印刷可保持较低的进料速度,从而保证材料的流动性。脱脂和烧结工艺可生产出宏观上无缺陷的氧化铝成分,两种粉末形态的相对密度均超过 89%。这项工作的重点是比较两种不同粉末颗粒形态对进料行为、印刷保真度和烧结部件性能的影响。
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引用次数: 0
Towards a debinding-free additive manufacturing of ceramics: A development perspective of water-based LSD and LIS technologies 实现陶瓷的无排胶增材制造:水基 LSD 和 LIS 技术的发展前景
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-27 DOI: 10.1016/j.oceram.2024.100632
Andrea Zocca , Jens Günster

Ceramic additive manufacturing (AM) requires a complex process chain with various post-processing steps that require expensive machines and special expertise. The key to further market penetration is AM that makes it possible to integrate into an already established ceramic process chain. Most successful AM technologies for ceramics are, however, based on processes that initially have been developed for polymeric materials. For ceramics AM, polymers or precursors are loaded with ceramic particles. This strategy facilitates the entry into AM, however the introduction of organic additives into the ceramic process chain represents a considerable technological challenge to ultimately obtain a ceramic component after additive shaping. In the present communication, two technologies based on ceramic suspensions will be introduced, the “layerwise slurry deposition” (LSD) and “laser induced slip casting” (LIS) technology. Both technologies take advantage of the high packing densities reached by conventional slip casting and moreover enable the processing of fines, even nanoparticles.

陶瓷增材制造(AM)需要一个复杂的工艺链,其中包括各种后加工步骤,需要昂贵的机器和特殊的专业知识。要想进一步打入市场,关键在于能将 AM 技术整合到已经建立的陶瓷工艺链中。然而,大多数成功的陶瓷 AM 技术都是基于最初为聚合物材料开发的工艺。在陶瓷自动成型技术中,聚合物或前驱体中加入了陶瓷颗粒。这种策略为进入 AM 领域提供了便利,但在陶瓷工艺链中引入有机添加剂对最终获得添加成型后的陶瓷部件是一个相当大的技术挑战。本文将介绍两种基于陶瓷悬浮液的技术,即 "分层浆料沉积"(LSD)和 "激光诱导滑移铸造"(LIS)技术。这两种技术都利用了传统滑模铸造所能达到的高堆积密度,而且还能加工细小颗粒,甚至是纳米颗粒。
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引用次数: 0
3D printing of multi-scale porous β-tricalcium phosphate scaffolds: Mechanical properties and degradation 多尺度多孔β磷酸三钙支架的三维打印:机械性能和降解
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-27 DOI: 10.1016/j.oceram.2024.100630
Shareen S.L. Chan , Daniel E. Heath , George V. Franks

Processing-structure-property relationships of 3D-printed multi-scale porous ceramics were investigated. Direct ink writing (DIW) of oil-templated colloidal pastes produced hierarchically porous beta-tricalcium phosphate (TCP) scaffolds. Print architecture and microporosity within filaments were varied, mimicking bone structure. The scaffolds exhibited 60–70 % porosity with interconnected macropores 300–700 μm and microporosity within the filaments at the 10 micron-scale. Varying surfactant and oil concentrations created two micro-pore morphologies – bubble-like pores (emulsion) and channel-like pores (capillary suspension). Emulsion scaffolds were stronger, stiffer and more reliable than capillary suspension scaffolds under both compression and bending. Reducing nozzle diameter and inter-filament distance improved strength and stiffness, at lower density. Immersed at physiological pH, the hierarchically porous TCP scaffolds' strength and modulus degraded at a moderate rate suitable for bone tissue engineering (BTE). Mechanical behavior can be controlled by manipulating process parameters which influence the material's structure. These properties were comparable with trabecular bone, promising for BTE.

研究了三维打印多尺度多孔陶瓷的加工-结构-性能关系。油性胶体浆料的直接墨水写入(DIW)产生了分层多孔的β-磷酸三钙(TCP)支架。打印结构和细丝内的微孔度各不相同,模拟了骨骼结构。支架的孔隙率为 60-70%,相互连接的大孔隙为 300-700 μm,细丝内的微孔为 10 微米级。不同浓度的表面活性剂和油会产生两种微孔形态--气泡状孔隙(乳液)和通道状孔隙(毛细悬浮液)。在压缩和弯曲条件下,乳液支架比毛细悬浮支架更坚固、更硬、更可靠。在密度较低的情况下,缩小喷嘴直径和纤维间距可提高强度和刚度。浸泡在生理 pH 值条件下,分层多孔 TCP 支架的强度和模量降解速度适中,适合骨组织工程(BTE)。机械行为可通过调节影响材料结构的工艺参数来控制。这些特性与骨小梁相当,有望用于 BTE。
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引用次数: 0
SiC-bonded diamond material with excellent abrasive wear resistance 碳化硅结合剂金刚石材料具有出色的耐磨性
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-26 DOI: 10.1016/j.oceram.2024.100627
Steffen Kunze, Björn Matthey, Mathias Herrmann

The wear behavior of SiC bonded diamond materials produced by liquid silicon infiltration in diamond preforms was investigated. The wear behavior in sand blasting tests (SiC abrasives, 5 bar pressure) was correlated with the microstructure. All SiC bonded diamond materials showed a wear, which was approximately 10 times less than the wear behavior of the reference SiC material.

Systematic changed microstructures were created by increasing the infiltration temperature. As the infiltration temperature increases, a graphite layer is formed at the diamond-SiC interface. At the highest infiltration temperature (1670 °C), the layer thickness reaches approx. 580 nm. The results show that wear resistance is not negatively affected by the graphite layer. On the contrary, for materials with a graphite layer thickness of up to 70 nm, the wear resistance increases by up to 30 %. The wear increases again only at the highest infiltration temperature. However, this is probably caused more by the internal damage to the diamonds and not by the graphite layer at the interface.

研究了通过在金刚石预型件中渗入液态硅而制成的碳化硅结合金刚石材料的磨损行为。喷砂测试(SiC 磨料,5 巴压力)中的磨损行为与微观结构相关。所有与碳化硅结合的金刚石材料都出现了磨损,磨损程度大约是碳化硅参考材料的 10 倍。随着浸润温度的升高,金刚石-碳化硅界面上形成了石墨层。在最高渗入温度(1670 °C)下,石墨层厚度达到约 580 nm。结果表明,石墨层不会对耐磨性产生负面影响。相反,对于石墨层厚度达 70 nm 的材料,耐磨性最多可增加 30%。只有在最高渗透温度下,磨损才会再次增加。不过,这可能更多是由金刚石的内部损坏造成的,而不是由界面上的石墨层造成的。
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引用次数: 0
Ceramic additive manufacturing and microstructural analysis of tricalcium phosphate implants using X-ray microcomputed tomography 利用 X 射线微计算机断层扫描技术进行陶瓷快速成型和磷酸三钙植入物的微结构分析
IF 2.9 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-06-26 DOI: 10.1016/j.oceram.2024.100628
Sascha Senck , Jonathan Glinz , Sarah Heupl , Johann Kastner , Klemens Trieb , Uwe Scheithauer , Sif Sofie Dahl , Martin Bonde Jensen

Additive manufacturing (AM) of ceramic bone implants from tricalcium phosphate (TCP) offers several benefits for bone regeneration and defect treatment. TCP scaffolds, e.g. featuring lattice or gyroid geometries, can effectively induce bone ingrowth and integration, showing a high potential in the treatment of large bone defects, e.g. as filler material for large bone defects. A major advantage of TCP is its osteoconductivity making it an effective choice for a broad range of orthopedic and dental applications. In addition, AM allows for the possibility to create precise, patient-specific implants with controllable mechanical properties. Those properties can be controlled by the implants' microstructure, e.g. in relation to bulk density and internal porosity. In this contribution, eleven resorbable bone implants were produced from β-tricalcium phosphate (β-TCP) in order to quantify the internal porosity in three dimensions using microcomputed tomography (μ CT). All components were manufactured using an extrusion-based process and scanned using an industrial μCT system at a voxel size of 10 μm. Two samples were physically prepared to allow a high-resolution μCT analysis at a voxel size of 1 μm. Results show that post-processed image data enables the non-destructive inspection of highly complex ceramic AM implants. Using μCT we were able to quantify internal porosity in β-TCP bone implant and quantify the geometry and distribution of wall thicknesses in the gyroid geometry. However, a detailed microstructural analysis is only possible using high-resolution μCT volume data, e.g. in relation to internal porosity. The findings emphasize that ceramic AM is able to produce complex components. However, NDT using μCT is crucial in the development of new materials and geometries. μCT provides high-resolution insights into the internal and external structure of ceramic AM components. It plays a critical role in detecting internal features, including small-scale porosity and delamination which are crucial for the integrity and functionality of medical implants. Moreover, μCT provides volumetric data that supports the design and manufacturing process at various stages, enabling an iterative approach of continuous improvement in mechanical performance and osseointegration.

利用磷酸三钙(TCP)对陶瓷骨植入物进行增材制造(AM)可为骨再生和骨缺损治疗带来多种益处。具有晶格或陀螺几何形状等特点的 TCP 支架可有效诱导骨的生长和整合,在治疗大面积骨缺损(如作为大面积骨缺损的填充材料)方面显示出巨大潜力。TCP 的一个主要优势是其骨传导性,这使其成为骨科和牙科广泛应用的有效选择。此外,AM 还能制造出具有可控机械性能的精确的患者专用植入体。这些特性可以通过植入物的微观结构来控制,例如与体积密度和内部孔隙率有关的微观结构。在这篇论文中,我们用β-磷酸三钙(β-TCP)制作了 11 个可吸收骨植入体,以便使用微计算机断层扫描(μ CT)对内部孔隙率进行三维量化。所有部件均采用挤压工艺制造,并使用工业级 μCT 系统进行扫描,体素尺寸为 10 μm。对两个样品进行了物理制备,以便以 1 μm 的体素尺寸进行高分辨率 μCT 分析。结果表明,经过后处理的图像数据可以对高度复杂的陶瓷 AM 植入物进行无损检测。利用μCT,我们能够量化β-TCP骨植入物的内部孔隙率,并量化陀螺几何形状中的几何形状和壁厚分布。不过,只有使用高分辨率的μCT体积数据才能进行详细的微观结构分析,例如与内部孔隙率有关的分析。研究结果表明,陶瓷 AM 能够生产复杂的部件。然而,使用 μCT 进行无损检测对新材料和新几何形状的开发至关重要。它在检测内部特征(包括对医疗植入物的完整性和功能至关重要的小尺度气孔和分层)方面发挥着关键作用。此外,μCT 还能提供体积数据,为不同阶段的设计和制造过程提供支持,从而采用迭代方法不断改进机械性能和骨结合性能。
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引用次数: 0
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