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Selective removal of dolomite from rare earth element-bearing phosphorite by flotation and leaching and the adsorption mechanism of agents on mineral surfaces 浮选浸出法选择性去除含稀土磷矿中的白云石及药剂在矿物表面的吸附机理
IF 1.7 4区 化学 Q2 Chemistry Pub Date : 2023-11-21 DOI: 10.1002/sia.7271
Jun Xie
The rare earth elements (REEs)-bearing phosphorite was a potential REE resource, which contained all REEs except polonium, among them lanthanide, cerium, neodymium, and yttrium were especially enriched. REEs mainly occurred in fluorapatite (Fap) and had a high positive correlation with phosphorus content. By adopting a new green environmental fatty acid collector GJBW and through one roughing and one refining reverse flotation process, all REEs were pre-enriched. The flotation concentrate was further leached with citric acid (CA), and all REEs were further enriched. The results of X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS) showed that dolomite (Dolo) was removed and Fap was enriched in phosphorite, the selective enrichment of phosphorus and REEs was realized. Density functional theory (DFT) calculation revealed the mechanism of deep purification of REEs and phosphorus in phosphorite by CA at the micro-scale. The results showed that the number and strength of bonding between CA and Dolo (104) surface were greater than that between CA and Fap (001) surface, and CA was more easily adsorbed on Dolo (104) surface. Under the same conditions, Dolo in phosphorite was more easily leached by CA, while Fap was further enriched. This process provided a theoretical basis for the comprehensive recovery of REEs and phosphorus from phosphorite.
含稀土磷矿是一种潜在的稀土资源,除钋外,其余稀土元素均富集,其中镧系元素、铈、钕和钇富集。稀土元素主要赋存于氟磷灰石(Fap)中,与磷含量呈高度正相关。采用新型绿色环保型脂肪酸捕收剂GJBW,通过1粗1精反浮选工艺,对所有稀土元素进行了预富集。浮选精矿用柠檬酸(CA)进一步浸出,所有稀土元素进一步富集。x射线衍射仪(XRD)、傅里叶变换红外光谱(FT-IR)和x射线光电子能谱(XPS)分析结果表明,磷矿中白云石(Dolo)被去除,Fap富集,实现了磷和稀土的选择性富集。密度泛函理论(DFT)计算揭示了微尺度CA深度净化磷矿中稀土和磷的机理。结果表明,CA与Dolo(104)表面的结合次数和强度大于CA与Fap(001)表面的结合次数和强度,CA更容易吸附在Dolo(104)表面。在相同条件下,磷酸矿中的Dolo更容易被CA浸出,而Fap则进一步富集。该工艺为磷矿中稀土和磷的综合回收提供了理论依据。
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引用次数: 0
Surface analysis insight note: An example of a cluster analysis of spectra from an X-ray photoelectron spectroscopy image 表面分析洞察注:x射线光电子能谱图像的光谱聚类分析示例
IF 1.7 4区 化学 Q2 Chemistry Pub Date : 2023-11-14 DOI: 10.1002/sia.7270
Behnam Moeini, John M. Linford, Neal Gallagher, Matthew R. Linford
Identification of similar and dissimilar spectra is an important part of analyzing X-ray photoelectron spectroscopy (XPS) images. Cluster analysis (CA) is a commonly used exploratory data analysis (EDA) method that groups similar spectra in a data set. CA can be performed in either an agglomerative fashion, for example, using Ward's method, which involves successively linking together/clustering the most similar spectra in a data set, or in a divisive fashion, for example, using the K-means approach, which involves partitioning all the data into a specified number of clusters. In this note, we show the application of CA to an XPS image dataset. The use of Ward's method identified two major clusters in the image, where one of the clusters appeared as two subclusters. The K-means image based on two clusters agrees well with previous analyses of the same image. The average spectra corresponding to clusters helped confirm the assignments made by the CA algorithms, as did a multivariate curve resolution (MCR) analysis of the interior region identified in our cluster analysis. “Elbow” plots can help determine the number of clusters to keep in K-means clustering. The combination of the agglomerative and divisive forms of CA, where the first informs the second, can be effective in revealing the structures of XPS image datasets. The Procrustean bed is a metaphor for overfitting and underfitting in EDA.
相似和不同光谱的识别是分析x射线光电子能谱(XPS)图像的重要组成部分。聚类分析(CA)是一种常用的探索性数据分析(EDA)方法,它将数据集中相似的光谱进行分组。CA可以以聚集方式执行,例如,使用Ward的方法,它涉及到将数据集中最相似的光谱依次连接在一起/聚类,或者以分裂方式执行,例如,使用K-means方法,它涉及到将所有数据划分到指定数量的聚类中。在本文中,我们将展示CA对XPS图像数据集的应用程序。使用Ward的方法在图像中识别出两个主要簇,其中一个簇以两个子簇的形式出现。基于两个聚类的K-means图像与先前对同一图像的分析非常吻合。与聚类对应的平均光谱有助于确认CA算法所做的分配,正如我们在聚类分析中确定的内部区域的多元曲线分辨率(MCR)分析一样。“肘形”图可以帮助确定K-means聚类中需要保留的聚类数量。CA的凝聚和分裂形式的结合,其中第一种形式通知第二种形式,可以有效地揭示XPS图像数据集的结构。Procrustean床是EDA中过拟合和欠拟合的隐喻。
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引用次数: 0
The effect of electrophoretic deposition of carbon nanotubes on carbon fiber on interfacial properties of the thermoplastic polyimide composite 碳纳米管在碳纤维表面电泳沉积对热塑性聚酰亚胺复合材料界面性能的影响
4区 化学 Q2 Chemistry Pub Date : 2023-11-11 DOI: 10.1002/sia.7272
Li Jian
In order to improve the interfacial properties of carbon fiber/polyimide (CF/PI) composite, silanization reaction carbon nanotubes (CNTs) were introduced to the surface of carbon fiber by electrophoretic deposition to prepare CF/CNT/PI composite. The effects of carbon fiber surface treatment on the mechanical properties of the composites were studied. The results showed that the interlaminar shear strength and bending strength of the composite materials were increased by 11% and 9%, respectively. The scanning electron microscope and Atomic Force Microscope (AFM) was used to analyze the fine structure of composite interface phase. The results show that the introduction of CNTs creates an interface transition layer of CNTs reinforced PI resin between the fiber and the matrix.
为了提高碳纤维/聚酰亚胺(CF/PI)复合材料的界面性能,采用电泳沉积的方法在碳纤维表面引入硅烷化反应碳纳米管(CNTs)制备CF/CNT/PI复合材料。研究了碳纤维表面处理对复合材料力学性能的影响。结果表明,复合材料的层间剪切强度和弯曲强度分别提高了11%和9%。采用扫描电镜和原子力显微镜(AFM)对复合材料界面相的精细结构进行分析。结果表明,CNTs的引入在纤维和基体之间形成了CNTs增强PI树脂的界面过渡层。
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引用次数: 0
Comparing three strategies for surface treatment of Mg coated by hexamethylene diamine tetra methylene phosphonic acid for corrosion protection 比较了六亚乙二胺四亚甲基膦酸包覆镁合金的三种防腐处理策略
4区 化学 Q2 Chemistry Pub Date : 2023-11-10 DOI: 10.1002/sia.7269
Hanaa Soliman, Fatma Abdel Mouez, Hoda Hussien, Abdel Salam Makhlouf, Guojiang Wan
Manufacturing Mg and Mg‐based alloys with controllable degradation rate has always been a challenge. Surface modification is one of the best ways to acquire protection against corrosion. Previously, many approaches such as phosphating (Na 3 PO 4 ), fluoridation (HF), and alkalization (NaOH) treatments have been used to regulate the corrosion rate. Here, we compare the corrosion rates of 3‐surface modified Mg samples coated with hexamethylene diamine tetra methylene phosphonic (HMDTMPA). The protection of those different layers was ranked in the order: phosphate > alkaline > fluoridation treatment. The chemistry of those chemical conversion layers was discussed in the light of scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), and X‐ray photoelectron spectroscopy (XPS). The mechanism of tailoring a protective film of HMDTMPA on phosphated Mg was discussed according to the ability of P to bridge the substrate with the coating.
制造降解率可控的镁和镁基合金一直是一个挑战。表面改性是获得抗腐蚀保护的最好方法之一。以前,许多方法,如磷化(na3po4)、氟化(HF)和碱化(NaOH)处理已被用来调节腐蚀速率。在这里,我们比较了三表面改性Mg样品涂覆六亚乙二胺四亚甲基膦(HMDTMPA)的腐蚀速率。这些不同层的保护顺序是:磷酸盐>碱性比;氟化反应治疗。利用扫描电子显微镜(SEM)、傅里叶变换红外光谱(FTIR)和X射线光电子能谱(XPS)分析了这些化学转化层的化学性质。根据磷与涂层的桥接能力,探讨了在磷酸镁表面制备HMDTMPA保护膜的机理。
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引用次数: 0
Deep core level hard X‐ray photoelectron spectroscopy for catalyst characterization 催化剂表征的深核级硬X射线光电子能谱
4区 化学 Q2 Chemistry Pub Date : 2023-11-07 DOI: 10.1002/sia.7267
Filippo Longo, Marin Nikolic, Andreas Borgschulte
Abstract Heterogeneous catalysts are the crucial element for many catalytic processes. In most of the cases, the pivotal structure consists of catalytic metals/alloy particles supported by oxides. Knowledge of the interaction between metal and oxide is central to understand the structure–performance relationship of such systems. X‐ray photoelectron spectroscopy provides access to the chemical–physical properties of metal and oxide interface as well as polarization effects. The results are usually derived from changes of the measured binding energies based on initial state analysis. We propose to extend the analysis using photoelectron as well as Auger transition to include final state effects (Wagner/Hohlneichner plots). This gives additional information on the specific chemical neighborhood of the excited atom. Three archetypal systems are investigated by hard X‐ray photoelectron spectroscopy (HAXPES) to introduce two approaches to this analysis for the most common support elements Al and Si.
摘要非均相催化剂是许多催化过程的关键因素。在大多数情况下,关键结构由氧化物支撑的催化金属/合金颗粒组成。了解金属和氧化物之间的相互作用对于理解这类体系的结构-性能关系至关重要。X射线光电子能谱提供了金属和氧化物界面的化学物理性质以及极化效应的途径。结果通常是基于初始态分析的测量结合能的变化而得出的。我们建议扩展使用光电子和俄歇跃迁的分析,以包括最终态效应(Wagner/Hohlneichner图)。这就提供了关于受激原子的特定化学邻域的额外信息。通过硬X射线光电子能谱(HAXPES)研究了三个原型系统,介绍了两种方法来分析最常见的支持元素Al和Si。
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引用次数: 0
Synthesis and characterization of iron sulfide immobilized on Algerian halloysite clay (HKDD3) with enhanced removal of methylene blue from aqueous medium 阿尔及利亚高岭土黏土(HKDD3)固定化硫化铁的合成及对亚甲基蓝的去除效果研究
4区 化学 Q2 Chemistry Pub Date : 2023-11-07 DOI: 10.1002/sia.7268
Asma Hayoune, Hocine Akkari, Marcello Marelli, Valeria Pappalardo, Jia Yang, Muhammad Zubair
The aim of this study is to functionalize an Algerian halloysite clay (kaolin Djebel Debbagh, HKDD3) with FeS nanoparticles by employing a hydrothermal approach and exploring its ability to remove methylene blue under visible light irradiation. The FeS‐HKDD3 photocatalyst was synthesized successfully and exhibited good crystallinity. Different techniques were used to characterize the produced photocatalyst, including XRD, STEM/EDS, TEM, BET, and UV–vis DRS in order to investigate its structure, morphology, and optical performance. The HKDD3 is a natural halloysite having a tubular shape with a length ranging from 500 nm to several micrometers and a diameter that is estimated from 50 to 100 nm. The iron sulfide nanoparticles are immobilized as cube aggregates on the surface of the halloysite. The visible range displayed a strong absorption of the obtained photocatalyst, with an estimated bandgap of 1.60 eV, according to UV–vis DRS findings. The results exhibited a higher efficiency toward synergic adsorption‐photocatalytic degradation effect for methylene blue dye removal.
本研究的目的是利用水热方法将阿尔及利亚高岭土粘土(高岭土Djebel Debbagh, HKDD3)与FeS纳米颗粒功能化,并探索其在可见光照射下去除亚甲基蓝的能力。成功合成了FeS - HKDD3光催化剂,并表现出良好的结晶度。采用XRD、STEM/EDS、TEM、BET、UV-vis DRS等技术对制备的光催化剂进行表征,考察其结构、形貌和光学性能。HKDD3是一种天然高岭土,呈管状,长度为500纳米至几微米,直径约为50至100纳米。硫化铁纳米颗粒以立方体聚集体的形式固定在高岭土表面。根据UV-vis DRS的发现,在可见光范围内显示出对所获得的光催化剂的强吸收,估计带隙为1.60 eV。结果表明,该材料具有较高的协同吸附-光催化降解亚甲基蓝染料的效果。
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引用次数: 0
Fabrication of molecularly imprinted polymer‐based interdigital sensor for L‐ascorbic acid L -抗坏血酸分子印迹聚合物数字间传感器的制备
4区 化学 Q2 Chemistry Pub Date : 2023-11-07 DOI: 10.1002/sia.7266
Muafia Akbar, Nauman Sadiq, Memoona Shakoor, Muhammad Shafique, Anum Tahir, Muhammad Zahid, Ghulam Mustafa
The level of L‐ascorbic acid (AA) in various natural and artificial foods, medicines and other substances must be determined for biological and agricultural purposes. In this study, an AA‐imprinted poly (methacrylic acid)‐based receptor was synthesized by thermal free‐radical bulk polymerization for the detection of ascorbic acid using the methacrylic acid as monomer, ethylene glycol dimethacrylate (EGDMA) as cross‐linker, and azobisisobutyronitrile (AIBN) as initiator, in the presence of a porogenic solvent dimethyl sulfoxide (DMSO). The synthesized molecularly imprinted polymer (MIP) was used as a receptor. Immobilization of the receptor layer on IDEs provided a suitable sensor for AA detection by measuring changes in electrical parameters including inductance, capacitance, and resistance with the help of LCR meter. In the series and parallel inductance, the lowest detection limits were 0.13 and 0.001 ppm, respectively. While, for series and parallel capacitance, the lowest detection limits were 0.01548 and 1.3698 ppm, respectively. In the case of resistance, the lowest limit of detection was 0.0076 and 0.08121 ppm in series and parallel, respectively. The imprinted polymer‐based sensor showed sensitivity, selectivity, and reversibility for ascorbic acid.
L -抗坏血酸(AA)在各种天然和人工食品、药品和其他物质中的含量必须用于生物和农业目的。本研究以甲基丙烯酸为单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,偶氮二异丁腈(AIBN)为引发剂,在致孔溶剂二甲亚砜(DMSO)的存在下,采用热自由基本体聚合法制备了AA印迹聚甲基丙烯酸基受体,用于检测抗坏血酸。合成的分子印迹聚合物(MIP)作为受体。将受体层固定在IDEs上,通过LCR计测量电感、电容、电阻等电参数的变化,为AA检测提供了合适的传感器。在串联和并联电感中,最低检出限分别为0.13 ppm和0.001 ppm。串联电容和并联电容的最低检出限分别为0.01548 ppm和1.3698 ppm。在电阻情况下,串联和并联的最低检出限分别为0.0076和0.08121 ppm。印迹聚合物传感器对抗坏血酸具有灵敏度、选择性和可逆性。
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引用次数: 0
Comparative investigation on organosilicon film growth by cyclonic plasma using hexamethyldisilazane and hexamethyldisilazane/nitrogen gas mixture 六亚甲基二氮氮和六亚甲基二氮氮/氮气混合物在旋流等离子体中生长有机硅薄膜的比较研究
4区 化学 Q2 Chemistry Pub Date : 2023-10-29 DOI: 10.1002/sia.7263
Li‐Yu Wu, Shu‐Mei Wang, Ya‐Shin Ji, Chun Huang
This study aimed to discover the surface characteristics of cyclonic plasma‐deposited films and the effect of nitrogen gas addition. The influence of nitrogen gas addition on the surface characteristics of organosilicon films in hexamethyldisilazane (HMDSN) and HMDSN/nitrogen (HMDSN/N 2 ) cyclonic plasmas at atmospheric pressure was evaluated. It was found that the addition of nitrogen gas is a crucial factor affecting organosilicon film growth in the plasma cyclone in one atmosphere. SEM, AFM, and ATR‐FTIR results indicated that on adding nitrogen gas, the surface morphology became rougher, the peak corresponding to the Si–O–Si group was detected at approximately 1050 cm −1 , the degree of porosity was relatively low, and the proportion of the SiCHx group decreased. In general, the surface energies of the films deposited in the HMDSN discharge and the HMDSN/N 2 gas mixture discharge exhibited similar features. SEM and AFM evaluations showed high roughness values of 44.5 nm for the film formation in the HMDSN/N 2 gas mixture discharge, while the films grown in the HMDSN discharge exhibited a relatively flat surface with a roughness of 24.5 nm. Based on ATR‐FTIR detection, cyclonic plasma‐deposited films deposited in the HMDSN discharge obtained organic moieties, while the films generated in the HMDSN/N 2 gas mixture discharge exhibited strong Si–O–Si absorption signals. A possible nano‐organosilicon film growth that prevails in atmospheric pressure plasma deposition is proposed based on atmospheric‐pressure plasma chemistry, nitrogen gas addition, and experimental observations.
本研究旨在探讨旋流等离子体沉积膜的表面特性及氮气的加入对膜的影响。研究了常压下氮气加入对六甲基二氮杂烷(HMDSN)和HMDSN/氮气(HMDSN/ n2)旋风等离子体中有机硅膜表面特性的影响。结果表明,氮气的加入是影响等离子体旋风中有机硅膜生长的关键因素。SEM、AFM和ATR‐FTIR结果表明,加入氮气后,表面形貌变得粗糙,Si-O-Si基团对应的峰出现在约1050 cm−1处,孔隙度相对较低,SiCHx基团的比例下降。总的来说,HMDSN放电和HMDSN/ n2气体混合放电中沉积的膜的表面能表现出相似的特征。SEM和AFM评价表明,HMDSN/ n2气体混合放电形成的膜具有44.5 nm的高粗糙度,而HMDSN放电生长的膜具有相对平坦的表面,粗糙度为24.5 nm。基于ATR - FTIR检测,HMDSN放电中沉积的旋流等离子体沉积膜获得了有机部分,而HMDSN/ n2气体混合放电中生成的膜表现出强烈的Si-O-Si吸收信号。基于常压等离子体化学、氮气添加和实验观察,提出了常压等离子体沉积中普遍存在的一种可能的纳米有机硅膜生长。
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引用次数: 0
Chemical functionality of surfaces for the characteristic adsorption of melamine 三聚氰胺特性吸附表面的化学功能
4区 化学 Q2 Chemistry Pub Date : 2023-10-25 DOI: 10.1002/sia.7265
Mohit Tiwari, Sudip K. Pattanayek
The surface functionality leading to a high reversibility adsorption of melamine was determined. Four different silane coupling agents, namely, 3‐(tri‐methoxysilyl) propyl methacrylate (TMSPMA), n‐propyl tri‐methoxy‐silane (PTMS), 3‐(tri‐ethoxysilyl) propionitrile (TESPN), and tri‐methoxy‐(octadecyl) silane (OTMS) were taken for making chemical functionality methacrylate, short methyl, nitrile, and extended methyl group respectively. The adsorption behavior of melamine over the substrates with four functionalities was determined using quartz crystal microbalance (QCM). The adsorption kinetics and adsorption isotherms of the adsorption studies were analyzed. The initial adsorption rate depends on the hydrophobicity and roughness of the surfaces. However, the subsequent adsorption rate depends on the specific interaction. The data of equilibrium adsorbed mass at various equilibrium concentrations were fitted with the modified Brunauer–Emmett–Teller (BET) and Freundlich adsorption isotherms. The estimated model parameters were analyzed and compared with the reported parameters of the relevant systems. There is good agreement between our results and the reported results. In addition, very high adsorption with a very high binding constant was observed for the adsorption of melamine OTMS surface. On the other hand, high adsorption with an intermediate layer binding constant for the adsorption of melamine on the methacrylate surface was observed. Based on this, we propose using acrylate chemical functionality to develop molecularly imprinted polymer‐based melamine sensors.
测定了导致三聚氰胺高可逆性吸附的表面官能团。采用3‐(三甲氧基硅基)甲基丙烯酸丙酯(TMSPMA)、正丙基三甲氧基硅烷(PTMS)、3‐(三乙氧基硅基)丙腈(TESPN)和三甲氧基十八烷基硅烷(OTMS)四种不同的硅烷偶联剂,分别制备了化学官能团甲基丙烯酸酯、短甲基、腈基和扩展甲基。用石英晶体微天平(QCM)测定了三聚氰胺在四种官能团底物上的吸附行为。分析了吸附动力学和吸附等温线。初始吸附速率取决于表面的疏水性和粗糙度。然而,随后的吸附速率取决于特定的相互作用。用改进的brunauer - emmet - teller (BET)吸附等温线和Freundlich吸附等温线拟合不同平衡浓度下的平衡吸附质量数据。对估计的模型参数进行了分析,并与相关系统的报告参数进行了比较。我们的结果和报道的结果吻合得很好。此外,三聚氰胺在OTMS表面的吸附具有很高的吸附常数。另一方面,对三聚氰胺在甲基丙烯酸酯表面的吸附具有较高的吸附性。在此基础上,我们提出利用丙烯酸酯化学功能开发分子印迹聚合物基三聚氰胺传感器。
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引用次数: 0
Large‐area growth of monolayer MoS2 by using atmospheric‐pressure chemical vapor deposition with nucleation controlling process 常压化学气相沉积法在成核控制过程中大面积生长单层MoS2
4区 化学 Q2 Chemistry Pub Date : 2023-10-23 DOI: 10.1002/sia.7264
Binbin Ding, Changjun Zhu, Tianming Wang, Lianbi Li, Zebin Li, Lin Cheng, Song Feng, Guoqing Zhang, Yuan Zang, Jichao Hu, Lei Li, Caijuan Xia
The epitaxial growth of high‐quality and large‐area monolayer (ML) MoS 2 has attracted widespread attention in recent years. Here, MoS 2 on Al 2 O 3 substrate was prepared by using atmospheric‐pressure chemical vapor deposition. The process parameters such as temperature difference and distance between MoO 3 and Al 2 O 3 , nucleation temperature, and heating rate were optimized. The high MoO 3 evaporation temperature facilitates Mo vapor transport to grow ML‐MoS 2 . The introduction of nucleation temperature facilitates the deposition of MoS 2 , and the morphology of the nucleation point is related to the amount of MoO 3‐x deposited on Al 2 O 3 . This process optimization method is also applicable to growth MoS 2 on SiO 2 . The ML‐MoS 2 with a size greater than 1 cm 2 was successfully fabricated on Al 2 O 3 and SiO 2 , which laid a foundation for the practical application of ML‐MoS 2 .
近年来,高质量、大面积单层MoS 2的外延生长引起了广泛的关注。本文采用常压化学气相沉积的方法在al_2o_3衬底上制备了mos2。对moo3与al2o3之间的温差和距离、成核温度、加热速率等工艺参数进行了优化。较高的mo2o3蒸发温度有利于Mo蒸气输运生长ML - mo2o3。成核温度的引入有利于mo2o3的沉积,成核点的形貌与沉积在al2o3上的mo2o3的量有关。该工艺优化方法同样适用于在sio2上生长MoS 2。在al2o3和sio2上成功制备了尺寸大于1 cm 2的ML - MoS 2,为ML - MoS 2的实际应用奠定了基础。
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引用次数: 0
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Surface and Interface Analysis
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