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Synergistic effects of hydroxyapatite and graphene nanoplatelets on mechanical, corrosion, and biocompatibility of pure magnesium 羟基磷灰石和石墨烯纳米片对纯镁的机械、腐蚀和生物相容性的协同效应
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-06 DOI: 10.1016/j.ceramint.2025.12.517
Shahrukh Abid , Ching-Chi Hsu , Song-Jeng Huang , Punnoli Muhsin , Meng Ze Lin
Biodegradable magnesium (Mg) and its alloys are valued for their biocompatibility, mechanical properties, and natural degradability within the body. However, their susceptibility to rapid corrosion often surpasses tissue healing, undermining their mechanical integrity. This study explores hybrid magnesium-based composites reinforced with 0.7 wt% hydroxyapatite (HAP) and 0.1 wt% graphene nanoplatelets (GNPs), synthesized via the stir casting process. X-ray diffraction (XRD) confirmed the successful incorporation of the reinforcements, while microstructural analysis showed grain refinement resulting from the pinning effect of HAP and GNPs. Mechanical testing revealed substantial enhancements in tensile yield strength, ultimate tensile strength, and elongation, with improvements of 37.34 %, 34.95 %, and 15.54 % respectively, for the HAP-GNP-reinforced magnesium composites compared to pure magnesium. Additionally, the inclusion of HAP and GNPs significantly enhanced corrosion resistance by forming a protective barrier against aggressive corrosive agents. The hybrid composites exhibited enhanced biocompatibility under in vitro conditions, as evidenced by cell viability outcomes. Electrochemical analysis reveals a significantly lower corrosion rate for the MGNPHAP composite (0.25 mm/y) compared to the MHAP (0.49 mm/y) and PM (1.51 mm/y) samples. These properties coupled with controlled corrosion, demonstrate the potential of HAP-GNP reinforced magnesium composites as advanced biodegradable materials for orthopedic applications, offering an optimal balance of mechanical strength, biocompatibility, and controlled degradation.
可生物降解镁(Mg)及其合金因其生物相容性、机械性能和在体内的自然降解性而受到重视。然而,它们对快速腐蚀的敏感性往往超过组织愈合,破坏了它们的机械完整性。本研究探索了由0.7 wt%羟基磷灰石(HAP)和0.1 wt%石墨烯纳米片(GNPs)通过搅拌铸造工艺合成的杂化镁基复合材料。x射线衍射(XRD)证实了增强剂的成功结合,而显微组织分析表明HAP和GNPs的钉住作用导致了晶粒的细化。力学试验表明,与纯镁相比,hap - gnp增强镁复合材料的抗拉屈服强度、极限抗拉强度和伸长率分别提高了37.34%、34.95%和15.54%。此外,HAP和GNPs的加入通过形成对腐蚀性物质的保护屏障,显著提高了耐腐蚀性。在体外条件下,混合复合材料表现出增强的生物相容性,证明了细胞活力结果。电化学分析表明,与MHAP (0.49 mm/y)和PM (1.51 mm/y)样品相比,MGNPHAP复合材料(0.25 mm/y)的腐蚀速率显著降低。这些性能加上可控腐蚀,证明了HAP-GNP增强镁复合材料作为骨科应用的先进生物降解材料的潜力,提供了机械强度、生物相容性和可控降解的最佳平衡。
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引用次数: 0
Structural, morphological and radiation shielding performance of rare-earth pyrochlores against gamma rays and neutrons: A comparative study of Gd2Ti2O7, Gd2TiZrO7, Gd2Zr2O7, Eu2Zr2O7, Sm2Zr2O7 and Nd2Zr2O7 稀土烧绿石对γ射线和中子的结构、形态和辐射屏蔽性能:Gd2Ti2O7、Gd2TiZrO7、Gd2Zr2O7、Eu2Zr2O7、Sm2Zr2O7和Nd2Zr2O7的比较研究
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2025-12-30 DOI: 10.1016/j.ceramint.2025.12.467
Yara Haddad , Morad Kh Hamad , Gael Sattonnay
In this work, six rare-earth pyrochlores ceramics were prepared using the conventional solid-state method to investigate their ionizing radiation shielding performance. X-ray diffraction (XRD) experiments were performed, and the diffraction patterns were analyzed by Rietveld refinement to confirm the phase purity and structural stability of the samples. Scanning electron microscopy (SEM) was employed to complement the structural characterization of the samples, revealing grain refinement and residual porosity with zirconium substitution. Different shielding parameters, including mass attenuation coefficient (μm), linear attenuation coefficient (μ), half-value layer (λ1/2), kinetic energy released per unit mass (KERMA) relative to air, transmission factor (TF%), radiation protection efficiency (RPE), and specific gamma-ray constant (Γ), were calculated across in the energy range of 15 keV to 15 MeV using the Phy-X software. For instance, μ hits 486.58 cm−1, 344.423 cm−1 at 15 keV for Gd2Ti2O7 and Nd2Zr2O7 respectively. Consistently, their λ1/2 thicknesses were as low as ∼0.002 cm, confirming their superior shielding efficiency in the region below 0.1 MeV. Around 0.5 MeV, radiation protection efficiency remained near 50 %. Among the studied systems, Gd2Ti2O7 consistently outperformed the others due to its higher gadolinium fraction and lower molar mass, which increased photon interaction probability per unit mass. The results revealed that our samples are strong candidates for applications in nuclear waste management, reactor safety, and medical radiation protection.
本文采用传统的固态法制备了6种稀土焦绿石陶瓷,研究了它们的电离辐射屏蔽性能。进行了x射线衍射(XRD)实验,并用Rietveld细化法对衍射图进行了分析,以确定样品的相纯度和结构稳定性。利用扫描电镜(SEM)对样品进行了结构表征,揭示了锆取代的晶粒细化和残余孔隙度。在15 keV ~ 15 MeV的能量范围内,利用Phy-X软件计算了不同的屏蔽参数,包括质量衰减系数(μm)、线性衰减系数(μ)、半值层(λ1/2)、单位质量相对于空气释放的动能(KERMA)、透射系数(TF%)、辐射防护效率(RPE)和比伽马射线常数(Γ)。例如,在15 keV下,Gd2Ti2O7和Nd2Zr2O7的μ分别达到486.58 cm−1和344.423 cm−1。同时,它们的λ1/2厚度低至~ 0.002 cm,证实了它们在0.1 MeV以下区域的优越屏蔽效率。在0.5 MeV左右,辐射防护效率保持在50%左右。在所研究的体系中,Gd2Ti2O7由于其较高的钆含量和较低的摩尔质量而始终优于其他体系,这增加了单位质量的光子相互作用概率。结果表明,我们的样品在核废料管理、反应堆安全和医疗辐射防护方面具有很强的应用前景。
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引用次数: 0
Novel development of low-loss MnZn ferrites by sintering process optimisation and CaTiO3 doping 烧结工艺优化及CaTiO3掺杂制备低损耗锰锌铁氧体
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2025-12-29 DOI: 10.1016/j.ceramint.2025.12.464
Mengrui Li , Shuyu Sun , Boon Xian Chai , Guibing Shi , Jiahui Li , M. Akbar Rhamdhani , Li Wang , Shanqing Xu
Renewable energy systems such as solar inverters increasingly require efficient and compact components. This drives the need for MnZn ferrites with low power loss and high permeability at high frequencies. This study addresses this challenge by optimising the sintering process and introducing CaTiO3 through a novel doping method. A higher heating rate and shorter sintering period refined the grain size, which was further enhanced by CaTiO3 doping. This microstructural improvement reduced eddy current loss and increased cut-off frequency. With the addition of 1200 ppm CaTiO3, MnZn ferrites achieved minimal power loss of under 130 mW/cm3 at 1 MHz/30 mT and 300 mW/cm3 at 3 MHz/10 mT over the temperature range of −20 °C–100 °C. Sintering temperature was successfully lowered to 1150 °C with only 30 min of holding time, promoting energy savings and sustainability. The combined sintering and doping strategy effectively improved electromagnetic properties, offering a scalable route for producing high-performance MnZn ferrites suitable for next-generation high-frequency applications.
可再生能源系统,如太阳能逆变器,越来越需要高效和紧凑的组件。这就需要在高频下具有低功耗和高磁导率的锰锌铁氧体。本研究通过优化烧结工艺和通过一种新的掺杂方法引入CaTiO3来解决这一挑战。较高的升温速率和较短的烧结时间细化了晶粒尺寸,CaTiO3的掺杂进一步增强了晶粒尺寸。这种微观结构的改进减少了涡流损耗,提高了截止频率。在- 20°C - 100°C的温度范围内,添加1200 ppm的CaTiO3, MnZn铁氧体在1 MHz/30 mT和3 MHz/10 mT下的最小功率损耗低于130 mW/cm3和300 mW/cm3。烧结温度降至1150℃,保温时间仅为30 min,促进了节能和可持续发展。烧结和掺杂相结合的策略有效地改善了电磁性能,为生产适合下一代高频应用的高性能MnZn铁氧体提供了可扩展的途径。
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引用次数: 0
The effect of LiOH addition and Aluminium morphology on the synthesis of AlN nanoparticles at low temperature LiOH添加量和铝的形貌对低温合成纳米AlN的影响
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2025-12-29 DOI: 10.1016/j.ceramint.2025.12.481
A. Bashiri, H. Ghanbari, S.M. Mirkazemi
The present study aimed to synthesize aluminum nitride (AlN) nanoparticles at low temperatures using a combination of mechanical alloying and direct nitridation processes. Aluminium (Al) powder with different morphology and limited lithium addition were employed to enhance the nitridation efficiency. The effects of Al particle morphology, Li incorporation, milling time, and nitridation temperature were systematically investigated. To investigate the phases, bonds, micro- and nanostructure, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy with map element analysis (FESEM), and high-resolution transmission electron microscopy (HR-TEM) analysis were performed, respectively. Moreover, the thermogravimetry differential thermal analysis (TG/DTA) was carried out to determine the nitridation mechanism. This study successfully demonstrated the effect of Al morphology, milling time, and temperature nitridation on the low-temperature AlN synthesis. The best results were achieved when the mixture of spherical Al, 0.5 wt% Li, and 6wt% N2H4 was used. Then, the optimized mixture was milled for 1 h in N2 atmosphere and nitrided at the temperature of 1100 °C for 3 h in N2 atmosphere. This process led to the synthesis of hexagonal AlN nanoparticles with a crystallite size of 30 ± 10 nm.
本研究旨在采用机械合金化和直接氮化相结合的方法,在低温下合成氮化铝纳米颗粒。采用不同形态的铝粉和少量的锂加入来提高氮化效率。系统考察了Al颗粒形貌、Li掺入量、磨粒时间和氮化温度等因素对氮化效果的影响。采用x射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、场发射扫描电子显微镜(FESEM)和高分辨率透射电子显微镜(HR-TEM)分析了其相、键、微观和纳米结构。采用热重差热分析(TG/DTA)确定了氮化机理。本研究成功地证明了Al的形貌、铣削时间和氮化温度对低温AlN合成的影响。以球形Al、0.5 wt% Li和6wt% N2H4为混合料,效果最佳。然后,将优化后的混合物在N2气氛中研磨1 h,在1100℃的N2气氛中氮化3 h。该工艺合成了晶粒尺寸为30±10 nm的六方AlN纳米颗粒。
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引用次数: 0
First-principles theoretical study of pure and Ti, Zr, and Hf doped K0.5Na0.5NbO3: Structural, electronic, mechanical, and piezoelectric properties 纯和掺Ti, Zr, Hf的K0.5Na0.5NbO3的第一性原理理论研究:结构、电子、机械和压电性能
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-05 DOI: 10.1016/j.ceramint.2026.01.059
Hicham Kacimi-Naciri , Mohamed Rguiti , Assia Mabrouk , Rachid Amrousse , Christian Courtois , Mohamed Aymen Ben Achour , Ahmed Bachar
Lead-free piezoelectric materials are gaining attention as environmentally sustainable alternatives to lead zirconate titanate (PZT)-based ceramics. Among these, potassium-sodium niobate (K0.5Na0.5NbO3, KNN) shows promising piezoelectric properties but faces challenges in densification and functional stability. This study uses first-principles density functional theory (DFT) calculations with the Wien2k code to explore the structural, electronic, mechanical, and piezoelectric properties of sodium-doped KNbO3. The optimized K0.5Na0.5NbO3 model was doped with 12.5 % transition metals (Ti, Zr, and Hf) at the B-site to investigate how ionic radius and electronic configuration affect the piezoelectric response, particularly the piezoelectric coefficient e33 (C/m2) and the piezoelectric constant d33 (pC/N). The results indicate significant enhancements in polarization behavior and electronic band characteristics with zirconium (Zr) doping in comparison to titanium (Ti) and hafnium (Hf); notably, the piezoelectric constant d33 reaches 118 pC/N, compared to 75 pC/N for KNN, aligning with previous experimental results. This theoretical study offers valuable insights for designing high-performance lead-free piezoelectric and lays a strong foundation for future experimental synthesis and applications in piezoelectric and ferroelectric technologies.
无铅压电材料作为锆钛酸铅(PZT)基陶瓷的环保可持续替代品正受到人们的关注。其中铌酸钾钠(K0.5Na0.5NbO3, KNN)具有良好的压电性能,但在致密化和功能稳定性方面面临挑战。本研究使用第一性原理密度泛函理论(DFT)计算和Wien2k代码来探索钠掺杂KNbO3的结构、电子、机械和压电特性。优化后的K0.5Na0.5NbO3模型在b位掺杂12.5%的过渡金属(Ti, Zr和Hf),研究离子半径和电子构型对压电响应的影响,特别是压电系数e33 (C/m2)和压电常数d33 (pC/N)。结果表明,与钛(Ti)和铪(Hf)相比,锆(Zr)掺杂显著增强了材料的极化行为和电子带特性;值得注意的是,压电常数d33达到118 pC/N,而KNN为75 pC/N,与之前的实验结果一致。该理论研究为高性能无铅压电材料的设计提供了有价值的见解,并为未来压电和铁电技术的实验合成和应用奠定了坚实的基础。
{"title":"First-principles theoretical study of pure and Ti, Zr, and Hf doped K0.5Na0.5NbO3: Structural, electronic, mechanical, and piezoelectric properties","authors":"Hicham Kacimi-Naciri ,&nbsp;Mohamed Rguiti ,&nbsp;Assia Mabrouk ,&nbsp;Rachid Amrousse ,&nbsp;Christian Courtois ,&nbsp;Mohamed Aymen Ben Achour ,&nbsp;Ahmed Bachar","doi":"10.1016/j.ceramint.2026.01.059","DOIUrl":"10.1016/j.ceramint.2026.01.059","url":null,"abstract":"<div><div>Lead-free piezoelectric materials are gaining attention as environmentally sustainable alternatives to lead zirconate titanate (PZT)-based ceramics. Among these, potassium-sodium niobate (K<sub>0.5</sub>Na<sub>0.5</sub>NbO<sub>3</sub>, KNN) shows promising piezoelectric properties but faces challenges in densification and functional stability. This study uses first-principles density functional theory (DFT) calculations with the Wien2k code to explore the structural, electronic, mechanical, and piezoelectric properties of sodium-doped KNbO<sub>3</sub>. The optimized K<sub>0.5</sub>Na<sub>0.5</sub>NbO<sub>3</sub> model was doped with 12.5 % transition metals (Ti, Zr, and Hf) at the B-site to investigate how ionic radius and electronic configuration affect the piezoelectric response, particularly the piezoelectric coefficient e<sub>33</sub> (C/m<sup>2</sup>) and the piezoelectric constant d<sub>33</sub> (pC/N). The results indicate significant enhancements in polarization behavior and electronic band characteristics with zirconium (Zr) doping in comparison to titanium (Ti) and hafnium (Hf); notably, the piezoelectric constant d<sub>33</sub> reaches 118 pC/N, compared to 75 pC/N for KNN, aligning with previous experimental results. This theoretical study offers valuable insights for designing high-performance lead-free piezoelectric and lays a strong foundation for future experimental synthesis and applications in piezoelectric and ferroelectric technologies.</div></div>","PeriodicalId":267,"journal":{"name":"Ceramics International","volume":"52 7","pages":"Pages 8607-8618"},"PeriodicalIF":5.6,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147412826","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Tb4O7-Sm2O3 doped glass ceramics containing Ba3Bi(PO4)3: Energy transfer mechanisms, temperature sensing performance and theoretical investigation on the substitution site 含Ba3Bi(PO4)3的Tb4O7-Sm2O3掺杂玻璃陶瓷:能量传递机理、温度传感性能及取代位的理论研究
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-07 DOI: 10.1016/j.ceramint.2026.01.087
Qianwen Wang , Haotian Zhao , Hongbo Zhang
To achieve color tunability and optical thermometry in a single matrix, Tb4O7-Sm2O3 co-doped glass ceramics containing Ba3Bi(PO4)3 crystalline phases were prepared by melt-annealing-crystallization. To balance the high transmittance and crystallinity, 690 °C/2 h was chosen as the optimum heat treatment condition. Color-tunable emission was achieved by varying the Sm2O3 concentration, and the energy transfer from Tb3+ to Sm3+ was demonstrated. Based on temperature dependence of the Tb3+/Sm3+ fluorescence intensity ratio, it was calculated that Sa reaches its maximum at 473 K for 0.00431 K-1 and Sr at 298 K for 2.42 % K−1. XRD Rietveld refinement and density-functional theory (DFT) calculations, it was demonstrated that rare-earth ions displace and occupy Bi sites within the Ba3Bi(PO4)3 lattice to enhance luminescence properties. These results indicate that Tb4O7-Sm2O3 co-doped glass ceramics are promising for applications in color-tunable emission and optical temperature sensing.
为了在单一基体中实现颜色可调性和光学测温,采用熔融退火结晶法制备了含Ba3Bi(PO4)3晶相的Tb4O7-Sm2O3共掺杂玻璃陶瓷。为了平衡高透光率和结晶度,选择690℃/2 h作为最佳热处理条件。通过改变Sm2O3的浓度,实现了颜色可调的发射,并证明了从Tb3+到Sm3+的能量转移。根据Tb3+/Sm3+荧光强度比的温度依赖性,计算出Sa在473 K时达到最大值,为0.00431 K-1; Sr在298 K时达到最大值,为2.42% K−1。XRD Rietveld细化和密度泛函理论(DFT)计算表明,稀土离子取代并占据了Ba3Bi(PO4)3晶格内的Bi位,从而增强了发光性能。这些结果表明Tb4O7-Sm2O3共掺杂玻璃陶瓷在颜色可调发射和光学温度传感方面具有广阔的应用前景。
{"title":"Tb4O7-Sm2O3 doped glass ceramics containing Ba3Bi(PO4)3: Energy transfer mechanisms, temperature sensing performance and theoretical investigation on the substitution site","authors":"Qianwen Wang ,&nbsp;Haotian Zhao ,&nbsp;Hongbo Zhang","doi":"10.1016/j.ceramint.2026.01.087","DOIUrl":"10.1016/j.ceramint.2026.01.087","url":null,"abstract":"<div><div>To achieve color tunability and optical thermometry in a single matrix, Tb<sub>4</sub>O<sub>7</sub>-Sm<sub>2</sub>O<sub>3</sub> co-doped glass ceramics containing Ba<sub>3</sub>Bi(PO<sub>4</sub>)<sub>3</sub> crystalline phases were prepared by melt-annealing-crystallization. To balance the high transmittance and crystallinity, 690 °C/2 h was chosen as the optimum heat treatment condition. Color-tunable emission was achieved by varying the Sm<sub>2</sub>O<sub>3</sub> concentration, and the energy transfer from Tb<sup>3+</sup> to Sm<sup>3+</sup> was demonstrated. Based on temperature dependence of the Tb<sup>3+</sup>/Sm<sup>3+</sup> fluorescence intensity ratio, it was calculated that S<sub>a</sub> reaches its maximum at 473 K for 0.00431 K<sup>-1</sup> and S<sub>r</sub> at 298 K for 2.42 % K<sup>−1</sup>. XRD Rietveld refinement and density-functional theory (DFT) calculations, it was demonstrated that rare-earth ions displace and occupy Bi sites within the Ba<sub>3</sub>Bi(PO<sub>4</sub>)<sub>3</sub> lattice to enhance luminescence properties. These results indicate that Tb<sub>4</sub>O<sub>7</sub>-Sm<sub>2</sub>O<sub>3</sub> co-doped glass ceramics are promising for applications in color-tunable emission and optical temperature sensing.</div></div>","PeriodicalId":267,"journal":{"name":"Ceramics International","volume":"52 7","pages":"Pages 8909-8920"},"PeriodicalIF":5.6,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147413107","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Synthesis of non-porous and nanocrystalline zirconium oxide - erbium oxide layers using metalorganic reactants 用金属有机反应物合成无孔纳米晶氧化锆-氧化铒层
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-08 DOI: 10.1016/j.ceramint.2026.01.099
Agata Sawka
In this work, zirconium oxide – erbium oxide (ZrO2-Er2O3) layers were synthesized using MOCVD (Metalorganic Chemical Vapour Deposition) on quartz glass plates. Zr(tmhd)4 (Zirconium tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionate)) and Er(tmhd)3 (Erbium tris((2,2,6,6-tetramethyl-3,5-heptanedionate)) were chosen as reactants. Pure argon (99,9999 %) was used as a carrier gas. The deposition temperature was in the range of 600–800 °C. The evaporation temperatures of reactants were 240–260 °C for Zr(tmhd)4 and 130–140 °C for Er(tmhd)3. Their vapours were transported to CVD (MOCVD) reactor by means of a carrier gas. The content of Er(tmhd)3 was 10 and 20 mol.% in the gas mixture. The value of the extended Grx/Rex2 (Gr-Grashof number, Re-Reynolds number, x-the distance from the point of gas inflow) criterion was assumed to be less than 0.1. Such a low value of this expression should ensure the growth of layers without the participation of homogeneous nucleation process.
Chemical composition, microstructure and structure of deposited layers were investigated. The layers were non-porous and uniform in thickness. They contained Zr, as well as Er. The shares of Er2O3 in ZrO2-Er2O3 layers were about 5 and 10 mol.%, respectively. The obtained layers were nanocrystalline. ZrO2-Er2O3 layers were single cubic phase and presented solid solution. UV–Vis transmittance of the deposited layers also was investigated. The estimated band gap (Eg) of the obtained layers was in the range of 5.33–5.65 eV.
本文采用金属有机化学气相沉积(MOCVD)技术在石英玻璃板上合成氧化锆-氧化铒(ZrO2-Er2O3)层。选择Zr(tmhd)4(四烷基锆(2,2,6,6-四甲基-3,5-庚二酸))和Er(tmhd)3(三烷基锆(2,2,6,6-四甲基-3,5-庚二酸))作为反应物。纯氩(99.9999%)作为载气。沉积温度为600 ~ 800℃。Zr(tmhd)4的蒸发温度为240 ~ 260℃,Er(tmhd)3的蒸发温度为130 ~ 140℃。它们的蒸汽通过载气输送到CVD (MOCVD)反应器。混合气中Er(tmhd)3的含量分别为10%和20%。扩展Grx/Rex2 (Gr-Grashof数,Re-Reynolds数,x-入气点距离)准则的值均小于0.1。这个表达式的如此低的值应该保证层的生长不参与均匀成核过程。研究了沉积层的化学成分、显微组织和结构。各层无孔,厚度均匀。它们含有Zr和Er。ZrO2-Er2O3层中Er2O3的含量分别约为5%和10%。所得层为纳米晶。ZrO2-Er2O3层为单立方相,呈固溶体。研究了沉积层的紫外-可见透射率。所得层的带隙(Eg)在5.33 ~ 5.65 eV之间。
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引用次数: 0
Time-resolved remote in-situ Raman system combined with infrared laser ablation: Validation on ZrO2 and oxidation pathway of SiC ceramics 时间分辨远程原位拉曼系统结合红外激光烧蚀:对ZrO2和SiC陶瓷氧化途径的验证
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-13 DOI: 10.1016/j.ceramint.2026.01.112
Weilong Kang , Kang He , Zhiguo Chen , Fengping Wang , Yuhang Wang
Real time in situ acquisition of material properties under extreme conditions is a critical technical challenge in advanced materials research. In this paper, a hybrid system integrating remote gated Raman technology, confocal Raman microscopy, and infrared laser ablation was developed. This integrated in situ system allows high temperature Raman spectroscopy measurements for materials resistant to extreme thermal environments, achieving spectral resolution and measurement performance comparable to commercial confocal Raman spectrometers.
Zirconia ceramics were used as standard samples to validate the functionality of the spectroscopic testing system. The calibrated in situ spectroscopic setup was then employed to conduct high temperature in situ Raman measurements on SiC materials. The in situ Raman spectra during SiC ablation revealed the oxidation products and their evolution, from which the onset of the passive to active oxidation transition window, under the present pO2 about 20 % and heating rate more than 300 °C, about 1200 °C was determined. This analysis also clarifies the self-healing role of the silicate scale and its coupling to lattice reordering in SiC.
This method reduces acquisition from hours to minutes, and enables phase or oxidation mapping while revealing reaction pathways in ultrahigh temperature ceramics, where capturing transient intermediates in real time provides robust data support for ceramics material investigations.
在极端条件下实时获取材料性能是先进材料研究的关键技术挑战。本文开发了一种集远程门控拉曼技术、共聚焦拉曼显微技术和红外激光烧蚀技术于一体的混合系统。这种集成的原位系统允许对耐极端热环境的材料进行高温拉曼光谱测量,实现光谱分辨率和测量性能可与商用共聚焦拉曼光谱仪相媲美。以氧化锆陶瓷为标准样品,验证了光谱测试系统的功能。然后利用校准后的原位光谱装置对SiC材料进行了高温原位拉曼测量。原位拉曼光谱揭示了碳化硅烧蚀过程中的氧化产物及其演化过程,确定了在pO2含量约为20%、升温速率超过300℃、1200℃的条件下,从被动氧化转变为主动氧化的过渡窗口。该分析还阐明了硅垢的自愈作用及其与碳化硅晶格重排序的耦合作用。该方法将采集时间从几小时减少到几分钟,并在揭示超高温陶瓷中的反应途径的同时实现相或氧化映射,其中实时捕获瞬态中间体为陶瓷材料研究提供了强大的数据支持。
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引用次数: 0
Study on the performance of inflatable porous electrode electrochemical discharge milling of quartz glass 膨胀多孔电极电化学放电铣削石英玻璃的性能研究
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-16 DOI: 10.1016/j.ceramint.2026.01.195
Linglei Kong , Lifeng Wei , Weining Lei , Yu Ji , Zhou Sun , Pan Zhang , Jinjin Han , Yafeng He
Quartz glass holds significant application value in microfluidic chip and microelectromechanical system device manufacturing due to its excellent optical transparency, chemical inertness, and biocompatibility. To enhance the machining quality of quartz glass microgrooves, this study proposes a novel process: Inflatable porous electrode electrochemical discharge milling (IP-ECDM). Through theoretical modeling and experimental validation, it reveals that gas injection into porous electrodes enhances gas film stability and optimizes discharge energy distribution, thereby improving machining efficiency. Fluid simulation analysis of the auxiliary gas within the porous electrode indicates that the flow resistance generated by the electrode's porous structure facilitates smoother, slower gas discharge. Simultaneously, electrode rotation promotes the renewal of auxiliary gas and electrolyte while improving the removal of machining debris. Experimental results from the IP-ECDM system demonstrate that material removal rate, microgroove depth, and width all increase with rising gas pressure. Under conditions of 0.15 MPa gas pressure and 46 V voltage, the porous electrode achieved a material removal rate 47.22 % higher than conventional solid electrodes, with average machining accuracy improved by 6.98 % and microgroove depth increased by 31.1 %. Furthermore, at relatively high feed rates, microgrooves machined with the porous electrode exhibited superior surface quality.
石英玻璃具有优异的光学透明性、化学惰性和生物相容性,在微流控芯片和微机电系统器件制造中具有重要的应用价值。为了提高石英玻璃微槽的加工质量,提出了一种新的加工工艺:充气多孔电极电化学放电铣削(IP-ECDM)。通过理论建模和实验验证,揭示了多孔电极注入气体增强了气膜稳定性,优化了放电能量分布,从而提高了加工效率。对多孔电极内辅助气体的流体模拟分析表明,电极的多孔结构产生的流动阻力有利于更平稳、更缓慢的气体放电。同时,电极旋转促进辅助气体和电解液的更新,同时提高了加工碎屑的去除率。IP-ECDM系统的实验结果表明,随着气体压力的升高,材料去除率、微槽深度和宽度均增加。在0.15 MPa气体压力和46 V电压条件下,多孔电极的材料去除率比传统固体电极高47.22%,平均加工精度提高6.98%,微槽深度增加31.1%。此外,在相对较高的进给速率下,用多孔电极加工的微槽表现出优异的表面质量。
{"title":"Study on the performance of inflatable porous electrode electrochemical discharge milling of quartz glass","authors":"Linglei Kong ,&nbsp;Lifeng Wei ,&nbsp;Weining Lei ,&nbsp;Yu Ji ,&nbsp;Zhou Sun ,&nbsp;Pan Zhang ,&nbsp;Jinjin Han ,&nbsp;Yafeng He","doi":"10.1016/j.ceramint.2026.01.195","DOIUrl":"10.1016/j.ceramint.2026.01.195","url":null,"abstract":"<div><div>Quartz glass holds significant application value in microfluidic chip and microelectromechanical system device manufacturing due to its excellent optical transparency, chemical inertness, and biocompatibility. To enhance the machining quality of quartz glass microgrooves, this study proposes a novel process: Inflatable porous electrode electrochemical discharge milling (IP-ECDM). Through theoretical modeling and experimental validation, it reveals that gas injection into porous electrodes enhances gas film stability and optimizes discharge energy distribution, thereby improving machining efficiency. Fluid simulation analysis of the auxiliary gas within the porous electrode indicates that the flow resistance generated by the electrode's porous structure facilitates smoother, slower gas discharge. Simultaneously, electrode rotation promotes the renewal of auxiliary gas and electrolyte while improving the removal of machining debris. Experimental results from the IP-ECDM system demonstrate that material removal rate, microgroove depth, and width all increase with rising gas pressure. Under conditions of 0.15 MPa gas pressure and 46 V voltage, the porous electrode achieved a material removal rate 47.22 % higher than conventional solid electrodes, with average machining accuracy improved by 6.98 % and microgroove depth increased by 31.1 %. Furthermore, at relatively high feed rates, microgrooves machined with the porous electrode exhibited superior surface quality.</div></div>","PeriodicalId":267,"journal":{"name":"Ceramics International","volume":"52 8","pages":"Pages 10189-10200"},"PeriodicalIF":5.6,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147419177","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Microstructural and optical–infrared properties of Ag–TiN–Al2O3 multilayers fabricated by magnetron sputtering 磁控溅射制备Ag-TiN-Al2O3多层膜的显微组织和光学红外性能
IF 5.6 2区 材料科学 Q1 MATERIALS SCIENCE, CERAMICS Pub Date : 2026-03-01 Epub Date: 2026-01-17 DOI: 10.1016/j.ceramint.2026.01.200
Rohit Bharti , Mohammad Mursaleen , Abhijit Dey
Ag–TiN–Al2O3 multilayer coatings were deposited on silicon substrates using sequential magnetron sputtering and examined for their structural and optical–infrared performance. The architecture consisted of a DC-sputtered Ag layer, an RF-sputtered TiN layer, and an RF-sputtered Al2O3 capping layer, with a total thickness of ∼512 nm. Vacuum annealing at 300 °C and 400 °C was carried out to study thermal stability. XRD confirmed enhanced crystallinity and preferred orientation with annealing, while FESEM showed gradual grain coarsening and improved surface densification. UV–Vis measurements indicated an increase in average reflectance from ∼71 % (as-deposited) to ∼82 % (400 °C). FTIR reflectance-based emissivity calculations showed values of 0.027 in the MWIR (3–5 μm) band and 0.075 in the LWIR (8–14 μm) band at 400 °C. These emissivity levels are lower than those reported for conventional ceramic, nitride, and composite coatings. The study demonstrates that the Ag–TiN–Al2O3 configuration can achieve low infrared emissivity through a simple sputtered multilayer design without requiring nanostructuring or complex fabrication steps.
采用顺序磁控溅射技术在硅衬底上沉积了Ag-TiN-Al2O3多层涂层,并对其结构性能和光学红外性能进行了测试。该结构由dc溅射Ag层、rf溅射TiN层和rf溅射Al2O3覆盖层组成,总厚度为~ 512 nm。在300℃和400℃下进行真空退火,研究其热稳定性。XRD证实退火后晶粒结晶度增强,取向择优,FESEM显示晶粒逐渐粗化,表面致密化程度提高。UV-Vis测量表明,平均反射率从~ 71%(沉积时)增加到~ 82%(400°C)。基于FTIR反射率的发射率计算表明,在400℃时,MWIR (3-5 μm)波段的发射率为0.027,LWIR (8-14 μm)波段的发射率为0.075。这些发射率水平低于传统陶瓷、氮化物和复合涂层。研究表明,Ag-TiN-Al2O3结构可以通过简单的溅射多层设计实现低红外发射率,而不需要纳米结构或复杂的制造步骤。
{"title":"Microstructural and optical–infrared properties of Ag–TiN–Al2O3 multilayers fabricated by magnetron sputtering","authors":"Rohit Bharti ,&nbsp;Mohammad Mursaleen ,&nbsp;Abhijit Dey","doi":"10.1016/j.ceramint.2026.01.200","DOIUrl":"10.1016/j.ceramint.2026.01.200","url":null,"abstract":"<div><div>Ag–TiN–Al<sub>2</sub>O<sub>3</sub> multilayer coatings were deposited on silicon substrates using sequential magnetron sputtering and examined for their structural and optical–infrared performance. The architecture consisted of a DC-sputtered Ag layer, an RF-sputtered TiN layer, and an RF-sputtered Al<sub>2</sub>O<sub>3</sub> capping layer, with a total thickness of ∼512 nm. Vacuum annealing at 300 °C and 400 °C was carried out to study thermal stability. XRD confirmed enhanced crystallinity and preferred orientation with annealing, while FESEM showed gradual grain coarsening and improved surface densification. UV–Vis measurements indicated an increase in average reflectance from ∼71 % (as-deposited) to ∼82 % (400 °C). FTIR reflectance-based emissivity calculations showed values of 0.027 in the MWIR (3–5 μm) band and 0.075 in the LWIR (8–14 μm) band at 400 °C. These emissivity levels are lower than those reported for conventional ceramic, nitride, and composite coatings. The study demonstrates that the Ag–TiN–Al<sub>2</sub>O<sub>3</sub> configuration can achieve low infrared emissivity through a simple sputtered multilayer design without requiring nanostructuring or complex fabrication steps.</div></div>","PeriodicalId":267,"journal":{"name":"Ceramics International","volume":"52 8","pages":"Pages 10244-10254"},"PeriodicalIF":5.6,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147419179","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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Ceramics International
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