Transmission Electron Energy Loss Spectroscopy Research Articles

Fabrication of 3D Nanocarbon Structure for Potential Sensor Applications

An all-carbon 3D nanocarbon structure has been designed and fabricated using carbon nanotubes (CNT) grown on multi-layer graphene (MLG). This work was motivated by the need of current integrated circuit (IC) technology to eventually replace copper (Cu) and tungsten (W) as interconnect materials. Such a structure can also potentially be part of a chemical or biological sensing system. Our experimental process consists of using a plasma-enhanced chemical vapor deposition (PECVD) process to grow CNT arrays directly on an MLG-covered silicon substrate after sputtering a thin nickel, iron, or cobalt (Co) catalyst film. The fabricated devices are evaluated and characterized through a combination of scanning electron microscopy and electrical measurements using a nanoprober. The PECVD process results in highly aligned but non-conductive CNT/Graphene structures due to damages in the graphene film during CNT growth. To mitigate this challenge, we successfully identified the source for graphene damage as the plasma in the CNT growth process and, as a result, replaced PECVD with a thermal CVD growth process. The resulting CNT/Graphene devices fabricated using Co as catalyst are conductive, with an estimated CNT-graphene contact resistance of 1.4 kΩ. Thus, we have taken the first step in demonstrating electrical conduction through an all-carbon, 3D nanostructure fabricated by growing CNTs directly on graphene. Further experimentation is currently underway to verify and improve upon our process, including in situ nanoprobing to fully characterize the electrical properties of these devices. In addition, we use a combination of transmission electron microscopy and electron energy loss spectroscopy to verify a homogenous interface between the CNT and MLG by demonstrating the continuation of C-C sp2 bonding. Independently, we are investigating the compatibility of our current process with other CNT growth catalysts. To achieve effective sensing, additional improvements are needed, such as vertical CNT alignment, high CNT areal density, and small average CNT diameter.

HRTEM and EELS investigations of flame-formed soot nanostructure

High resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS) were applied to soot probed along a premixed methane flame from the inception phase up to the burnout region in order to follow the transformations of soot nanostructures. The nascent methane soot presented the predominance of large coalesced disordered structures in comparison to young, intermediate and mature soot presenting spherule aggregates. Quantitative structural information describing the shape, size and orientation of sp2-bonded (aromatic) layers and their distribution inside the carbon particle were obtained by HRTEM image analysis. A moderate structural improvement in terms of a better stacking of longer and more planar layers along with the tortuosity fringe decrease was observed along the methane flame. EELS was instead used to provide quantitative information about the relative concentrations of sp3 and sp2 hybridized carbon. It is the first time that quantitative EELS is applied to soot from the inception to maturation along a premixed laminar flame. The aromatic content for the nascent soot resulted to be rather high (84%) indicating the predominant aromatic character of soot precursors. The steep increase of sp2 content from 84 to 94% in the passage from nascent to young soot was noteworthy. The similar sp2 content (94–96%) as well as the invariance of fringe length of young, intermediate and mature soot testified that most of the structural changes occurred at the inception, after then methane soot did not undergo a significant nanostructural restructuring, possibly because of the less reactive environment generated from methane combustion.

Atomic diffusion in laser irradiated Ge rich GeSbTe thin films for phase change memory applications

The atomic diffusion and compositional variations upon melting have been studied by transmission electron microscopy and electron energy loss spectroscopy in Ge rich GeSbTe films, with a composition optimized for memory applications. Melting and quenching has been achieved by laser pulses, in order to study pure thermal diffusion without electric field induced electromigration. The effect of different laser energy densities has been investigated. The diffusion of Ge atoms in the molten phase is found to be a prominent mechanism and, by employing finite elements computational analysis, a diffusion coefficient of Ge on the order of 5 × 10−5 cm2 s−1 has been estimated.

Effect of annealing on the structure and magnetic properties of Co2FeAl0.5Si0.5 thin films on Ge(111)

We present a magnetic and structural properties study of epitaxially grown B2-ordered full Heusler Co2FeSi0.5Al0.5 single crystal films on Ge(111) substrates, as a function of annealing temperature. Hysteresis loop measurements reveal that the magnetic properties of Co2FeSi0.5Al0.5 are stable up to 450 °C while ferromagnetic resonance linewidth measurements show a reduction of Gilbert damping from 5.6 × 10−3 to 2.9 × 10−3 for as-grown and annealed film, respectively. Above 500 °C, the films have increased coercivity, decreased saturation magnetisation, and show characteristic two-magnon scattering resonance line-shapes. Magnetic inhomogeneities developed within the film when annealed above 500 °C were correlated to significant interdiffusion at the film-substrate interface, as confirmed by scanning transmission electron microscopy and electron energy loss spectroscopy. By performing first-principles calculations based on atomistic models developed from atomically-resolved microscopy images, we show the magnetic moment of the Co2FeSi0.5Al0.5 film reduces upon Co substitution by Ge atoms.

B-site cation order/disorder and their valence states in Ba3MnNb2O9 perovskite oxide

Polycrystalline samples Ba3MnNb2O9 synthesized by solid state reaction and single crystal samples grown by optical floating zone have been characterized using scanning transmission electron microscopy and electron energy loss spectroscopy. Three types of B-site Mn and Nb ordering phase are observed: fully ordered 1Mn:2Nb; fully disordered; nano-sized 1Mn:1Nb ordered. No electronic structure change for crystals with different ordering/disordering. The Mn valence is determined to be 2+, and Nb valence is 5+. Oxygen 2p orbitals hybridize with Mn 3d and Nb 4d orbitals. Factors that affect the electron energy loss near edge structures of transition metal white-lines in electron energy loss spectroscopy are explicitly illustrated and discussed.

Imaging the atomic structure and local chemistry of platelets in natural type Ia diamond.

In the past decades, many efforts have been devoted to characterizing {001} platelet defects in type Ia diamond. It is known that N is concentrated at the defect core. However, an accurate description of the atomic structure of the defect and the role that N plays in it is still unknown. Here, by using aberration-corrected transmission electron microscopy and electron energy-loss spectroscopy we have determined the atomic arrangement within platelet defects in a natural type Ia diamond and matched it to a prevalent theoretical model. The platelet has an anisotropic atomic structure with a zigzag ordering of defect pairs along the defect line. The electron energy-loss near-edge fine structure of both carbon K- and nitrogen K-edges obtained from the platelet core is consistent with a trigonal bonding arrangement at interstitial sites. The experimental observations support an interstitial aggregate mode of formation for platelet defects in natural diamond.

Probing the Chemistry of Adhesion between a 316L Substrate and Spin-on-Glass Coating.

Hydrogen silsesquioxane ([HSiO3/2] n)-based "spin-on-glass" has been deposited on a 316L substrate and cured in Ar/H2 gas atmosphere at 600 °C to form a continuous surface coating with submicrometer thickness. The coating functionality depends primarily on the adhesion to the substrate, which is largely affected by the chemical interaction at the interface between the coating and the substrate. We have investigated this interface by transmission electron microscopy and electron energy loss spectroscopy. The analysis identified a 5-10 nm thick interaction zone containing signals from O, Si, Cr, and Fe. Analysis of the energy loss near edge structure of the present elements identified predominantly signal from [SiO4]4- units together with Fe2+, Cr2+, and traces of Cr3+. High-resolution transmission electron microscopy images of the interface region confirm a crystalline Fe2SiO4 interfacial region. In agreement with computational thermodynamics, it is proposed that the spin-on-glass forms a chemically bonded silicate-rich interaction zone with the substrate. It was further suggested that this zone is composed of a corundum-type oxide at the substrate surface, followed by an olivine-structure intermediate phase and a spinel-type oxide in the outer regions of the interfacial zone.

Intergranular amorphous films formed by DC electric field in pure zirconia

AbstractIt is difficult to obtain pure ZrO2 sintered compacts with a bulk style at room temperature because a large volumetric expansion from tetragonal to monoclinic phase (t/m) transformation occurs at around 1000°C, which is lower than the sintering temperature. In contrast, pure monoclinic ZrO2 can be consolidated without shattering using flash‐sintering at 1350°C for 5 minutes under an applied DC electric field of 175 V/cm. High‐resolution transmission electron microscopy and electron energy loss spectroscopy have revealed that amorphous films are formed along grain boundaries after flash‐sintering at 1350°C for 5 minutes. Monoclinic ZrO2 flash‐sintered compact including the amorphous films are able to survive without shattering through the t/m transformation, as the amorphous films partially absorb the large volumetric expansion arising from the t/m transformation. The formation of the amorphous films results from the severe reducing condition due to the applied DC electric fields during flash‐sintering.

Nanoanalytical electron microscopy of events predisposing to mineralisation of turkey tendon

The macro- and micro-structures of mineralised tissues hierarchy are well described and understood. However, investigation of their nanostructure is limited due to the intrinsic complexity of biological systems. Preceding transmission electron microscopy studies investigating mineralising tissues have not resolved fully the initial stages of mineral nucleation and growth within the collagen fibrils. In this study, analytical scanning transmission electron microscopy and electron energy-loss spectroscopy were employed to characterise the morphology, crystallinity and chemistry of the mineral at different stages of mineralization using a turkey tendon model. In the poorly mineralised regions, calcium ions associated with the collagen fibrils and ellipsoidal granules and larger clusters composed of amorphous calcium phosphate were detected. In the fully mineralised regions, the mineral had transformed into crystalline apatite with a plate-like morphology. A change in the nitrogen K-edge was observed and related to modifications of the functional groups associated with the mineralisation process. This transformation seen in the nitrogen K-edge might be an important step in maturation and mineralisation of collagen and lend fundamental insight into how tendon mineralises.

Identification and paleoclimatic significance of magnetite nanoparticles in soils

In the world-famous sediments of the Chinese Loess Plateau, fossil soils alternate with windblown dust layers to record monsoonal variations over the last ∼3 My. The less-weathered, weakly magnetic dust layers reflect drier, colder glaciations. The fossil soils (paleosols) contain variable concentrations of nanoscale, strongly magnetic iron oxides, formed in situ during the wetter, warmer interglaciations. Mineralogical identification of the magnetic soil oxides is essential for deciphering these key paleoclimatic records. Formation of magnetite, a mixed Fe2+/Fe3+ ferrimagnet, has been linked to soil redox oscillations, and thence to paleorainfall. An opposite hypothesis states that magnetite can only form if the soil is water saturated for significant periods in order for Fe3+ to be reduced to Fe2+, and suggests instead the temperature-dependent formation of maghemite, an Fe3+-oxide, much of which ages subsequently into hematite, typically aluminum substituted. This latter, oxidizing pathway would have been temperature, but not rainfall dependent. Here, through structural fingerprinting and scanning transmission electron microscopy and electron energy loss spectroscopy analysis, we prove that magnetite is the dominant soil-formed ferrite. Maghemite is present in lower concentrations, and shows no evidence of aluminum substitution, negating its proposed precursor role for the aluminum-substituted hematite prevalent in the paleosols. Magnetite dominance demonstrates that magnetite formation occurs in well-drained, generally oxidizing soils, and that soil wetting/drying oscillations drive the degree of soil magnetic enhancement. The magnetic variations of the Chinese Loess Plateau paleosols thus record changes in monsoonal rainfall, over timescales of millions of years.

Operando Raman spectroscopy on CO2 methanation over alumina-supported Ni, Ni3Fe and NiRh0.1 catalysts: Role of carbon formation as possible deactivation pathway

The methanation of CO2, as a part of the power-to-gas concept, was studied under various industrially relevant feed compositions with a focus on the formation and influence of carbonaceous species. For this purpose, 5 wt.% Ni/Al2O3, 5 wt.% Ni3Fe/Al2O3 and 3.4 wt.% NiRh0.1/Al2O3 catalysts were prepared and characterized by X-ray diffraction (XRD), temperature-programmed reduction (TPR), scanning transmission electron microscopy (STEM) combined with energy-dispersive X-ray spectroscopy (EDX) and electron energy loss spectroscopy (EELS). During the methanation of CO2, the Ni3Fe catalyst emerged as the most active and selective catalyst in the mid-temperature regime (300–350 °C). At 400 °C, all three tested catalysts showed high conversion of CO2 (67–75%; Ni > Ni3Fe > NiRh0.1) and selectivity towards CH4 (95–98%). Operando Raman spectroscopy was applied to elucidate the possible influence of carbonaceous species on the performance of the catalysts. Notably, no carbon deposition was observed under various feed compositions, even in CO2 or CO2/CH4 mixtures, e.g. as provided by biogas plants. Only in pure CH4 atmosphere an intensive carbon deposition with graphitic structure occurred as uncovered by operando Raman spectroscopy. Experiments in the lab-scale reactor and a spectroscopic microreactor could be correlated and revealed a strong catalytic deactivation of the carbon covered catalysts including a pronounced shift of the selectivity towards CO. The initial activity could be recovered after reactivation in H2 at elevated temperatures, which led to a removal of the deposits especially from the metal particles. Raman spectroscopy, supported by the results from high-resolution transmission electron microscopy (HRTEM) and EELS, revealed that carbon remained on the support material. The latter did not have any significant influence on the catalytic activity and could be removed in an oxidizing atmosphere.

Reduced interface spin polarization by antiferromagnetically coupled Mn segregated to the Co2MnSi /GaAs (001) interface

We have investigated the interfacial structure and its correlation with the calculated spin polarization in $\mathrm{C}{\mathrm{o}}_{2}\mathrm{MnSi}$/GaAs(001) lateral spin valves. $\mathrm{C}{\mathrm{o}}_{2}\mathrm{MnSi}$ (CMS) films were grown on As-terminated c($4\ifmmode\times\else\texttimes\fi{}4$) GaAs(100) by molecular beam epitaxy using different first atomic layers: MnSi, Co, and Mn. Atomically resolved $Z$-contrast scanning transmission electron microscopy (STEM) imaging and electron energy loss spectroscopy (EELS) were used to develop atomic structural models of the CMS/GaAs interfaces that were used as inputs for first-principles calculations to understand the magnetic and electronic properties of the interface. First-principles structures were relaxed and then validated by comparing experimental and simulated high-resolution STEM images. STEM-EELS results show that all three films have similar six atomic layer thick, Mn- and As-rich multilayer interfaces. However, the Co-initiated interface contains a $\mathrm{M}{\mathrm{n}}_{2}\mathrm{As}$-like layer, which is antiferromagnetic, and which is not present in the other two interfaces. Density functional theory calculations show a higher degree of interface spin polarization in the Mn- and MnSi-initiated cases, compared to the Co-initiated case, although none of the interfaces are half-metallic. The loss of half-metallicity is attributed, at least in part, to the segregation of Mn at the interface, which leads to the formation of interface states. The implications for the performance of lateral spin valves based on these interfaces are discussed briefly.

EPR Study of Porous Si:C and SiO2:C Layers

Initial porous silicon (por‐Si), carbonized porous silicon (por‐Si:C), and carbon‐incorporated porous silicon oxide (por‐SiO2:C) layers are studied by electron paramagnetic resonance (EPR) at T = 10–13 K. Scanning transmission electron microscopy and electron energy loss (EEL) spectroscopy show that por‐Si:C and por‐SiO2:C layers have a highly disordered structure with mixing sp2 and sp3 CC bonds. In the por‐SiO2:C layers, the peak of the oxygen bonded to carbon in the form of hydroxyl groups is found in the EEL spectrum of the C K‐edge region. Low‐intensity signals of Lorentzian lineshape are detected in the EPR spectrum of por‐Si, por‐Si:C, por‐SiO2:C layers. One of them is attributed to the Pb0 defect at the Si/SiO2 interface of nanocrystalline grain and the second to the silicon dangling bonds (SiDB) localized in nanocrystalline Si. The carbonization of por‐Si layers and subsequent oxidation of por‐Si:C gives rise to the appearance of additional EPR signals of high intensity at g = 2.0035(3) in por‐Si:C and at g = 2.0030(3) in por‐SiO2:C, which are assigned to carbon‐related defects (CRD) and carbon clusters, correspondingly. It was found that predominant defect types in por‐Si:C and por‐SiO2:C layers are CRD and carbon clusters, respectively, while the spin concentration of Pb0 interface defects and SiDB is low.

Sonochemical Preparation and Subsequent Fixation of Oxygen-Free Graphene Sheets at N,N-Dimethyloctylamine-Aqua Boundary

In this study, the syntheses of oxygen-free graphene sheets and the method of its fixation at an oil-aqua interface were presented. The graphene sheets were prepared by exfoliation of synthetic graphite powder in an aqua-organic medium under ultrasound irradiation. N,N-Dimethyloctylamine- (DMOA-) aqua emulsion was used as the liquid medium, and pH was equal to 3. The obtained graphene nanosuspension was fractionated by sedimentation and decanted according to the weight. The graphene nanoparticle fractions, differing in configuration and number of layers, have been characterized using transmission electron microscopy (TEM), electron diffraction, HRTEM, Raman spectroscopy, and electron energy loss spectroscopy (EELS). It was found that using a DMOA-aqua mixture as the liquid medium in ultrasonic treatment of synthetic graphite leads to the formation of oxygen-free 1-2-layer graphene sheets attached to the DMOA-aqua interface. The proposed method differs from known ones by using a small amount of more environmentally friendly organic substances. It allows to obtain large quantities of oxygen-free graphene, and finally unconverted graphite can be directed for reuse. The proposed method allows to obtain both 2D graphene sheets with micron linear dimensions and 3D packages with a high content of defects. Both these species are in demand in areas related to the development of new materials with unique electrophysical properties.

Quaternary Chalcogenide-Based Misfit Nanotubes LnS(Se)-TaS(Se)2 (Ln = La, Ce, Nd, and Ho): Synthesis and Atomic Structural Studies.

We have synthesized quaternary chalcogenide-based misfit nanotubes LnS(Se)-TaS2(Se) (Ln = La, Ce, Nd, and Ho). None of the compounds described here were reported in the literature as a bulk compound. The characterization of these nanotubes, at the atomic level, has been developed via different transmission electron microscopy techniques, including high-resolution scanning transmission electron microscopy, electron diffraction, and electron energy-loss spectroscopy. In particular, quantification at sub-nanometer scale was achieved by acquiring high-quality electron energy-loss spectra at high energy (∼between 1000 and 2500 eV). Remarkably, the sulfur was found to reside primarily in the distorted rocksalt LnS lattice, while the Se is associated with the hexagonal TaSe2 site. Consequently, these quaternary misfit layered compounds in the form of nanostructures possess a double superstructure of La/Ta and S/Se with the same periodicity. In addition, the interlayer spacing between the layers and the interatomic distances within the layer vary systematically in the nanotubes, showing clear reduction when going from the lightest (La atom) to the heaviest (Ho) atom. Amorphous layers, of different nature, were observed at the surface of the nanotubes. For La-based NTs, the thin external amorphous layer (inferior to 10 nm) can be ascribed to a Se deficiency. Contrarily, for Ho-based NTs, the thick amorphous layer (between 10 and 20 nm) is clearly ascribed to oxidation. All of these findings helped us to understand the atomic structure of these new compounds and nanotubes thereof.

Embedding MnO@Mn3 O4 Nanoparticles in an N-Doped-Carbon Framework Derived from Mn-Organic Clusters for Efficient Lithium Storage.

The first synthesis of MnO@Mn3 O4 nanoparticles embedded in an N-doped porous carbon framework (MnO@Mn3 O4 /NPCF) through pyrolysis of mixed-valent Mn8 clusters is reported. The unique features of MnO@Mn3 O4 /NPCF are derived from the distinct interfacial structure of the Mn8 clusters, implying a new methodological strategy for hybrids. The characteristics of MnO@Mn3 O4 are determined by conducting high angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and electron energy loss spectroscopy (EELS) valence-state analyses. Due to the combined advantages of MnO@Mn3 O4 , the uniform distribution, and the NPCF, MnO@Mn3 O4 /NPCF displays unprecedented lithium-storage performance (1500 mA h g-1 at 0.2 A g-1 over 270 cycles). Quantitative analysis reveals that capacitance and diffusion mechanisms account for Li+ storage, wherein the former dominates. First-principles calculations highlight the strong affiliation of MnO@Mn3 O4 and the NPCF, which favor structural stability. Meanwhile, defects of the NPCF decrease the diffusion energy barrier, thus enhancing the Li+ pseudocapacitive process, reversible capacity, and long cycling performance. This work presents a new methodology to construct composites for energy storage and conversion.

Microstructure Analysis of Neutron Absorber Al/B4C Metal Matrix Composites

The microstructure of Al/B4C metal matrix composites (MMCs) used as neutron absorbers in both dry storage casks and wet storage pools of spent nuclear fuel was analyzed by SEM and TEM. A polishing method of a focused Ga+ ion beam was used to obtain an ideal sample surface with very low roughness, which was used to statistically analyze the distribution characteristics and size factor of B4C particles in the aluminum matrix. The area of B4C particles mainly ranged from 0 to 0.5 μm2, which was the proportion of 64.29%, 86.99% and 76.86% of total statistical results for the Al-15%B4C, Al-25%B4C and Al-30%B4C MMCs, respectively. The average area of B4C particles in the Al-15%B4C, Al-25%B4C and Al-30%B4C MMCs were about 1.396, 0.528 and 1.183 μm2, respectively. The nanoscale precipitates were analyzed by the element mappings in scanning transmission electron microscopy (STEM) mode and electron energy loss spectroscopy (EELS) mode, which included elliptic alloy precipitates with elemental Cu, Cr, Fe and Si, except for Al, and B4C nanoparticles with polygonal shape. The interface characteristics showed that the (021) crystal plane of B4C particle and (111) crystal plane of aluminum matrix grew together. The lattice misfit was about 1.68% for (111)Al//(021)B4C. The corrosion properties and corresponding mechanism of Al/B4C MMCs were investigated in an aqueous solution with 5000 ppm boric acid at 100 °C and atmospheric pressure, which showed that the mass increment rate was first decreased with increasing corrosion time and then increased.

Transmission electron microscopy assessment of conductive-filament formation in Ni–HfO2–Si resistive-switching operational devices

Resistive random-access memory (ReRAM) devices are currently the object of extensive research to replace flash non-volatile memory. However, elucidation of the conductive-filament formation mechanisms in ReRAM devices at nanoscale is mandatory. In this study, the different states created under real operation conditions of HfO2-based ReRAM devices are characterized through transmission electron microscopy and electron energy-loss spectroscopy. The physical mechanism behind the conductive-filament formation in Ni/HfO2/Si ReRAM devices based on the diffusion of Ni from the electrode to the Si substrate and of Si from the substrate to the electrode through the HfO2 layer is demonstrated.

Cubic crystalline erbium oxide growth on GaN(0001) by atomic layer deposition

Growth of crystalline Er2O3, a rare earth sesquioxide, on GaN(0001) is described. Ex situ HCl and NH4OH solutions and an in situ N2 plasma are used to remove impurities on the GaN surface and result in a Ga/N stoichiometry of 1.02. Using atomic layer deposition with erbium tris(isopropylcyclopentadienyl) [Er(iPrCp)3] and water, crystalline cubic Er2O3 (C-Er2O3) is grown on GaN at 250 °C. The orientation relationships between the C-Er2O3 film and the GaN substrate are C-Er2O3(222) ǁ GaN(0001), C-Er2O3⟨-440⟩ ǁ GaN ⟨11-20⟩, and C-Er2O3⟨-211⟩ ǁ GaN ⟨1-100⟩. Scanning transmission electron microscopy and electron energy loss spectroscopy are used to examine the microstructure of C-Er2O3 and its interface with GaN. With post-deposition annealing at 600 °C, a thicker interfacial layer is observed, and two transition layers, crystalline GaNwOz and crystalline GaErxOy, are found between GaN and C-Er2O3. The tensile strain in the C-Er2O3 film is studied with x-ray diffraction by changes in both out-of-plane and in-plane d-spacing. Fully relaxed C-Er2O3 films on GaN are obtained when the film thickness is around 13 nm. Additionally, a valence band offset of 0.7 eV and a conduction band offset of 1.2 eV are obtained using x-ray photoelectron spectroscopy.

Revealing the Atomic Defects of WS2 Governing Its Distinct Optical Emissions

AbstractDefects and their spatial distribution are crucial factors in controlling the electronic and optical properties of semiconductors. By using scanning transmission electron microscopy and electron energy loss spectroscopy, the type of impurities/defects in WS2 subdomains with different optical properties is successfully assigned. A higher population of Cr impurities is found in the W‐terminated edge domain, while the S‐terminated domain contains more Fe impurities, in accordance with the luminescence characteristics of chemical‐vapor‐grown WS2 of a hexagonal shape. In agreement with the first‐principles calculations, the domains with Cr substitutional dopants exhibit strong trion emission. Fe atoms tend to gather into trimer configuration and introduce deep acceptor levels which compensate the n‐type doping and suppress trion emission. It is also discovered that the domain with higher luminescence but smaller defect concentration tends to get oxidized more rapidly and degrade the 2D structure with many triangular holes. Excitons tend to accumulate at the edges of the oxidized triangular holes and results in enhanced PL emission. The findings indicate that choosing stable elements as dopant and controlling the number of specific edge structures within a crystal domain of 2D transitional metal dichalcogenides can be a new route to improve the optical properties of these materials.