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Experimental determination of phase stability of the cubic L12 HfAl3-xZnx phase 立方 L12 HfAl3-xZnx 相的相稳定性实验测定
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-02 DOI: 10.1016/j.tca.2024.179873
S. Delsante , G. Borzone , N. Parodi , S. Guerrucci
The present study is devoted to the experimental investigation of homogeneity range and heat of formation (Δf at 300 K) of the cubic L12–HfAl3-xZnx solid solution. A high-temperature direct drop calorimeter has been employed to synthesize and simultaneously determine the Δf of several alloys along the HfZn3–HfAl3 section (25 at. % Hf) whereas X-Ray Powder Diffraction (XRPD) and Scanning Electron Microscopy (SEM) paired with an EDS (Energy Dispersive Spectrometer detector) have been employed to characterize the samples. The performed analysis confirmed that the ternary HfAl3-xZnx alloys were nearly single phase in the range 1 ≤ x ≤ 2.24 having the cubic L12 structure; this in turn helps establish the trend of L12 lattice parameter (at room temperature) with composition. Thanks to the interpolation of our experimental data, the following values of ΔfH° (kJ/mol-atom at 300 K) for the L12–HfAl3-xZnx were determined: -37.1 ± 2.0 (HfAl0.8Zn2.2 corresponding to Hf25Al20Zn55 at. %), -41.7 ± 2.0 (HfAl1.2Zn1.8 corresponding to Hf25Al30.0Zn45.0 at. %), -45.1 ± 2.0 (HfAl1.5Zn1.5 corresponding to Hf25Al37.5Zn37.5 at. %) and -48.5 ± 2.0 (HfAl1.8Zn1.2 corresponding to Hf25Al45.0Zn30.0 at. %). For two pertinent binary intermetallic phases, the following ΔfH° values (in kJ/mol-atom) at 300 K have been obtained: -31.8 ± 3.0 for HfZn3 (unknown structure) and -37.0 ± 2.0 for HfAl3 (tetragonal DO23 – type structure).
本研究致力于对立方体 L12-HfAl3-xZnx 固溶体的均匀性范围和形成热(ΔfH°,300 K)进行实验研究。我们使用高温直接滴热量计合成并同时测定了 HfZn3-HfAl3 部分(25% Hf)几种合金的 ΔfH°,同时使用 X 射线粉末衍射 (XRPD) 和扫描电子显微镜 (SEM) 搭配 EDS(能量色散光谱仪检测器)对样品进行表征。所进行的分析证实,三元 HfAl3-xZnx 合金在 1 ≤ x ≤ 2.24 的范围内几乎是单相的,具有立方 L12 结构;这反过来又有助于确定 L12 晶格参数(室温下)随成分变化的趋势。通过对我们的实验数据进行插值,确定了 L12-HfAl3-xZnx 的 ΔfH° 值(300 K 时为 kJ/mol-原子):-37.1 ± 2.0(HfAl0.8Zn2.2 对应 Hf25Al20Zn55 at.%)、-41.7 ± 2.0(HfAl1.2Zn1.8,相当于 Hf25Al30.0Zn45.0 at.%)、-45.1 ± 2.0(HfAl1.5Zn1.5,相当于 Hf25Al37.5Zn37.5 at.%)和 -48.5 ± 2.0(HfAl1.8Zn1.2,相当于 Hf25Al45.0Zn30.0 at.%)。对于两种相关的二元金属间相,在 300 K 时获得了以下 ΔfH° 值(单位:kJ/mol-atom):HfZn3(未知结构)为 -31.8 ± 3.0,HfAl3(四方 DO23 型结构)为 -37.0 ± 2.0。
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引用次数: 0
Kinetics of L-lactide bulk polymerization initiated with zirconium(IV) acetylacetonate studied by non-isothermal differential scanning calorimetry 通过非等温差示扫描量热法研究乙酰丙酮锆(IV)引发的 L-内酰胺大体积聚合动力学
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-10-01 DOI: 10.1016/j.tca.2024.179872
Kirill T. Kalinin , Dmitry R. Streltsov , Petr V. Dmitryakov , Nikita G. Sedush , Sergei N. Chvalun
The kinetics of L-lactide bulk polymerization initiated with a non-toxic initiator, zirconium(IV) acetylacetonate, was studied by non-isothermal differential scanning calorimetry. The polymerization kinetics was analyzed using a combination of isoconversional “model–free” and model–fitting methods. It was revealed that the model–free analysis results in an autocatalytic reaction model function. To provide a physical meaning for this effective reaction model, a model–fitting analysis with a two–step kinetic model taking into account irreversible initiation and reversible propagation reactions was applied. It was demonstrated, that even such simple multi–step kinetic model can explain the general features of the polymerization reaction revealed by the isoconversional analysis, i.e. a variation of the effective activation energy with a conversion degree and an autocatalytic character of the effective reaction model. The rate constants for the initiation, ki, and propagation, kp, reactions were evaluated. It was revealed that the values of ki are about two decimal orders lower than that of kp indicating slow initiation in the studied temperature range.
采用非等温差示扫描量热法研究了无毒引发剂乙酰丙酮锆(IV)引发的 L-内酯批量聚合的动力学。聚合动力学分析采用了等转换 "无模型 "法和模型拟合法相结合的方法。结果表明,无模型分析得出了一个自催化反应模型函数。为了给这一有效的反应模型提供物理意义,采用了考虑到不可逆启动和可逆传播反应的两步动力学模型进行模型拟合分析。结果表明,即使是这种简单的多步动力学模型也能解释等转化分析所揭示的聚合反应的一般特征,即有效活化能随转化率的变化和有效反应模型的自催化特性。对引发反应的速率常数 ki 和传播反应的速率常数 kp 进行了评估。结果表明,ki 的值比 kp 的值低约小数点后两位,这表明在所研究的温度范围内,起始速度较慢。
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引用次数: 0
Kinetics and mechanism of thermal and thermo-oxidative degradation for high-density polyethylene modified by fullerene and its derivative 富勒烯及其衍生物改性高密度聚乙烯的热降解和热氧化降解动力学与机理
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-24 DOI: 10.1016/j.tca.2024.179871
Bingtao Wang , Yanqun Pan , Liping Zhao , Juan Li , Zhenghong Guo
To investigate the effect of fullerene (C60) and its iron compound (C60-Fe) on the thermal and thermo-oxidative degradation mechanism of high-density polyethylene (HDPE), the Kissinger method, Flynn-Wall-Ozawa method and Coats-Redfern methods are used. The data of thermal and thermo-oxidative degradation are achieved through the thermogravimetric (TG) analysis, and the trapping free-radical ability and the dispersion of C60 or C60-Fe in matrix are characterized by the electron spin resonance (ESR) and transmission electron microscopy (TEM). C60 and C60-Fe improve effectively the thermal and thermo-oxidative stability of HDPE. In N2, C60 and C60-Fe do not change the degradation mechanism of HDPE, and the degradation rate is determined by the random generation and growth of free-radicals. In air, C60 changes the reaction order (n) of HDPE at the oxidation stage and the degradation mechanism at the random fracture. C60-Fe changes the thermo-oxidative mechanism of HDPE due to the formation of cross-linked network.
为了研究富勒烯(C60)及其铁化合物(C60-Fe)对高密度聚乙烯(HDPE)热降解和热氧化降解机理的影响,采用了基辛格法、Flynn-Wall-Ozawa 法和 Coats-Redfern 法。热重(TG)分析获得了热降解和热氧化降解的数据,电子自旋共振(ESR)和透射电子显微镜(TEM)表征了 C60 或 C60-Fe 在基体中捕获自由基的能力和分散性。C60 和 C60-Fe 能有效提高高密度聚乙烯的热稳定性和热氧化稳定性。在氮气中,C60 和 C60-Fe 不会改变高密度聚乙烯的降解机理,降解速率由自由基的随机生成和增长决定。在空气中,C60 改变了高密度聚乙烯氧化阶段的反应顺序(n)和随机断裂的降解机理。由于形成了交联网络,C60-Fe 改变了高密度聚乙烯的热氧化机理。
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引用次数: 0
Pyrolysis kinetics and flame retardant enhancement of bio-based polyamide 56/6 生物基聚酰胺 56/6 的热解动力学和阻燃性能的提高
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-21 DOI: 10.1016/j.tca.2024.179869
Xiaoqi Zhang , Haoyu Yang , Yaxin Guo , Jie Zhou , Hao Liu , Suqin He , Miaoming Huang , Wanlin Xu , Chengshen Zhu , Wentao Liu
The development of polyamide materials with fire safety is of great importance at this stage. A novel nitrogen-phosphorus bisystem flame retardant (MC) with a multi-branched structure was synthesized and applied to a new bio-based polyamide 56/6 (PA56/6). Notably, at 8 wt% MC content, flame-retardant PA56/6@MC8% (FRPA56/6@MC8%) achieved an Limiting Oxygen Index (LOI) of 26.6% and a V-0 rating in UL-94 tests. Cone calorimetry results indicated that FRPA56/6@MC8% exhibited a 22.9% reduction in total heat release (THR) and a 41.0% decrease in peak heat release rate (PHRR), underscoring the flame retardancy promotion by MC in PA56/6. The study further explored the pyrolysis kinetics and mechanisms of polyamide materials, offering insights crucial for flame-retardant modifications. Overall, the findings present an innovative strategy for enhancing the flame retardant properties of PA56/6, potentially applicable in automotive components and other pertinent fields.
现阶段,开发具有防火安全性的聚酰胺材料具有重要意义。研究人员合成了一种具有多分支结构的新型氮磷双体系阻燃剂(MC),并将其应用于新型生物基聚酰胺 56/6(PA56/6)。值得注意的是,在 MC 含量为 8 wt% 时,阻燃 PA56/6@MC8% (FRPA56/6@MC8%)的极限氧指数(LOI)达到 26.6%,在 UL-94 测试中达到 V-0 级。锥形量热仪结果表明,FRPA56/6@MC8% 的总放热量 (THR) 降低了 22.9%,峰值放热率 (PHRR) 降低了 41.0%,突出表明了 MC 在 PA56/6 中的阻燃性能。该研究进一步探讨了聚酰胺材料的热解动力学和机理,为阻燃改性提供了至关重要的见解。总之,研究结果提出了一种增强 PA56/6 阻燃性能的创新策略,可用于汽车部件和其他相关领域。
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引用次数: 0
Flammability of Novolac epoxy cured with aromatic diamines 用芳香族二胺固化的 Novolac 环氧树脂的可燃性
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-19 DOI: 10.1016/j.tca.2024.179870
Mauro R.S. Silveira , Vicente F. Moritz , Carlos A. Ferreira , Laurent Ferry , José-Marie Lopez-Cuesta
The modification of Novolac epoxy with the organophosphorus compound 9,10-dihydro-9-oxa-10-phosphaphenanthren-10-oxide (DOPO) to reduce flammability and its influence on curing reactions has been investigated. Three aromatic diamine curing agents were used, namely 4,4′-diaminodiphenylmethane (DDM), 4,4′-diaminodiphenylsulphone (DDS), and diethyltoluenediamine (DETDA). The thermal stability and dynamic-mechanical behaviour of the cured resin depend on interactions of the curing agent with DOPO. The onset degradation temperature decreased with increasing phosphorus content, indicating the influence of DOPO on thermal stability. The DDM 3 %P sample exhibited the highest glass transition (Tg) of 136 °C, while DDS-crosslinked simples displayed the highest Tg of 147 °C among all samples. An improvement in the reaction of Novolac epoxy to fire was achieved by incorporating DOPO compound, as indicated by cone calorimetry results, showing up to a 67 % reduction in the peak heat release rate (pHRR) and 53 % reduction in total heat release (THR) for DDM 3 %P. The modified samples containing DOPO presented a self-extinguishing performance, displaying a UL-94 V-0 rating and a limiting oxygen index (LOI) values reached a maximum of 37.1 % for DDM 3 %P, with less flame propagation than for neat Novolac epoxy.
研究了用有机磷化合物 9,10-二氢-9-氧杂-10-磷菲-10-氧化物(DOPO)对 Novolac 环氧树脂进行改性以降低易燃性及其对固化反应的影响。使用了三种芳香族二胺固化剂,即 4,4′-二氨基二苯甲烷(DDM)、4,4′-二氨基二苯砜(DDS)和二乙基甲苯二胺(DETDA)。固化树脂的热稳定性和动态机械性能取决于固化剂与 DOPO 的相互作用。起始降解温度随着磷含量的增加而降低,这表明 DOPO 对热稳定性有影响。DDM 3 %P 样品的玻璃化转变温度(Tg)最高,为 136 °C,而在所有样品中,DDS 交联模拟物的玻璃化转变温度(Tg)最高,为 147 °C。锥形量热仪结果表明,加入 DOPO 化合物后,Novolac 环氧树脂的着火反应有所改善,DDM 3 %P 的峰值放热率(pHRR)降低了 67%,总放热率(THR)降低了 53%。含有 DOPO 的改性样品具有自熄灭性能,达到了 UL-94 V-0 等级,DDM 3 %P 的极限氧指数(LOI)值最高达到 37.1%,与纯净的 Novolac 环氧树脂相比,火焰蔓延更小。
{"title":"Flammability of Novolac epoxy cured with aromatic diamines","authors":"Mauro R.S. Silveira ,&nbsp;Vicente F. Moritz ,&nbsp;Carlos A. Ferreira ,&nbsp;Laurent Ferry ,&nbsp;José-Marie Lopez-Cuesta","doi":"10.1016/j.tca.2024.179870","DOIUrl":"10.1016/j.tca.2024.179870","url":null,"abstract":"<div><div>The modification of Novolac epoxy with the organophosphorus compound 9,10-dihydro-9-oxa-10-phosphaphenanthren-10-oxide (DOPO) to reduce flammability and its influence on curing reactions has been investigated. Three aromatic diamine curing agents were used, namely 4,4′-diaminodiphenylmethane (DDM), 4,4′-diaminodiphenylsulphone (DDS), and diethyltoluenediamine (DETDA). The thermal stability and dynamic-mechanical behaviour of the cured resin depend on interactions of the curing agent with DOPO. The onset degradation temperature decreased with increasing phosphorus content, indicating the influence of DOPO on thermal stability. The DDM 3 %P sample exhibited the highest glass transition (Tg) of 136 °C, while DDS-crosslinked simples displayed the highest Tg of 147 °C among all samples. An improvement in the reaction of Novolac epoxy to fire was achieved by incorporating DOPO compound, as indicated by cone calorimetry results, showing up to a 67 % reduction in the peak heat release rate (pHRR) and 53 % reduction in total heat release (THR) for DDM 3 %P. The modified samples containing DOPO presented a self-extinguishing performance, displaying a UL-94 V-0 rating and a limiting oxygen index (LOI) values reached a maximum of 37.1 % for DDM 3 %P, with less flame propagation than for neat Novolac epoxy.</div></div>","PeriodicalId":23058,"journal":{"name":"Thermochimica Acta","volume":"741 ","pages":"Article 179870"},"PeriodicalIF":3.1,"publicationDate":"2024-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142312810","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Organic compounds as temperature calibrants for fast scanning calorimetry 用作快速扫描量热仪温度校准器的有机化合物
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-14 DOI: 10.1016/j.tca.2024.179868
Timur A. Mukhametzyanov , Airat A. Notfullin , Alisa A. Fatkhutdinova , Christoph Schick

Organic compounds can be used as temperature calibrants in fast scanning calorimetry. Their advantages include ease of surface cleaning of the calorimetric chip and good thermal contact with the chip surface. Among several compounds tested, benzoic acid was identified as a convenient and reliable calibrant for temperatures below approximately 130 °C. However, organic calibrants often exhibit unusual heating rate dependencies of the onset temperatures of melting. This phenomenon can be semi-quantitatively explained by considering different heat flows within the sensor. Notably, the thermal resistance between the heater and thermopile, often overlooked, introduces an additional time constant that can sometimes result in a negative apparent thermal lag. In addition, the onset temperatures are influenced by factors such as sample position, thickness, surface wetting, and spreading. These factors limit the accuracy of transition temperature determinations to approximately ±1 K below 130 °C and ±5 K up to 220 °C.

有机化合物可用作快速扫描量热仪的温度校准器。有机化合物的优点包括易于清洁量热芯片的表面以及与芯片表面良好的热接触。在测试的几种化合物中,苯甲酸被认为是温度低于约 130 °C 时方便可靠的校准物。然而,有机定标物在开始熔化的温度上往往表现出不寻常的加热速率依赖性。考虑到传感器内的不同热流,这种现象可以得到半定量的解释。值得注意的是,加热器和热电堆之间的热阻经常被忽视,它会带来一个额外的时间常数,有时会导致负的表观热滞后。此外,起始温度还受到样品位置、厚度、表面润湿和扩散等因素的影响。这些因素将过渡温度测定的精确度限制在 130 °C 以下约 ±1 K 和 220 °C 以下 ±5 K。
{"title":"Organic compounds as temperature calibrants for fast scanning calorimetry","authors":"Timur A. Mukhametzyanov ,&nbsp;Airat A. Notfullin ,&nbsp;Alisa A. Fatkhutdinova ,&nbsp;Christoph Schick","doi":"10.1016/j.tca.2024.179868","DOIUrl":"10.1016/j.tca.2024.179868","url":null,"abstract":"<div><p>Organic compounds can be used as temperature calibrants in fast scanning calorimetry. Their advantages include ease of surface cleaning of the calorimetric chip and good thermal contact with the chip surface. Among several compounds tested, benzoic acid was identified as a convenient and reliable calibrant for temperatures below approximately 130 °C. However, organic calibrants often exhibit unusual heating rate dependencies of the onset temperatures of melting. This phenomenon can be semi-quantitatively explained by considering different heat flows within the sensor. Notably, the thermal resistance between the heater and thermopile, often overlooked, introduces an additional time constant that can sometimes result in a negative apparent thermal lag. In addition, the onset temperatures are influenced by factors such as sample position, thickness, surface wetting, and spreading. These factors limit the accuracy of transition temperature determinations to approximately ±1 K below 130 °C and ±5 K up to 220 °C.</p></div>","PeriodicalId":23058,"journal":{"name":"Thermochimica Acta","volume":"741 ","pages":"Article 179868"},"PeriodicalIF":3.1,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142240431","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Secondary crystallization of low-isotacticity polypropylene 低异构聚丙烯的二次结晶
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-14 DOI: 10.1016/j.tca.2024.179867
Yoshitomo Furushima , Akihiko Toda , Kazuo Kimura , Masaru Nakada , Akihiro Masuda , Kazuya Nakamura , Hideaki Takahashi , Toshiumi Tatsuki , Kazuma Okada , Masatoshi Ohkura

This study aimed to clarify the secondary crystallization process of low-isotacticity polypropylene (LT-PP). LT-PP demonstrates an exceptionally low crystallization rate at room temperature, which is approximately 1/5000 lower than that of isotactic PP (iPP). During the secondary crystallization of LT-PP at 30 °C, the thickness of lamellar (c-axis) and a- and b-axes of crystallite size remained constant. In addition, no significant change was observed in the CC-C bending vibration. It seems that the direction of the CC-C molecular order is similar to the thickness direction. This vibration mode may be associated with changes in the thickness of the lamellae. To explain the log(t) dependence of crystallinity, the Seto–Frank model was employed.

本研究旨在阐明低异构聚丙烯(LT-PP)的二次结晶过程。LT-PP 在室温下的结晶速率极低,比同轴聚丙烯(iPP)低约 1/5000。LT-PP 在 30 °C 的二次结晶过程中,片层厚度(c 轴)以及结晶尺寸的 a 轴和 b 轴保持不变。此外,CC-C 弯曲振动也没有发生明显变化。由此看来,CC-C 分子顺序的方向与厚度方向相似。这种振动模式可能与薄片厚度的变化有关。为了解释结晶度的对数(t)依赖性,我们采用了 Seto-Frank 模型。
{"title":"Secondary crystallization of low-isotacticity polypropylene","authors":"Yoshitomo Furushima ,&nbsp;Akihiko Toda ,&nbsp;Kazuo Kimura ,&nbsp;Masaru Nakada ,&nbsp;Akihiro Masuda ,&nbsp;Kazuya Nakamura ,&nbsp;Hideaki Takahashi ,&nbsp;Toshiumi Tatsuki ,&nbsp;Kazuma Okada ,&nbsp;Masatoshi Ohkura","doi":"10.1016/j.tca.2024.179867","DOIUrl":"10.1016/j.tca.2024.179867","url":null,"abstract":"<div><p>This study aimed to clarify the secondary crystallization process of low-isotacticity polypropylene (LT-PP). LT-PP demonstrates an exceptionally low crystallization rate at room temperature, which is approximately 1/5000 lower than that of isotactic PP (iPP). During the secondary crystallization of LT-PP at 30 °C, the thickness of lamellar (c-axis) and a- and b-axes of crystallite size remained constant. In addition, no significant change was observed in the C<img>C-C bending vibration. It seems that the direction of the C<img>C-C molecular order is similar to the thickness direction. This vibration mode may be associated with changes in the thickness of the lamellae. To explain the log(<em>t</em>) dependence of crystallinity, the Seto–Frank model was employed.</p></div>","PeriodicalId":23058,"journal":{"name":"Thermochimica Acta","volume":"741 ","pages":"Article 179867"},"PeriodicalIF":3.1,"publicationDate":"2024-09-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142240429","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Doping SrSnO3 perovskite with transition metals: Synthesis of double hydroxides, thermal decomposition, and pigment potential 用过渡金属掺杂 SrSnO3 包晶:双氢氧化物的合成、热分解和颜料潜力
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-12 DOI: 10.1016/j.tca.2024.179864
Žaneta Dohnalová, Jan Hroch, Nataliia Reinders, Jana Luxová, Petra Šulcová

The primary objective of this research is to explore the feasibility of synthesizing phase-pure perovskite SrSnO3 doped with transition metals and to evaluate the potential of these products as high-temperature inorganic pigments. The initial step in preparing perovskite powders with the general formula SrSn0.95M0.05O3-δ (M = Mn, Fe, Co, Ni) involved synthesizing SrSn0.95M0.05(OH)6 followed by its thermal decomposition. The thermal decomposition processes and the reaction pathway for perovskite formation were analyzed using thermal analysis and X-ray diffraction analysis. Single-phase products of beige SrSn0.95Fe0.05O3-δ and brown SrSn0.95Co0.05O3-δ were successfully obtained by calcining the precursors at 1,100 °C. In contrast, brown SrSn0.95Mn0.05O3-δ contained a phase impurity of SnO2 and doping with Ni ions resulted in a phase mixture of SrSnO3 and NiO. The pigment quality of the powders was assessed based on their color parameters, described using the CIE Lab system.

本研究的主要目的是探索合成掺杂过渡金属的相纯包晶 SrSnO3 的可行性,并评估这些产品作为高温无机颜料的潜力。制备通式为 SrSn0.95M0.05O3-δ(M = Mn、Fe、Co、Ni)的包晶粉末的第一步是合成 SrSn0.95M0.05(OH)6,然后进行热分解。热分析和 X 射线衍射分析对热分解过程和包晶形成的反应途径进行了分析。通过在 1100 ℃ 下煅烧前驱体,成功获得了米色 SrSn0.95Fe0.05O3-δ 和棕色 SrSn0.95Co0.05O3-δ 的单相产物。相比之下,棕色 SrSn0.95Mn0.05O3-δ 中含有 SnO2 相杂质,掺入 Ni 离子后会产生 SrSnO3 和 NiO 相混合物。这些粉末的颜料质量是根据其颜色参数进行评估的,颜色参数采用 CIE Lab 系统进行描述。
{"title":"Doping SrSnO3 perovskite with transition metals: Synthesis of double hydroxides, thermal decomposition, and pigment potential","authors":"Žaneta Dohnalová,&nbsp;Jan Hroch,&nbsp;Nataliia Reinders,&nbsp;Jana Luxová,&nbsp;Petra Šulcová","doi":"10.1016/j.tca.2024.179864","DOIUrl":"10.1016/j.tca.2024.179864","url":null,"abstract":"<div><p>The primary objective of this research is to explore the feasibility of synthesizing phase-pure perovskite SrSnO<sub>3</sub> doped with transition metals and to evaluate the potential of these products as high-temperature inorganic pigments. The initial step in preparing perovskite powders with the general formula SrSn<sub>0.95</sub>M<sub>0.05</sub>O<sub>3-δ</sub> (<em>M</em> = Mn, Fe, Co, Ni) involved synthesizing SrSn<sub>0.95</sub>M<sub>0.05</sub>(OH)<sub>6</sub> followed by its thermal decomposition. The thermal decomposition processes and the reaction pathway for perovskite formation were analyzed using thermal analysis and X-ray diffraction analysis. Single-phase products of beige SrSn<sub>0.95</sub>Fe<sub>0.05</sub>O<sub>3-δ</sub> and brown SrSn<sub>0.95</sub>Co<sub>0.05</sub>O<sub>3-δ</sub> were successfully obtained by calcining the precursors at 1,100 °C. In contrast, brown SrSn<sub>0.95</sub>Mn<sub>0.05</sub>O<sub>3-δ</sub> contained a phase impurity of SnO<sub>2</sub> and doping with Ni ions resulted in a phase mixture of SrSnO<sub>3</sub> and NiO. The pigment quality of the powders was assessed based on their color parameters, described using the CIE Lab system.</p></div>","PeriodicalId":23058,"journal":{"name":"Thermochimica Acta","volume":"741 ","pages":"Article 179864"},"PeriodicalIF":3.1,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142232862","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Thermal conductivity of epoxy/multilayered graphene composites prepared with different curing agents 使用不同固化剂制备的环氧树脂/多层石墨烯复合材料的导热性能
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-10 DOI: 10.1016/j.tca.2024.179866
Miyuki Harada, Masafumi Horimoto, Tomoki Tsukuda

Epoxy/multilayer graphene (ML-graphene) composites were prepared using different curing agents to control the graphene dispersion by changing the curing reactivity. With increasing initial reactivity, the aggregation size of the ML-graphene decreased and their thermal conductivity increased. In particular, the thermal conductivity of the composite prepared with p-phenylenediamine showed a maximum value of 1.46 W/(m·K) at 25 wt% ML-graphene loading because of the highest initial curing reactivity. The application of a magnetic field led to graphene alignment along the applied field, resulting in two times higher thermal conductivity than that of the corresponding system without magnetic field. The relationship between the interfacial affinity for epoxy/graphene and thermal conductivity was also investigated. As a result, resulting in a biphenyl epoxy composite showed higher thermal conductivity (6.17 W/(m·K)) than that of the bisphenol-A epoxy composite. This is derived that the π-conjugated and planar structure of biphenyl epoxy can easily interact with the surface of graphene.

使用不同的固化剂制备了环氧树脂/多层石墨烯(ML-石墨烯)复合材料,通过改变固化反应活性来控制石墨烯的分散。随着初始反应活性的增加,多层石墨烯的聚集尺寸减小,导热系数增加。特别是用对苯二胺制备的复合材料,由于初始固化反应活性最高,在石墨烯含量为 25 wt% 时,热导率达到最大值 1.46 W/(m-K)。磁场的施加导致石墨烯沿着施加的磁场排列,从而使热导率比相应的无磁场体系高出两倍。此外,还研究了环氧树脂/石墨烯界面亲和性与导热性之间的关系。结果表明,联苯环氧复合材料的热导率(6.17 W/(m-K))高于双酚 A 环氧复合材料。这说明联苯环氧的 π 共轭和平面结构很容易与石墨烯表面相互作用。
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引用次数: 0
Experimental investigation and thermodynamic modeling for isobaric heat capacity of ethanol at elevated temperatures and pressures 高温高压下乙醇等压热容的实验研究和热力学建模
IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Pub Date : 2024-09-10 DOI: 10.1016/j.tca.2024.179865
Lingyan Gui , Jian Yang , Jiangtao Wu , Xianyang Meng

Ethanol is a promising sustainable fuel for its environmental friendliness and renewability. Due to the association effect in ethanol molecules, the particular behavior in isobaric heat capacity was explored by combining experimental and theoretical methods. Experimental isobaric heat capacity measurements of ethanol were performed over the temperature range from (298.15 to 573.15) K and at pressures up to 15 MPa in both liquid and vapor phases by a flow calorimeter. Different association schemes were combined respectively with PC-SAFT equation of state and SAFT-VR Mie equation of state to compare their accuracy in isobaric heat capacity prediction, and it could be concluded that two-site (2B) model was better than three-site (3B) model. It was also found that PC-SAFT equation of state was able to yield good results in predicting the isobaric heat capacity far from the saturated state and critical region, however, SAFT-VR Mie equation of state showed better prediction performance near the saturated state and critical region.

乙醇具有环境友好性和可再生性,是一种前景广阔的可持续燃料。由于乙醇分子中的关联效应,研究人员结合实验和理论方法探索了乙醇等压热容的特殊行为。使用流动热量计对乙醇进行了等压热容量实验测量,测量温度范围为 298.15 至 573.15 K,测量压力为 15 MPa,测量条件包括液相和气相。将不同的关联方案分别与 PC-SAFT 状态方程和 SAFT-VR Mie 状态方程相结合,比较了它们在等压热容预测中的准确性,得出的结论是双位点(2B)模型优于三位点(3B)模型。研究还发现,PC-SAFT 状态方程在预测远离饱和状态和临界区域的等压热容时能产生良好的结果,而 SAFT-VR Mie 状态方程在预测接近饱和状态和临界区域的等压热容时表现更好。
{"title":"Experimental investigation and thermodynamic modeling for isobaric heat capacity of ethanol at elevated temperatures and pressures","authors":"Lingyan Gui ,&nbsp;Jian Yang ,&nbsp;Jiangtao Wu ,&nbsp;Xianyang Meng","doi":"10.1016/j.tca.2024.179865","DOIUrl":"10.1016/j.tca.2024.179865","url":null,"abstract":"<div><p>Ethanol is a promising sustainable fuel for its environmental friendliness and renewability. Due to the association effect in ethanol molecules, the particular behavior in isobaric heat capacity was explored by combining experimental and theoretical methods. Experimental isobaric heat capacity measurements of ethanol were performed over the temperature range from (298.15 to 573.15) K and at pressures up to 15 MPa in both liquid and vapor phases by a flow calorimeter. Different association schemes were combined respectively with PC-SAFT equation of state and SAFT-VR Mie equation of state to compare their accuracy in isobaric heat capacity prediction, and it could be concluded that two-site (2B) model was better than three-site (3B) model. It was also found that PC-SAFT equation of state was able to yield good results in predicting the isobaric heat capacity far from the saturated state and critical region, however, SAFT-VR Mie equation of state showed better prediction performance near the saturated state and critical region.</p></div>","PeriodicalId":23058,"journal":{"name":"Thermochimica Acta","volume":"741 ","pages":"Article 179865"},"PeriodicalIF":3.1,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142229086","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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Thermochimica Acta
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