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Features of forming a low-temperature cubic Li7La3Zr2O12 film by tape casting 通过胶带浇铸形成低温立方 Li7La3Zr2O12 薄膜的特点
Q4 Materials Science Pub Date : 2023-11-21 DOI: 10.15826/chimtech.2023.10.4.09
E. Lyalin, Larisa Pershina, Evgeniy a Il’ina, Konstantin Druzhinin, Semen Belyakov
Currently, interest to lithium and lithium-ion all-solid-state power sources is rapidly growing all over the world. However, several issues should be addressed before all-solid-state batteries production: high resistance values of the solid electrolyte membrane and poor contact between electrolyte and electrode materials. The transition to thin-film technologies is one of the promising ways to solve these problems. Tape casting can be proposed to obtain thin-film solid electrolytes. In this research, the features of the structure formation, morphology and lithium-ion conductivity of Li7La3Zr2O12 films were investigated. Li7La3Zr2O12 films with the thickness of 35 µm were obtained by tape casting on Ni substrate. The influence of organic components’ content on homogeneous coatings formation was established. Heat treatment conditions for dried films were chosen based on differential scanning calorimetry and optical dilatometry. Phase change from tetragonal to low-temperature cubic modification occurs after annealing the Li7La3Zr2O12 films at 700 °C and higher. The annealed Li7La3Zr2O12 films have developed surface, which can lead to improved contact between the solid electrolyte and an electrode in an electrochemical cell. Li7La3Zr2O12 films annealed at 800 °C have the highest lithium-ion conductivity values (2.5·10–7 and 1.5·10–5 S·cm–1 at 90 and 215 °С, respectively). The technology of Li7La3Zr2O12 films formation with the thickness of ~23 µm by tape casting was developed.
目前,全世界对锂和锂离子全固态电源的兴趣正在迅速增长。然而,在生产全固态电池之前,有几个问题需要解决:固体电解质膜的电阻值过高以及电解质和电极材料之间的接触不良。向薄膜技术过渡是解决这些问题的可行方法之一。为获得薄膜固态电解质,可建议采用带式浇注法。本研究考察了 Li7La3Zr2O12 薄膜的结构形成、形貌和锂离子电导率特征。在镍基底上通过胶带浇铸获得了厚度为 35 µm 的 Li7La3Zr2O12 薄膜。确定了有机成分含量对均匀涂层形成的影响。根据差示扫描量热法和光学扩张仪选择了干燥薄膜的热处理条件。在 700 °C 或更高温度下退火后,Li7La3Zr2O12 薄膜发生了从四方到低温立方的相变。退火后的 Li7La3Zr2O12 薄膜具有发达的表面,可改善电化学电池中固体电解质与电极之间的接触。在 800 °C 下退火的 Li7La3Zr2O12 薄膜具有最高的锂离子电导率值(在 90 °С 和 215 °С 下分别为 2.5-10-7 和 1.5-10-5 S-cm-1)。通过胶带浇铸法形成厚度约为 23 µm 的 Li7La3Zr2O12 薄膜的技术已经开发成功。
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引用次数: 0
Kinetics of nitric acid leaching of bornite and chalcopyrite 用硝酸浸出辉锑矿和黄铜矿的动力学原理
Q4 Materials Science Pub Date : 2023-11-16 DOI: 10.15826/chimtech.2023.10.4.10
Yuri Shklyaev, O. Dizer, Tatyana Lugovitskaya, D. Golovkin, Denis Rogozhnikov
The paper presents a study of the process of nitric acid dissolution of the natural minerals chalcopyrite and bornite. The influence of various parameters, including temperature, nitric acid concentration and particle sizes, on this process was examined. Based on the data obtained, the values of apparent activation energy (57.41 and 42.98 kJ/mol for chalcopyrite and bornite, respectively), empirical orders with respect to nitric acid (1.62 and 1.57 for chalcopyrite and bornite, respectively) and with respect to particle size (–1.16 and –2.53 for chalcopyrite and bornite, respectively) were calculated using the shrinking core model. Generalized kinetic equations for the dissolution process of both minerals were derived. Based on the calculations performed, it was suggested that the dissolution processes of chalcopyrite and bornite under these conditions are limited by internal diffusion.
本文研究了天然矿物黄铜矿和辉铜矿的硝酸溶解过程。研究了温度、硝酸浓度和颗粒大小等各种参数对这一过程的影响。根据所获得的数据,利用缩核模型计算了表观活化能值(黄铜矿和辉铜矿分别为 57.41 和 42.98 kJ/mol)、与硝酸有关的经验阶数(黄铜矿和辉铜矿分别为 1.62 和 1.57)以及与粒度有关的经验阶数(黄铜矿和辉铜矿分别为 -1.16 和 -2.53)。得出了这两种矿物溶解过程的通用动力学方程。根据计算结果,黄铜矿和辉铜矿在这些条件下的溶解过程受到内部扩散的限制。
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引用次数: 0
Colloid-chemical properties of surfactant–nitric acid–water systems 表面活性剂-硝酸-水体系的胶体-化学特性
Q4 Materials Science Pub Date : 2023-11-03 DOI: 10.15826/chimtech.2023.10.4.08
Lev Danilin, Tatyana Lugovitskaya, Elvira Kolmachikhina, Denis Rogozhnikov
The behavior of the surfactants Tween 80, SaS and alkyl betaine in aqueous and nitric acid environments as promising additives for nitrate leaching of hard-to-process ore concentrates of non-ferrous metals was studied. The influence of surfactant concentration (0.04–1.28 g/dm3), nitric acid concentration (0.1–10 g/dm3) and temperature (295–343 K) on the surface tension, critical micelle concentration (CMC), pH and optical density of aqueous surfactant solutions and surfactant–HNO3–H2O systems was found. The critical micelle concentration of the surfactants used was estimated. A positive effect of nitric acid on the surface activity of surfactants was discovered, which manifests itself in a decrease in both the CMC and the surface tension at the liquid–gas interface. The values of surface activity and Gibbs energy of surfactant micelle formation in aqueous and nitric acid media were calculated. Associative processes in the solutions and compositions were confirmed by measuring the optical density of the systems under study.
研究了表面活性剂吐温 80、SaS 和烷基甜菜碱在水环境和硝酸环境中的行为,这些表面活性剂可作为添加剂用于难处理有色金属精矿的硝酸盐浸出。研究发现了表面活性剂浓度(0.04-1.28 g/dm3)、硝酸浓度(0.1-10 g/dm3)和温度(295-343 K)对表面活性剂水溶液和表面活性剂-HNO3-H2O 系统的表面张力、临界胶束浓度(CMC)、pH 值和光密度的影响。估算了所用表面活性剂的临界胶束浓度。发现硝酸对表面活性剂的表面活性有积极影响,表现为 CMC 和液气界面表面张力的降低。计算了表面活性剂在水介质和硝酸介质中形成胶束的表面活性值和吉布斯能。通过测量所研究体系的光密度,确认了溶液和组合物中的缔合过程。
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引用次数: 0
Facile synthesis of lanthanum-doped SrTiO3 nanocubes mediated by cetyltrimethylammonium bromide and tert-butylamine under solvothermal condition and their tunable electrical properties 溶剂热条件下十六烷基三甲基溴化铵和叔丁胺介导的镧掺杂SrTiO3纳米立方的快速合成及其可调电学性能
Q4 Materials Science Pub Date : 2023-10-26 DOI: 10.15826/chimtech.2023.10.4.07
Yulia Eka Putri, Humaira Faradilla, Dedi Satria, Diana Vanda Wellia
The electrical conductivity of low concentrations of lanthanum-doped SrTiO3 nanocube ceramics synthesized using the facile solvothermal method in mixed organic and inorganic solvents with cetyltrimethylammonium bromide (CTAB) as a capping agent and tert-butyl amine (TBA) as a mineralizer was investigated. X-ray diffraction patterns confirmed the formation of a high-purity perovskite phase, corresponding to the standard data and the pattern refinement results. The particles of the sample were nanocubes, whereas the La-doped SrTiO3 sample particles were more uniform in size and shape, as shown in TEM images. The FT-IR spectrum confirmed the vibration of the CH3-N+ groups from CTAB and TBA, indicating an electrostatic interaction between their functional groups and the particle surface. Substitution of La3+ ions at low concentrations increased electrical conductivity compared to the undoped SrTiO3 sample. Lanthanum donates excess electrons, thereby increasing the number of electron carriers, which causes a reduction in the band gap energy according to the UV-DRS spectrum analysis using the Tauc equation.
以十六烷基三甲基溴化铵(CTAB)为封盖剂,叔丁基胺(TBA)为矿化剂,采用易溶溶剂热法制备了低浓度掺镧SrTiO3纳米立方陶瓷,研究了其在有机和无机混合溶剂中的电导率。x射线衍射图证实了高纯度钙钛矿相的形成,与标准数据和图精结果相对应。TEM图像显示,样品的颗粒为纳米立方体,而la掺杂的SrTiO3样品颗粒在尺寸和形状上更为均匀。FT-IR光谱证实了CTAB和TBA的CH3-N+基团的振动,表明它们的官能团与颗粒表面之间存在静电相互作用。与未掺杂的SrTiO3样品相比,低浓度的La3+离子取代提高了电导率。根据使用Tauc方程的UV-DRS光谱分析,镧提供了多余的电子,从而增加了电子载流子的数量,从而导致带隙能量的降低。
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引用次数: 0
Corrigendum to The impact of dimethylformamide on the synthesis of graphene quantum dots derived from graphene oxide 二甲基甲酰胺对由氧化石墨烯衍生的石墨烯量子点合成的影响的更正
Q4 Materials Science Pub Date : 2023-10-26 DOI: 10.15826/chimtech.2023.10.4.06
Khuong T. Truong, Thach H. Pham, Khai V. Tran
The original article, “Khuong T. Truong, Thach H. Pham, Khai V. Tran. The impact of dimethylformamide on the synthesis of graphene quantum dots derived from graphene oxide. Chimica Techno Acta. 2023;10(4):202310405”, is available at: https://doi.org/10.15826/chimtech.2023.10.4.05
原文:“Khuong T. Truong, Thach H. Pham, Khai V. Tran。二甲基甲酰胺对氧化石墨烯衍生的石墨烯量子点合成的影响。中国科技学报,2023;10(4):202310405”,下载网址:https://doi.org/10.15826/chimtech.2023.10.4.05
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引用次数: 0
Features of calcium hexaaluminate formation in alumina-zirconia ceramics 氧化铝-氧化锆陶瓷中六铝酸钙形成的特征
Q4 Materials Science Pub Date : 2023-10-26 DOI: 10.15826/chimtech.2023.10.3.17
Nina Cherkasova, Kristina Antropova, Ruslan Kuzmin, Kemal Emurlaev, Ivanna Kuchumova, Nomina Burkhinova, Yulia Zobova
Alumina-zirconia composites containing calcium hexaaluminate in the amount from 0 to 15 wt.% were investigated. The materials were obtained by water dispersion, granulation, axial pressing, and free sintering. Density and open porosity were determined by the hydrostatic weighing method. Phase analysis was performed using synchrotron radiation. Structural investigations were conducted using scanning and transmission electron microscopy. Vickers hardness was determined at a load of 10 kg. Fracture toughness was determined by the indentation method. With increasing CaAl12O19 content in the composites, the relative density decreased from 98.5% to 91.8%, and the open porosity increased from 0.2 to 1.4%. The lattice parameters of t-ZrO2 crystal lattice did not change up to 12 wt.% CaAl12O19, and the degree of tetragonality was 1.435. The degree of tetragonality decreased for the material with 15 wt.% CaAl12O19 and reached 1.420. The lattice parameters of CaAl12O19 decreased with increasing content. Platelet size increased with increasing calcium hexaaluminate content. For the materials containing up to 9 wt.% CaAl12O19, the average length of the platelets was 2 μm, the width was 0.4 μm, and the aspect ratio was 5. For the material with maximum calcium hexaaluminate content, the average length of the platelets was 4.2 μm, the width was 0.6 μm, and the aspect ratio was 7. With increasing CaAl12O19 content, the hardness decreased from 1700±25 to 1390±30 Hv, and the critical stress intensity factor increased by 34% to 6.7±0.3 MPa·m1/2.
研究了六铝酸钙含量为0 ~ 15wt %的氧化铝-氧化锆复合材料。物料经水分散、造粒、轴压、自由烧结等工艺得到。采用流体静力称重法测定密度和开孔率。用同步辐射进行相位分析。利用扫描电镜和透射电镜对其结构进行了研究。在10kg载荷下测定维氏硬度。用压痕法测定断裂韧性。随着CaAl12O19含量的增加,复合材料的相对密度从98.5%降低到91.8%,孔隙率从0.2%提高到1.4%。当CaAl12O19含量达到12 wt.%时,t-ZrO2的晶格参数没有变化,正方度为1.435。当CaAl12O19质量分数为15 wt.%时,材料的四边形度下降,达到1.420。CaAl12O19的晶格参数随含量的增加而降低。血小板大小随六铝酸钙含量的增加而增加。当CaAl12O19含量高达9 wt.%时,血小板的平均长度为2 μm,宽度为0.4 μm,长径比为5。对于六铝酸钙含量最高的材料,血小板的平均长度为4.2 μm,宽度为0.6 μm,长径比为7。随着CaAl12O19含量的增加,合金硬度从1700±25 Hv下降到1390±30 Hv,临界应力强度因子增加34%,达到6.7±0.3 MPa·m1/2。
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引用次数: 0
Influence of the powders phase composition and sintering atmosphere on the structure and magnetic properties of Mn-Zn ferrites 粉末相组成和烧结气氛对Mn-Zn铁氧体结构和磁性能的影响
Q4 Materials Science Pub Date : 2023-10-23 DOI: 10.15826/chimtech.2023.10.3.16
Ruslan Kuzmin, Roman Khabirov, Anna Mass, Elena Lozhkina
The magnetic properties of Mn-Zn ferrites depend strongly on the microstructure, chemical and phase composition. In this paper the effect of synthesis and sintering conditions on the structure, phase composition and properties of Mn-Zn ferrites is investigated. The specimens for the study were obtained by pressureless sintering. The magnetic properties were measured on a B-H analyzer. The structure was investigated by XRD and SEM. Materials with an average grain size of 2.2 μm were obtained by sintering at a temperature of 1265 °C. It was found that an increase in the synthesis temperature from 700 to 1000 °C promotes the growth of the initial magnetic permeability of these materials from 1100 to 1370. The rapid cooling of the powders synthesized at 1000 °C allows maintaining a high content of the spinel phase. In the structure of materials obtained by sintering powders with initially high spinel content at 1300 °C, grains of abnormally large size are formed. This leads to an increase in the initial permeability, magnetic induction at Hm = 1200 A/m, f = 10 kHz and magnetic losses at high frequencies (up to 500 kHz). A material with fine-grained structure was obtained by using air at the heating stage of pressureless sintering. This contributed to the reduction of magnetic losses without a significant decrease in Bm.
锰锌铁氧体的磁性能很大程度上取决于其微观结构、化学成分和相组成。本文研究了合成条件和烧结条件对锰锌铁氧体结构、相组成和性能的影响。研究用的试样是通过无压烧结得到的。在B-H分析仪上测量了磁性能。采用XRD和SEM对其结构进行了表征。在1265℃的温度下烧结得到平均晶粒尺寸为2.2 μm的材料。结果表明,当合成温度从700℃升高到1000℃时,材料的初始磁导率从1100℃升高到1370℃。在1000℃下快速冷却合成的粉末可以保持高含量的尖晶石相。在1300℃烧结初始尖晶石含量高的粉末得到的材料结构中,形成了异常大的晶粒。这导致初始磁导率增加,Hm = 1200 A/m时的磁感应强度增加,f = 10 kHz,高频(高达500 kHz)时的磁损耗增加。在无压烧结的加热阶段,利用空气获得了具有细晶粒结构的材料。这有助于减少磁损耗,而不显著降低Bm。
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引用次数: 0
Structural transformations and their impact on the mechanical and antifriction properties in the process of alloying graphitized hypereutectoid steel with copper 石墨化过共析钢与铜合金化过程中的组织转变及其对力学性能和抗摩擦性能的影响
Q4 Materials Science Pub Date : 2023-10-20 DOI: 10.15826/chimtech.2023.10.3.15
Natalia V. Stepanova, Elena A. Lozhkina
The purpose of the work is to develop a cast antifriction material based on an iron-carbon alloy with a high copper content for use in large, heavy duty sliding friction units. Using the casting method in self-hardening liquid glass mixtures, two specimens of hypereutectoid graphitized steel with different copper contents (0.09 and 8.76 wt.%) were produced. To obtain graphite in the steel structure, modification with the silicocalcium (SiCa) was used. The microstructural examination was carried out using optical metallography, SEM and TEM methods. The impact of copper on the structure as well as the mechanical and antifriction properties of graphitized hypereutectoid steel was studied. It was found that adding 8.76 wt.% of copper to the steel composition leads to an increase in the Brinell hardness level of the material from 250 to 300 HB, ultimate tensile strength from 250 to 380 MPa and compressive strength from 1050 to 1200 MPa, which is associated with an increase in the microhardness of pearlite from 350 to 420 HV. To assess the impact of copper on the sliding friction coefficient of graphitized hypereutectoid steel, a curve of sliding friction coefficient vs applied load was plotted; the experiment was carried out according to the liner-on-disk scheme. The wear resistance of materials under sliding friction conditions was also assessed using this method. Copper alloying has a positive effect on the wear resistance of graphitized hypereutectoid steel by increasing the mechanical properties of the material and also by reducing the level of the sliding friction coefficient under boundary lubrication conditions.
这项工作的目的是开发一种基于高铜含量的铁碳合金的铸造减摩材料,用于大型重型滑动摩擦装置。采用自硬化玻璃液混合物浇铸的方法,制备了铜含量(0.09和8.76 wt.%)不同的过共析石墨化钢试样。为了在钢结构中获得石墨,采用了硅钙改性的方法。采用光学金相、扫描电镜和透射电镜等方法进行了显微组织分析。研究了铜对石墨化过共析钢组织、力学性能和抗摩擦性能的影响。结果表明,在钢中添加8.76 wt.%的铜可使材料的布氏硬度从250提高到300 HB,抗拉强度从250提高到380 MPa,抗压强度从1050提高到1200 MPa,珠光体显微硬度从350提高到420 HV。为了评估铜对石墨化过共析钢滑动摩擦系数的影响,绘制了滑动摩擦系数随外加载荷的变化曲线;实验采用磁盘衬垫方案进行。采用该方法对材料在滑动摩擦条件下的耐磨性进行了评价。铜合金通过提高材料的力学性能和降低边界润滑条件下的滑动摩擦系数水平,对石墨化过共析钢的耐磨性有积极的影响。
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引用次数: 0
Effect of sintering duration on structure and properties of Ni-Al metal-intermetallic composites produced by SPS 烧结时间对SPS制备的Ni-Al金属间化合物复合材料组织和性能的影响
Q4 Materials Science Pub Date : 2023-10-12 DOI: 10.15826/chimtech.2023.10.3.14
Tatiana Ogneva, Alexander Anisimov, Ruslan Kuzmin, Andrey Tyurin, Yulia Emurlaeva, Natalya Aleksandrova
The fabrication of Ni-Al based metal-intermetallic layered (MIL) composites is one of the actively developing directions in the production of materials for aircraft and space industries. Alternating hard intermetallic layers with ductile metal layers provides a unique combination of mechanical properties. In this study, metal-intermetallic layered composites consisting of Ni and nickel aluminides were fabricated using spark plasma sintering (SPS) of Ni and Al foils 100 and 25 μm in thickness, respectively. Samples sintered at 1100 °C for 0.5, 3, and 8 min were obtained. The purpose of this study was to fabricate Ni-Al MIL composites with increased strength properties using SPS technique and to investigate the effect of sintering duration on structure and properties. The structure of the samples sintered for 0.5 min consisted of Ni layers and intermetallic layers containing the sublayers with stoichiometric and Ni-rich B2 NiAl, L10 twinned martensite NiAl. The tensile strength of such composites was 485 MPa. The intermetallic layers in the sample sintered for 3 min have more Ni-rich NiAl, martensite NiAl, and Ni3Al phases, which promoted to an increase in tensile strength to 575 MPa. The sample sintered for 8 min consisted of Ni and a solid solution of Al in Ni and showed the highest tensile strength, 610 MPa, due to solid solution hardening in the interlayers. The samples did not break when applying bending load, which is the evidence of the good reliability and durability of the composites.
镍铝基金属间层状复合材料的制备是航空航天材料生产中积极发展的方向之一。交替的硬质金属间层和韧性金属层提供了独特的机械性能组合。采用火花等离子烧结技术,分别制备了厚度为100 μm和25 μm的Ni和Al箔,制备了镍和镍铝化物金属间层状复合材料。在1100℃下烧结0.5、3、8 min得到样品。本研究的目的是利用SPS技术制备具有更高强度性能的Ni-Al MIL复合材料,并研究烧结时间对其结构和性能的影响。烧结0.5 min后,样品的结构由Ni层和含有富Ni的B2 NiAl、L10孪晶NiAl亚层的金属间层组成。该复合材料的抗拉强度为485 MPa。烧结3min后的金属间层中含有较多的富ni NiAl、马氏体NiAl和Ni3Al相,抗拉强度提高到575 MPa。烧结8min后,试样由Ni和Al在Ni中的固溶体组成,由于层间的固溶体硬化,试样的抗拉强度最高,达到610 MPa。在弯曲载荷作用下,试样未发生断裂,证明复合材料具有良好的可靠性和耐久性。
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引用次数: 0
The impact of dimethylformamide on the synthesis of graphene quantum dots derived from graphene oxide 二甲基甲酰胺对氧化石墨烯衍生的石墨烯量子点合成的影响
Q4 Materials Science Pub Date : 2023-10-10 DOI: 10.15826/chimtech.2023.10.4.05
Khuong T. Truong, Thach H. Pham, Khai V. Tran
Graphene quantum dots (GQDs) have garnered immense interest in recent years due to their unique optical, electrical, and chemical properties, making them promising candidates for various applications in optoelectronics, bioimaging, and sensing. However, enhancing the control over the size, surface chemistry, and optical properties of GQDs remains a significant challenge. In this study, a novel recipe was proposed to successfully synthesize various GQDs via a typical solvothermal process, which has proven to be a versatile and scalable approach. In addition to the main ingredient – graphene oxide suspension, dimethylformamide (DMF) and hydrogen peroxide serving as a cutting agent were added to the reaction mixture. This synthesis method was found to be more promising than the reference one in which DMF was replaced by double distilled water. Through systematic experimentation, we demonstrated that the addition of DMF enables the successful GQD production over a wider range of reaction times; hence, the UV absorption band and photoluminescence properties of GQDs can be better adjusted. The dependence of photoluminescence on the excitation wavelength was observed in the as-prepared materials as they were excited with a range of wavelengths from 360 to 480 nm. The obtained insights not only advance our understanding of GQD synthesis but also open up avenues for tailoring their properties for specific applications.
石墨烯量子点(GQDs)由于其独特的光学、电学和化学性质,近年来引起了人们的极大兴趣,使其成为光电子、生物成像和传感等各种应用的有希望的候选者。然而,增强对GQDs的尺寸、表面化学和光学性质的控制仍然是一个重大挑战。本研究提出了一种新的方法,通过典型的溶剂热法成功合成了多种GQDs,该方法具有通用性和可扩展性。除了主要成分氧化石墨烯悬浮液外,还将二甲酰胺(DMF)和过氧化氢作为切削剂加入到反应混合物中。与用双蒸馏水代替DMF的合成方法相比,该合成方法更有前景。通过系统实验,我们证明添加DMF可以在更大的反应时间范围内成功地生产GQD;因此,可以更好地调节GQDs的紫外吸收带和光致发光性能。在360 ~ 480nm的激发波长范围内,观察到所制备材料的光致发光与激发波长的关系。获得的见解不仅促进了我们对GQD合成的理解,而且为定制特定应用的特性开辟了途径。
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引用次数: 0
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Chimica Techno Acta
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