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The effect of the synthesis temperature and time on the formation of boron suboxide 合成温度和时间对亚氧化硼生成的影响
IF 1.8 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-13 DOI: 10.1007/s41779-025-01147-6
Tuba Karamete, Hülya Biçer, Çağan Berker İyi, Mustafa Tuncer, Hasan Göçmez

Boron suboxide (B6O), offering a good balance between abundance of its constituents and promising tribological performance, is intriguing. Applications such as cutting tools, high-wear resistant coatings, and ballistics would benefit from such properties, however a feasible synthesis method is yet to be realized. The synthesis of B6O under atmospheric pressure is a challenging pursuit, and there is insufficient thermodynamic data for the formation of boron suboxide in the literature. In this study, boron suboxide powder was synthesized by reducing B2O3 by amorphous boron. Phase analysis of the formation of boron suboxide was demonstrated within the temperature range of 1200–1350 °C. The amorphous phase beside boron suboxide is present for all temperature treatments, but the best fitting crystalline phase was observed of the powder synthesized at 1300 °C. The powder was also heat treated at 1300 °C for various hours (2–6 h), and the crystalline phase was only observed for the powder heat treated for 4 h. The morphology of synthesized powder exhibited a star-like morphology. The production of B6O-TiB2 composite powder by reduction of TiO2 by amorphous boron with the excess addition of boron is also reported in this study.

亚氧化硼(b60),在其丰富的成分和有前途的摩擦学性能之间提供了良好的平衡,是有趣的。切削工具、高耐磨涂层和弹道学等应用将受益于这种性能,但一种可行的合成方法尚未实现。常压下合成b60是一项具有挑战性的工作,文献中也没有足够的亚氧化硼生成的热力学数据。本研究采用非晶硼还原B2O3合成亚氧化硼粉体。在1200 ~ 1350℃的温度范围内,对亚氧化硼的形成进行了物相分析。所有温度处理均存在亚氧化硼旁边的非晶相,但在1300℃合成的粉末中观察到最适合的结晶相。粉末在1300℃下热处理不同时间(2-6 h),仅在热处理4 h时观察到结晶相,合成的粉末形貌呈现星形形貌。本研究还报道了在过量添加硼的情况下,用无定形硼还原TiO2制备b60 - tib2复合粉体。
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引用次数: 0
Effect of hydrated aluminium fluoride on phase transformation and morphology evolution of alumina 水合氟化铝对氧化铝相变和形貌演变的影响
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-08 DOI: 10.1007/s41779-024-01135-2
Ziyu Zhang, Liang Zhang, Lingling Zhu, Mingtang Fu, Heqi Qi, Dong Zhang, Zihan Zhao, Shichen Xing, Dongmo Wu

In order to verify the formation of gaseous phase fluoride and its influence on the morphological evolution and the growth mechanism of α-Al2O3, the α-phase transformation temperature and morphology of α-Al2O3 powders from the calcination of commercial γ-Al2O3 and Al(OH)3 precursor with the addition of AlF3·3H2O additive have been studied through the incorporation of mixed placement experiments, layered placement experiments and separated placement experiments. The formation of gaseous phase fluoride has been experimentally confirmed by means of layered placement experiments and separated placement experiments, especially by the enhancement of the α-phase transformation occurred outside the small crucible in separated placement experiments. AlF3·3H2O additive significantly enhances shape anisotropy of α-Al2O3 precursor and lowers the total α-transformation temperature (900 °C for Al(OH)3 precursor and 1100 °C for γ-Al2O3 precursor ), even though the commercial precursor and AlF3·3H2O additive has been completely isolated by small crucible with cover.

为了验证气相氟化物的形成及其对α-Al2O3形态演化的影响和生长机理,通过混合放置实验、分层放置实验和分离放置实验,研究了添加AlF3·3H2O添加剂的γ-Al2O3和Al(OH)3前驱体煅烧后α-Al2O3粉末的α相变温度和形貌。通过分层放置实验和分离放置实验证实了气相氟化物的形成,特别是分离放置实验中小坩埚外α-相变的增强。AlF3·3H2O添加剂显著提高了α-Al2O3前驱体的形状各向异性,降低了α-转变总温度(Al(OH)3前驱体为900℃,γ-Al2O3前驱体为1100℃),而工业前驱体和AlF3·3H2O添加剂已被小坩埚完全隔离。
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引用次数: 0
Synthesis and Characterization of Cu-Vanadate Doped Hydroxyapatite Nanoparticles: Morphological, Structural, and Stability for Biomedical Use 钒酸铜掺杂羟基磷灰石纳米颗粒的合成和表征:形态、结构和生物医学用途的稳定性
IF 1.8 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-06 DOI: 10.1007/s41779-024-01120-9
Manal M. Alkhamisi

This study evaluates copper/vanadate co-doped hydroxyapatite (Cu-V-HAP) composites synthesized with varying vanadate concentrations to assess their crystallinity, hardness, antibacterial activity, and cell viability. The Cu-0.0V-HAP exhibited an average particle diameter of approximately 50 nm, while the Cu-0.8V-HAP showed a reduced size of around 30 nm, indicating significant disruption of the crystalline structure. Hardness measurements revealed values of 1.8 ± 0.1 GPa for Cu-0.0V-HAP, peaking at 4.5 ± 0.14 GPa for Cu-0.6V-HAP, with a decrease observed in Cu-0.8V-HAP. Antibacterial activity against E. coli ranged from 0 mm for Cu-0.0V-HAP to 8.1 ± 0.6 mm for Cu-0.8V-HAP. Furthermore, cell viability results indicated that Cu-0.6V-HAP achieved a high rate of 98.2 ± 4%, compared to 88.4 ± 4% for Cu-0.0V-HAP. These results suggest that optimal vanadate concentrations enhance the mechanical stability, antibacterial properties, and biocompatibility of co-doped HAP composites, indicating their potential for biomedical applications.

本研究评估了不同钒酸盐浓度下合成的铜/钒酸盐共掺杂羟基磷灰石(Cu-V-HAP)复合材料的结晶度、硬度、抗菌活性和细胞活力。Cu-0.0V-HAP的平均粒径约为50 nm,而Cu-0.8V-HAP的粒径减小了约30 nm,表明晶体结构明显破坏。Cu-0.0V-HAP的硬度值为1.8±0.1 GPa, Cu-0.6V-HAP的硬度峰值为4.5±0.14 GPa, Cu-0.8V-HAP的硬度值有所下降。Cu-0.0V-HAP对大肠杆菌的抑菌活性范围为0 mm ~ 8.1±0.6 mm。此外,细胞存活率结果表明,Cu-0.6V-HAP的存活率为98.2±4%,而Cu-0.0V-HAP的存活率为88.4±4%。这些结果表明,最佳钒酸盐浓度可以增强共掺杂HAP复合材料的机械稳定性、抗菌性能和生物相容性,表明其在生物医学上的应用潜力。
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引用次数: 0
Synthesis, morphology investigation and electrical conduction mechanism of rubidium yttrium diphosphate 二磷酸钇铷的合成、形貌研究及导电机理
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-04 DOI: 10.1007/s41779-024-01138-z
Souad Chkoundali, Hanen Ghoudi, Samia Aydi, Abderrazek Oueslati, Abdelhedi Aydi

The rubidium yttrium diphosphate compoundwas synthesized by solid route. The characteristics of this compound have been determined using X-ray powder diffraction, morphological, Raman and complex impedance spectroscopy. While X-ray powder diffraction revealed that RbYP2O7 compound crystallizes in the monoclinic system (P21/c space group), the SEM mapping demonstrated that the particles have the shape of squares of different sizes and demonstrate that the mean crystalline size of the specimen is 1.75 μm. The complex impedance spectra analysis indicated that the electrical features of the compound are largely dependent on temperature and frequency. Two semi circles are detectable in the Nyquist plots of the complex impedance spectra, suggesting the contribution of the effects of the grain and grain boundary. Non-Debye type relaxation mechanism coupled with negative temperature coefficient of resistance (NTCR) behaviour was indicated by temperature dependent impedance spectroscopy. Additionally, the AC conductivity frequency dependence was interpreted in terms of Jonscher’s law, whereas DC conductivity promotes the polaron assisted hopping in RbYP2O7 composition having activation energies of the grain σg and grain boundary are Eag= 0.81 eV and Eagb = 1.21 eV, respectively. The power law exponent (s) yielded that the correlated barrier hopping (CBH) model corresponds to the dominant transport process in this material. Furthermore, the multiple relaxation process was revealed by the modulus spectroscopy dominated by the mixed Rb+ cation motion within the investigated material structure.

采用固体法合成了二磷酸铷钇化合物。用x射线粉末衍射、形貌、拉曼光谱和复阻抗谱测定了该化合物的特征。x射线粉末衍射显示RbYP2O7化合物在单斜晶系(P21/c空间群)中结晶,SEM图显示颗粒具有不同大小的正方形,样品的平均晶粒尺寸为1.75 μm。复阻抗谱分析表明,化合物的电特性与温度和频率有很大关系。在复阻抗谱的奈奎斯特图中可以检测到两个半圆,表明晶粒和晶界的影响。温度相关阻抗谱分析表明了非debye型弛豫机制与负温度电阻系数(NTCR)行为耦合。此外,交流电导率频率依赖于Jonscher定律,而直流电导率促进了RbYP2O7成分的极化子辅助跳变,晶粒的活化能σg和晶界分别为Eag= 0.81 eV和Eagb = 1.21 eV。幂律指数(s)表明,相关垒跳(CBH)模型对应于该材料的主导输运过程。此外,在研究的材料结构中,以混合Rb+阳离子运动为主的模谱揭示了多重弛豫过程。
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引用次数: 0
Parameters influencing the characteristics of the nano-bonded aluminosilicate based refractory castables 影响纳米硅铝基耐火浇注料性能的参数
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-03 DOI: 10.1007/s41779-024-01139-y
Shirin Khanmohammadi, Masoomeh Mohtadinia

Replacing calcium aluminate cement as hydraulic binder by silica sol as sol-gel binder for refractory castables is known to reduce drawbacks of hydraulic binders but still comprehensive information regarding the effect of various raw materials and additives are required. In this research bauxite, andalusite and argellite were chosen as aluminosilicate aggregates and silica sol as binder and the effect of citric acid, micro silica and cement as setting agent were investigated for different compositions. Mechanical strength of the obtained castables at different temperatures of 110, 1000 and 1400°C were probed for various compositions. Finally based on the maximum mechanical strength of 342.5 and 241 Kg/cm2 at 110°C, workability and flowability of the castables, optimum compositions were selected. The used amounts of citric acid, micro silica and cement for bauxite optimized composition were 0.04%, 2% and 1% while there were 0.02%, 0% and 1%, respectively for andalusite based one. The effect of sol-gel binder on the corrosion resistance of the optimized compositions was investigated in contact with molten sodium silicate using static cup test. Bauxite based castables showed mechanical strength higher than andalusite ones, while the later exhibited better corrosion resistance which related to the intrinsic characteristics of the used aggregates.

用硅溶胶代替铝酸钙水泥作为水力粘结剂用于耐火浇注料的溶胶-凝胶粘结剂,可以减少水力粘结剂的缺点,但仍需要对各种原料和添加剂的影响进行全面的了解。本研究以铝土矿、红柱石和泥晶石为铝硅酸盐聚集体,以硅溶胶为粘结剂,考察了不同组成的柠檬酸、微二氧化硅和水泥作为凝结剂的效果。在110℃、1000℃和1400℃的不同温度下,对不同成分的浇注料进行了机械强度测试。最后根据浇注料在110℃时的最大机械强度342.5和241 Kg/cm2,以及浇注料的和易性和流动性,选择了最佳的浇注料组合。铝土矿优化配方中柠檬酸、微二氧化硅和水泥的用量分别为0.04%、2%和1%,红珠石优化配方中柠檬酸、微二氧化硅和水泥的用量分别为0.02%、0%和1%。采用静杯试验研究了溶胶-凝胶粘结剂对优化组合物与水玻璃熔液接触耐蚀性能的影响。铝土矿基浇注料的机械强度高于红柱石基浇注料,而红柱石基浇注料具有更好的耐腐蚀性能,这与所用骨料的内在特性有关。
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引用次数: 0
Spark plasma sintering of B4C-TiB2 composite: Effect of combustion synthesized nanoparticle on sinterability and mechanical properties 放电等离子烧结B4C-TiB2复合材料:燃烧合成纳米颗粒对烧结性能和力学性能的影响
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2025-01-03 DOI: 10.1007/s41779-024-01113-8
Ozan Coban, Mehmet Bugdayci, Salih Çagri Ozer, Serkan Baslayici, Servet Turan, M. Ercan Acma

This study investigated the effects of fine particles with high surface area synthesized by Self-propagating High-Temperature Synthesis (SHS) on the SPS process and the properties of the resulting products. Correlations were established between particle size, SHS product addition, sinterability, and mechanical properties. The products were characterized by measuring shrinkage percentages, relative density, microhardness, elastic modulus, and fracture toughness, which were further correlated with SEM–EDS results. The results revealed that SHS nanoparticles significantly increased fracture toughness, especially with additions above 60%, by reducing average particle size, increasing powder porosity, and adding composite powder. The product exhibited high relative density (99.03%), elastic modulus (464 GPa), and fracture toughness (4.65 MPa.m1/2) when SPS was used on B4C-TiB2 powders containing 80% SHS product at a low temperature of 1550 °C. By adding 80% SHS product, hardness increased by 62% (19.5 GPa) and fracture toughness by 24%, even at low sintering temperatures, thus reducing energy consumption.

研究了自传播高温合成法(SHS)合成的高比表面积细颗粒对SPS过程和产物性能的影响。建立了颗粒尺寸、SHS产品添加量、烧结性能和力学性能之间的相关性。通过测量收缩率、相对密度、显微硬度、弹性模量和断裂韧性来表征产品,并进一步与SEM-EDS结果相关联。结果表明,SHS纳米颗粒通过减小平均粒径、增加粉末孔隙率和添加复合粉末等方式显著提高了断裂韧性,特别是添加量在60%以上时。该产品具有较高的相对密度(99.03%)、弹性模量(464 GPa)和断裂韧性(4.65 MPa)。在1550℃的低温条件下,SPS对含有80% SHS产物的B4C-TiB2粉末进行处理时,得到了m1/2)。添加80% SHS产品,即使在低烧结温度下,硬度也提高62% (19.5 GPa),断裂韧性提高24%,从而降低了能耗。
{"title":"Spark plasma sintering of B4C-TiB2 composite: Effect of combustion synthesized nanoparticle on sinterability and mechanical properties","authors":"Ozan Coban,&nbsp;Mehmet Bugdayci,&nbsp;Salih Çagri Ozer,&nbsp;Serkan Baslayici,&nbsp;Servet Turan,&nbsp;M. Ercan Acma","doi":"10.1007/s41779-024-01113-8","DOIUrl":"10.1007/s41779-024-01113-8","url":null,"abstract":"<div><p>This study investigated the effects of fine particles with high surface area synthesized by Self-propagating High-Temperature Synthesis (SHS) on the SPS process and the properties of the resulting products. Correlations were established between particle size, SHS product addition, sinterability, and mechanical properties. The products were characterized by measuring shrinkage percentages, relative density, microhardness, elastic modulus, and fracture toughness, which were further correlated with SEM–EDS results. The results revealed that SHS nanoparticles significantly increased fracture toughness, especially with additions above 60%, by reducing average particle size, increasing powder porosity, and adding composite powder. The product exhibited high relative density (99.03%), elastic modulus (464 GPa), and fracture toughness (4.65 MPa.m<sup>1/2</sup>) when SPS was used on B<sub>4</sub>C-TiB<sub>2</sub> powders containing 80% SHS product at a low temperature of 1550 °C. By adding 80% SHS product, hardness increased by 62% (19.5 GPa) and fracture toughness by 24%, even at low sintering temperatures, thus reducing energy consumption.</p></div>","PeriodicalId":673,"journal":{"name":"Journal of the Australian Ceramic Society","volume":"61 3","pages":"937 - 951"},"PeriodicalIF":2.1,"publicationDate":"2025-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145161198","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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
Magnetic and luminescence properties of bioactive glass nanoparticles for biomedical applications 生物医学应用中生物活性玻璃纳米颗粒的磁性和发光特性
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-12-30 DOI: 10.1007/s41779-024-01141-4
Fatma Unal, Batur Ercan

This study explores the synthesis and characterization of superparamagnetic iron oxide nanoparticles (SPIONs) coated with zinc (Zn) and/or europium (Eu) doped bioactive glass. Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) confirmed spherical agglomerated morphology and core@shell structure, respectively. High-Resolution TEM (HR-TEM) revealed lattice fringe values consistent with the cubic magnetite phase. Magnetic property assessment showed stable superparamagnetic behavior with slight reductions in saturation magnetization (σs) after immersion in simulated body fluid (SBF) solution. Photoluminescence (PL) spectra of Eu-doped samples exhibited red emission, confirming Eu rare earth element incorporation and maintaining luminescence post-immersion in SBF. Upon the interaction with SBF, hydroxyapatite (HA) formation occurred on the nanoparticle surfaces, suggesting the bioactive nature of the nanoparticles. These findings suggest that the synthesized nanoparticles exhibit promising potential for biomedical applications, including imaging, and orthopedics, due to their bioactive, magnetic, and luminescent properties.

本研究探讨了超顺磁性氧化铁纳米粒子(SPIONs)的合成和表征,SPIONs包覆有锌(Zn)和/或铕(Eu)掺杂的生物活性玻璃。扫描电子显微镜(SEM)和透射电子显微镜(TEM)分别证实了球团形态和core@shell结构。高分辨率透射电镜(HR-TEM)显示晶格条纹值与立方磁铁矿相一致。磁性能评价表明,在模拟体液(SBF)溶液中浸泡后,饱和磁化强度(σs)略有降低,超顺磁性行为稳定。Eu掺杂样品的光致发光(PL)光谱显示出红色发射,证实了Eu稀土元素的掺入,并在SBF中浸没后保持发光。与SBF相互作用后,纳米颗粒表面形成羟基磷灰石(HA),表明纳米颗粒具有生物活性。这些发现表明,由于其生物活性、磁性和发光特性,合成的纳米颗粒在生物医学应用方面具有很大的潜力,包括成像和骨科。
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引用次数: 0
Texture induced superhydrophilic ceramic surfaces with hybrid structures 具有杂化结构的织构诱导超亲水性陶瓷表面
IF 2.1 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-12-27 DOI: 10.1007/s41779-024-01140-5
Gokhan Acikbas

There are two primary methods for creating superhydrophilic surfaces: applying photochemically active chemicals as coatings or creating a textured surface. Texture-induced superhydrophilic surfaces have a further advantage of being stable and without requiring radiation. The creation of texture on the surface mostly depends on the chemical composition and firing conditions. Therefore, this study aims to assess the influence of alterations in glaze composition and firing cycle on crystal phase development, microstructure, contact angle, surface roughness, and specific surface energy in nano ZnO/ZnO-Cu included glazes. In this sense, glaze formulations comprising 7.8% nano zinc oxide / 7.8% nano zinc oxide, and 0.780% nano copper, with industrial glaze, were developed. Glazed samples were sintered at 1210 °C and underwent heat treatment at 965 °C for periods of 8 and 32 h. The surfaces of the samples were examined utilizing scanning electron microscopy, X-ray diffraction, surface profilometry, and wetting angle goniometry. As a result, superhydrophilic surfaces was obtained with the formation of multi-layer structures consisting of micro-sized willemite islands at the bottom and on top of well crystalized smaller (around 1 micron in size) willemite grains and at the top nano spherical shape plagioclase granular structures. After 8 h of heat treatment, the surface achieves its maximum superhydrophilic state with a contact angle of 5◦. The superhydrophilicity was caused by the nano crystalline plagioclase granules’ surface architecture, not its chemical composition.

有两种主要的方法来创建超亲水性表面:应用光化学活性化学品作为涂层或创建一个纹理表面。纹理诱导的超亲水性表面具有稳定和不需要辐射的进一步优势。表面纹理的产生主要取决于化学成分和烧制条件。因此,本研究旨在评估釉料成分和烧成周期的变化对纳米ZnO/ZnO- cu含锌釉的晶相发育、微观结构、接触角、表面粗糙度和比表面能的影响。在此基础上,研制了含7.8%纳米氧化锌/ 7.8%纳米氧化锌和0.80%纳米铜的工业釉釉配方。上釉样品在1210°C下烧结,在965°C下进行8和32小时的热处理。样品的表面使用扫描电子显微镜、x射线衍射、表面轮廓仪和润湿角测量仪进行检查。结果,获得了超亲水表面,形成了多层结构,包括底部和顶部的微尺寸的威勒米特岛,晶体化良好的较小的威勒米特颗粒(尺寸约为1微米)和顶部的纳米球形斜长石颗粒结构。热处理8h后,表面达到最大的超亲水性,接触角为5◦。超亲水性是由纳米斜长石颗粒的表面结构引起的,而不是由其化学成分引起的。
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引用次数: 0
Investigation low-temperature densification and dielectric properties of glass/Al2O3/nano-TiO2 ceramics for microwave applications 研究微波用玻璃/Al2O3/纳米tio2陶瓷的低温致密化和介电性能
IF 1.8 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-12-20 DOI: 10.1007/s41779-024-01136-1
Oğuzhan Bilaç

A commercial SiO2-Al2O3-CaO-based commercial glass, Al2O3, and nano-TiO2 were used as initial materials. Glass/Al2O3/TiO2 samples were fabricated using the uniaxial dry pressing method, using C55 with 15 wt% TiO2, 23 wt% TiO2 and 36 wt% TiO2. The optimum bulk density temperature for the C55 was 800 ˚C, for the C55-15 T was 900 ˚C, for the C55-23 T was 900 ˚C, for the C55-36 T was 1000 ˚C. TiO2 neither chemically reacted with the other phases nor decomposed with temperature which was critical to increasing the dielectric constant. The C55-36 T sample was highlighted for its low sintering temperature of 1000 °C, high dielectric constant values (18.92 at 5 MHz, 17.40 at 1 GHz, and 17.03 at 10 GHz), low dielectric loss (0.0058 at 5 MHz, 0.0063 at 1 GHz, and 0.0075 at 10 GHz), as well as a near-zero temperature coefficient (1.7 ppm/°C) along with high mechanical properties.

以工业sio2 -Al2O3- cao基工业玻璃、Al2O3和纳米tio2作为初始材料。采用C55, 15wt % TiO2, 23wt % TiO2和36wt % TiO2,采用单轴干压法制备了玻璃/Al2O3/TiO2样品。C55的最佳容重温度为800˚C, C55-15的最佳容重温度为900˚C, C55-23的最佳容重温度为900˚C, C55-36的最佳容重温度为1000˚C。TiO2既不与其他相发生化学反应,也不随温度分解,这是提高介电常数的关键。C55-36 T样品具有低烧结温度(1000℃)、高介电常数值(5 MHz时为18.92、1 GHz时为17.40、10 GHz时为17.03)、低介电损耗(5 MHz时为0.0058、1 GHz时为0.0063、10 GHz时为0.0075)、近零温度系数(1.7 ppm/°C)和高机械性能。
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引用次数: 0
Understanding the processing of mullite-based ceramics from kaolin waste: a cautionary note on the inadvertent use of split-plot designs 了解从高岭土废料中加工莫来石基陶瓷:对无意中使用分块设计的警告
IF 1.8 4区 材料科学 Q2 MATERIALS SCIENCE, CERAMICS Pub Date : 2024-12-19 DOI: 10.1007/s41779-024-01126-3
Rivaildo M. Andrade, Allan J. M. Araújo, Rafael A. Raimundo, Ricardo P. S. Dutra, Liszandra F. A. Campos, Carla A. Vivacqua, André L. S. Pinho, Daniel A. Macedo

Experimentation plays an important role in ceramic science and engineering, which involves the design of new products, development of new manufacturing processes, and also the optimization of processing. In this work, a cautionary note on the inadvertent use of split-plot designs was presented to understand the processing of mullite-based ceramics from kaolin waste. Samples were obtained by solid-state reactive sintering of kaolin waste following a 22 × 2 full factorial split-plot design. The influence of firing temperature, time and applied pressing pressure on the physical properties was evaluated. The structural and microstructural analyses of fired samples were evaluated by X-ray diffractometry (XRD) and field emission scanning electron microscopy (FESEM). Kaolin waste processed ceramics at 1400 ºC consist of elongated mullite crystals uniformly embedded into a glassy phase and minor amounts of quartz. Statistical models were constructed for open porosity and density at 1% level of significance. The estimated P-values indicate that the coefficients associated with the applied pressing pressure and its interaction with firing temperature and time ((:gamma:) and (:{delta:}_{1})) were statistically significant for open porosity and density. The higher applied pressing pressure leads to lower open porosity. The densification process was influenced by different sintering mechanisms depending on temperature (solid phase sintering vs. liquid phase sintering). The lack of harmony between the planning and the execution of the experiment does not allow the testing of the main effects of firing temperature, time and the interaction between them (β1, β2 and β3). Understanding the proper way to plan, execute and analyze experiments are of urgent interest in the field of ceramic processing, and that is the key message of this paper.

实验在陶瓷科学与工程中起着重要的作用,它涉及到新产品的设计、新制造工艺的开发以及加工工艺的优化。在这项工作中,对无意中使用分裂图设计提出了一个警告,以了解从高岭土废料中加工莫来石基陶瓷的过程。采用22 × 2全因子裂图设计,对高岭土废料进行固态反应烧结制备样品。考察了烧成温度、时间和施加的压力对材料物理性能的影响。利用x射线衍射仪(XRD)和场发射扫描电镜(FESEM)对烧结样品的结构和微观结构进行了分析。在1400℃下,高岭土废料加工陶瓷由均匀嵌入玻璃相的细长莫来石晶体和少量石英组成。建立了1时孔隙度和密度的统计模型% level of significance. The estimated P-values indicate that the coefficients associated with the applied pressing pressure and its interaction with firing temperature and time ((:gamma:) and (:{delta:}_{1})) were statistically significant for open porosity and density. The higher applied pressing pressure leads to lower open porosity. The densification process was influenced by different sintering mechanisms depending on temperature (solid phase sintering vs. liquid phase sintering). The lack of harmony between the planning and the execution of the experiment does not allow the testing of the main effects of firing temperature, time and the interaction between them (β1, β2 and β3). Understanding the proper way to plan, execute and analyze experiments are of urgent interest in the field of ceramic processing, and that is the key message of this paper.
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引用次数: 0
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Journal of the Australian Ceramic Society
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