Situ Scanning Electron Microscopy Research Articles

In Situ Investigation of Tensile Response for Inconel 718 Micro-Architected Materials Fabricated by Selective Laser Melting.

Topology optimization enables the design of advanced architected materials with tailored mechanical properties and optimal material distribution. This method can result in the production of parts with uniform mechanical properties, reducing anisotropy effects and addressing a critical challenge in metal additive manufacturing (AM). The current study aims to examine the micro-tensile response of Inconel 718 architected materials utilizing the Selective Laser Melting Technique. In this context, three novel architected materials, i.e., Octet, Schwarz Diamond (SD), and hybrid Schwarz Diamond and Face Centered Cubic (FCC), were tested in three different relative densities. The specimens were then subjected to uniaxial quasi-static tensile tests to determine their key mechanical properties, including elastic modulus, yield strength, and ultimate tensile strength (UTS), as well as the scaling laws describing the tensile response of each architected material. In situ Scanning Electron Microscopy (SEM) has been performed to observe the structure and grain morphology of the 3D printed specimens along with the phase transitions (elastic, plastic), the crack propagation, and the overall failure mechanisms. The results highlight the effect of the lattice type and the relative density on the mechanical properties of architected materials. Topologically optimized structures presented a 70-80% reduction in overall strength, while the SD and SD&FCC structures presented higher stretching dominated behavior, which was also verified by the n-value range (1-2) extracted from the identification of the scaling laws.

A N–CoSe/CoSe2–C@Cu hierarchical architecture as a current collector-integrated anode for potassium-ion batteries

The highly reversible insertion/extraction of large-radius K+ into electrode materials remains a tough goal, especially for conversion-type materials. Herein, we design a current collector-integrated electrode (N–CoSe/CoSe2–C@Cu) as an advanced anode for potassium-ion battery (PIBs). The conductive CoSe/CoSe2 heterojunction with rich Se vacancy defects, conductive sp2 N-doped carbon layer, and the elastic copper foil matrix can greatly accelerate the electron transfer and enhance the structural stability. Consequently, the well-designed N–CoSe/CoSe2–C@Cu current collector-integrated electrode displays enhanced potassium storage performance with regard to a high capacity (325.1 mAh·g−1 at 0.1 A·g−1 after 200 cycles), an exceptional rate capability (223.5 mAh·g−1 at 2000 mA·g−1), and an extraordinary long-term cycle stability (a capacity fading of only 0.019% per cycle over 1200 cycles at 2000 mA·g−1). Impressively, ex situ scanning electron microscopy (SEM) characterizations prove that the elastic structure of copper foil is merged into the cleverly designed N–CoSe/CoSe2–C@Cu heterostructure, which buffers the deformation of structure and volume and greatly promotes the cycle life during the potassium/depotassium process.Graphical abstract

Influence of Nb substrate morphology and atomic structure on Sn nucleation and early Nb3Sn growth

The enhanced accelerating performance of Nb3Sn-coated Nb superconducting radio frequency (SRF) cavities is severely limited by quenching sites at material defects formed during the Nb3Sn film growth procedure. In this work, we aimed to understand the complex surface-mediated interactions that drive initial Nb3Sn formation during the Sn vapor deposition procedure used to fabricate Nb3Sn coated SRF cavities. Nb substrates were modified, coated with Sn, and then characterized using an ultra-high vacuum (UHV) chamber equipped with metal deposition and in situ surface analysis capabilities. The atomic structure of the Nb oxide surface was modified to assess how the Nb surface defect density and crystallographic orientation impact the size of nucleated Sn islands and relative Nb3Sn growth rates. Formed Nb3Sn/Nb surfaces were visualized using ex situ scanning electron microscopy (SEM) and post-deposition annealing revealed Sn desorption and Nb3Sn degradation pathways. Finally, we showed that the Sn deposition conditions can be modified to overcome the growth barriers that are imposed by the Nb morphology. This study provides a unique bridge between fundamental growth studies in pristine conditions with observed phenomena of Nb3Sn grown on realistic cavity surfaces.

Accelerated Li Penetration and Crack Propagation Due to Mechanical Degradation of Sulfide-Based Solid Electrolyte.

This work presents quantitative investigations into the relationships between lithium dendrite growth in the defects of Li6PS5Cl (LPSCl) solid electrolyte (SE), crack nucleation and propagation in the SE, and the associated mechanical forces driving these dendrites and cracks. Two different growth modes for lithium dendrites are identified by ex situ scanning electron microscopy (SEM) observation: longitudinal cracking inside pores in the SE and lateral penetration along boundaries of the SE particles. These in situ TEM tests reveal that concentrated Li plating in a nano-sized defect on the LPSCl surface will lead to the nucleation and propagation of cracks into the LPSCl under a stress much smaller than the expected mechanical strength of the LPSCl material. This unexpected mechanical degradation is caused by a reduction in the mechanical strength of LPSCl during electrochemical charge/discharge cycling, resulting from a disorder in the crystal structure of LPSCl as revealed by DFT simulations. Due to this mechanical degradation of LPSCl, the threshold force necessary to initiate crack growth is much lower than the previously expected force to drive dendrite growth.

Development of a microfurnace dedicated to in situ scanning electron microscope observation up to 1300 °C. I. Concept, fabrication, and validation.

The development of a new heating system dedicated to in situ scanning electron microscope (SEM) experimentation at high temperatures is reported. This system, called FurnaSEM, is a compact microfurnace, enabling heat treatments up to 1300 °C. The choice of materials for the microfurnace is explained. The design of the microfurnace is optimized by iterations of numerical simulations, and the thermal characteristics of the microfurnace are calculated numerically. The numerical results obtained are compared with the thermal characteristics of a manufactured microfurnace, measured on a specially developed dedicated test bench. This test bench includes a working chamber simulating a SEM chamber equipped with a thermal camera. The results obtained during various qualification tests enabled us to determine the main technical characteristics of the FurnaSEM microfurnace: temperature profiles on the sample support surface, energy consumption at high temperatures, and the range of achievable thermal cycles.

Analyzing dust particle size and size distribution on extracted particles by SEM and comparing with light scattering techniques

AbstractThis study investigates the measurement of plasma‐grown nanoparticles, comparing ex situ scanning electron microscopy (SEM) and an in situ light scattering method which is based on Mie theory and utilizes a neural network for evaluation. The research reveals that the particle size distribution (PSD) is normal and very narrow, supporting the common assumption of monodisperse particle clouds. Importantly, the study finds that the spread of the PSD increases proportionally with the mean size, suggesting varied growth rates based on the radius of the spherical dust grains. Both methods produce consistent results, which encourages the use of the interference‐free, real‐time, light‐based Mie method in similar studies.

Mechanical properties and deformation mechanisms of single crystal Mg micropillars subjected to high-strain-rate C-axis compression

The mechanical properties and deformation mechanisms of single crystal magnesium under c-axis quasi-static and high-strain rate compressions are investigated through in situ scanning electron microscope (SEM) experiments and post-mortem transmission electron microscope (TEM) characterization. The findings revealed that ductility and high rates of hardening are preserved for pillars as large as 15 μm. Furthermore, rate effects result in a mild increase in flow stress with plastic deformations controlled primarily by the slip of <a+c> type dislocations. Importantly and in contrast to other literature reports, plastic deformation occurs in the absence of twining. As the strain increases and plastic deformation exceeds about 4%, crystal rotation activates basal slip, <a> type dislocations, resulting in a more rate independent flow stress. TEM observation on micropillars compressed at a strain rate of 250/s, revealed the activation of {112‾2‾}<1‾1‾23> slip systems and high mobility of screw dislocations as major contributors to plastic strains in excess of 10% without fracture. These findings are relevant to the design of lightweight materials used in transportation systems, e.g., selection of material grain size. Moreover, the experimental data here reported provides the materials science community with a unique opportunity to validate discrete dislocation dynamics (DDD) formulations employed in multiscale design of materials.

A Comprehensive Study of the Parameters Affecting Magnesium Plating/Stripping Kinetics in Rechargeable Mg Batteries

Beyond the lithium ion battery (LIB) technology, alkali and alkaline earth metal (Li, Na, Mg, Ca etc.) anodes boost the prospect of next generation battery chemistry through their highly promising theoretical specific capacities.1,2 Mg metal anode based battery is thus one of the strong contenders for sustainable and alternative rechargeable battery systems, with its natural abundance and eco-friendly resources.3 Despite the first proof-of-concept of a Mg battery established back in 2000,4 its complete rechargeability still remains elusive due to the lack of suitable conventional electrolytes and low mobility of Mg2+ ions in typical intercalation cathodes. Although potentially safer than Li metal (less prone to dendritic growth), reversible Mg electrodeposition in non-aqueous liquid electrolytes is a challenge due to poor salt solubility and formation of ionically blocking surface passivation films.5,6 The study of the interphase between a Mg metal anode and electrolyte is therefore of critical worth as it can dictate stability and reversibility for a particular electrode/electrolyte combination.7 In this work, we explore the role of various parameters, including electrolyte composition, concentration, solvent and substrate nature (various metals and carbon based substrates) and their impact on Mg plating/stripping kinetics and coulombic efficiency. The deposit morphology was investigated via ex situ scanning electron microscopy (SEM) and the reductive stability of the electrolytes was studied by cyclic voltammetry (CV), X-ray Photoelectron Spectroscopy (XPS) and electrochemical quartz crystal microbalance (EQCM). Overall, a comprehensive discussion about the relationship between cation solvation structure, composition and stability of passivation layer (if any) and the degree of reversibility of Mg electrodeposition will be presented. Keywords: Beyond LIB chemistry, metal anode, magnesium, EQCM, plating/stripping.

Disproportionation of Iron in Almandine‐Pyrope‐Grossular Garnet From 25 to 65 GPa

AbstractThe production of metal via the iron disproportionation reaction in the deep Earth has been a long debated topic with important implications for the geochemistry of the lower mantle. To explore the occurrence of the iron disproportionation reaction from 25 to 65 GPa, a natural almandine‐pyrope‐grossular garnet was studied with in situ X‐ray diffraction (XRD) in the laser‐heated diamond anvil cell and ex situ scanning electron microscopy (SEM) techniques. Upon heating the natural almandine‐pyrope‐grossular garnet up to 3000 K up to 65 GPa, the formation of phase assemblage consisting of bridgmanite, stishovite, and davemaoite was confirmed by XRD, but because of the low abundance of Fe metal and small grain size, XRD was determined not to be effective in detecting the disproportionation reaction. Examination of the samples recovered between 39 and 64 GPa by SEM analysis revealed the presence of nm‐scale disproportionated iron metal grains as an additional product of this reaction that was not detectable in the XRD patterns. Volume compression data of bridgmanite synthesized in the experiments were fit to the Birch‐Murnaghan equation of state and compared to similar compositions. Bridgmanite was found to decompress to the LiNbO3‐type structure, indicating a high FeAlO3 content, in accordance with the occurrence of a disproportionation reaction. The experimental confirmation of disproportionated metallic Fe has significant implications for the distribution of siderophile and volatile elements in the lower mantle.

In situ X-ray computed micro-tomography imaging of failure processes in Cr-coated Zircaloy nuclear fuel cladding materials

Chromium (Cr)-coated Zircaloy fuel cladding has been considered a promising candidate materials system for accident tolerant fuels. In this work, two types of Cr coatings produced by cold sprayed (CS) and physical vapour deposited (PVD) methods were studied. In particular, a novel combination of C-ring compression tests at room temperature (RT) and 345 °C in an inert gas environment and real-time X-ray micro-computed tomography (XCT) imaging was adopted to investigate the failure processes. Before testing, the crystal structure and local properties were fully characterized; post testing, ex situ scanning electron microscope (SEM) imaging were conducted to complement the XCT measurements in crack density. It was found that the failure processes in both coatings vary with temperature, as discussed in detail. The hoop strength of first coating cracks’ formation of CS materials were higher than the PVD materials due to their higher interfacial roughness and distribution of splatted grains in CS coating. Based on a calculation of the first Dundurs’ parameter from the measured local properties and observed crack arrest/deflection at coating/substrate interface, it was found that the cold sprayed coating-cladding material system has a higher interfacial toughness in terms of critical strain energy release rate due to its interlocking interfacial structure.

Effect of texture evolution and defect on the crack initiation of a Ni‐based superalloy electron beam welded joint

AbstractElectron beam welding (EBW), a high‐quality and precise joining process, is widely used in aerospace manufacturing. In this study, through in situ scanning electron microscope (SEM) fatigue experiments and X‐ray computed tomography (CT) scanning technology, we revealed the fatigue crack initiation and propagation mechanism in GH4169 superalloy EBW joints under different post‐welding heat treatment conditions. The welded pores have a decisive effect on the fatigue properties of direct aging treatment welded joints. Fatigue cracks initiate from pore defects on the surface or in the subsurface. Due to the heterogeneous microstructure in weld seam, fatigue cracks tend to grow along the primary dendrite axis and secondary dendrite arms. Besides, in homogenization and aging treatment specimen, intergranular fatigue cracks tend to nucleate in the slip zone of large grains and twin boundaries. Although homogenization treatment can eliminate segregation, it also results in significant grain growth in both weld seam and base material.

Experimental and numerical investigation on meso-fracture behavior of Beishan granite subjected to grain size heterogeneity

Research on crack evolution mechanism and failure pattern of Beishan granite is vital for evaluation of the engineering stability of disposal repository. The mechanical properties, especially the strong heterogeneity, significantly affect the cracking behavior of granite. To investigate the fracture behavior of heterogeneous granite, mesoscopic three-point bending tests were conducted on Beishan granite using an in situ scanning electron microscope (SEM) with a loading device, and the entire cracking process was observed in real time. Additionally, the effect of grain size heterogeneity on strength and deformation behavior of granite was quantitatively investigated by introducing a statistically defined heterogeneity index into the grain-based model in two-dimensional Particle Flow Code (PFC-GBM), and the crack development was characterized through fractal theory. The results demonstrated that fracture mechanism of granite is mainly tensile and shear failure, and the fracture surface of tensile failure is rough and irregular, which is mainly caused by the tearing between various mineral crystals, whereas the fracture surface of shear failure is relatively smooth, which is mainly caused by the dislocation and slip between minerals. The crack edge can be regarded as the damage zone, and the development of the main crack is promoted by the continuous generation and combination of micro-damage at the crack tip. The crack propagation path from a mesoscale perspective is a process of continuous crack orientation, which depends on the competition mechanism between mineral properties and maximum tensile stress. Generally, the granite strength tends to increase with the increase of heterogeneity.

In Situ SEM, TEM, EBSD Characterization of Nucleation and Early Growth of Pure Fe/Pure Al Intermetallic Compounds.

The nucleation and growth processes of pure Fe/pure Al intermetallic compounds (IMCs) during heat treatment at 380 °C and 520 °C were observed through in situ scanning electron microscopy (SEM). The size of the IMCs were statistically analyzed using image analysis software. The types and distribution of IMCs were characterized using transmission electron microscopy (TEM) and electron backscattering diffraction (EBSD). The results showed that: at 380 °C, the primary phase of the Fe/Al composite intermetallic compounds was Fe4Al13, formed on the Fe side and habituated with Fe. The IMC was completely transformed from the initial Fe4Al13 to the most stable Fe2Al5, and the Fe2Al5 was the habitus with Fe during the process of holding at 380 °C for 15 min to 60 min. At 380 °C, the initial growth rate of the IMC was controlled by reaction, and the growth rate of the thickness and horizontal dimensions was basically the same as 0.02-0.17 μm/min. When the IMC layer thickness reached 4.5 μm, the growth rate of the thickness changed from reaction control to diffusion control and decreased to 0.007 μm/min. After heat treatment at 520 °C (≤20 min), the growth of IMC was still controlled by the reaction, the horizontal growth rate was 0.53 μm/min, the thickness growth rate was 0.23 μm/min, and the main phase of the IMC was the Fe2Al5 phase at 520 °C/20 min.

Degradation Mechanisms of Positive Electrode Materials for Sodium-Ion Batteries

Sodium-ion batteries (SIB) require less critical materials and lead to a significant cost reduction compared to state-of-the-art lithium-ion batteries [1]. Although a large-scale commercialization of SIBs is within reach [2], the understanding of the degradation mechanisms of these batteries is still incomplete. The larger ionic radius of sodium in comparison to that of lithium can induce larger stress changes in the host material causing poor long-term stability. Minimizing degradation of positive electrode materials is of high importance for the advancement of SIB technology. Here, we report on degradation of the important structure types: layered oxides, polyanionic compounds, and Prussian blue analogues. Our results show that the polyanionic Na3V2(PO4)3 is a highly reliable cathode material, which can be used as a benchmark or reference material.During battery operation, mechanical stresses are caused by volume changes of the active materials, when sodium ions are inserted or extracted into/from them. We use operando methods such as the substrate curvature technique to measure stresses in the electrode and draw conclusions about electrochemical and physical processes in the materials during cycling [3]. To investigate phenomena like volume changes, crack formation and overall morphology, ex situ scanning electron microscopy (SEM) is used intermittently. Here, we compare the same site on the electrode in different states of charge and for different cycle numbers. Additionally, X-ray diffraction (XRD) measurements are conducted to study phase transitions.Na2/3Fe1/3Mn2/3O2 is a layered P2-type oxide that offers a high specific capacity and is composed of abundant elements. Due to its intrinsic sodium deficiency, diverse presodiation methods become important [4]. We investigate Na2C4O4 as sacrificial salt and its effects on electrode morphology during decomposition. Our goal is to understand the resulting reaction pathways and optimize the full cell performance of layered oxides.Sodium hexacyanoferrate NaxFe[Fe(CN)6] is a Prussian blue analogue and one of the most prominent candidates for commercial SIBs [2]. It also offers high specific capacities and a long cycle life, but its high moisture sensitivity and interstitial water demand appropriate electrode drying procedures to avoid side reactions during cell operation. Crack formation and growth were studied with SEM after and during cycling. Phase transitions are observed by operando XRD and operando substrate curvature measurements.Sodium vanadium phosphate Na3V2(PO4)3 (NVP) with its highly stable three-dimensional network of a NASICON-type structure and its large diffusion channels for sodium ions is another promising electrode material that deserves attention. NVP can be sodiated and desodiated at two different voltage plateaus and therefore can serve either as cathode or anode material. SEM observations at different states of charge show how preexisting cracks open/close during desodiation/sodiation due to volume shrinkage/expansion. We compare symmetric NVP−NVP cells to full cells with NVP cathodes and anodes of Na metal, hard carbon, Sb/C, and SnSb/C. Our data suggests that problems of Na and Na-ion cells frequently result from the anode. NVP itself is extremely reliable and balanced symmetric NVP−NVP cells exhibit very high cycling stability. More than one thousand cycles can be easily achieved. Due to its distinct plateaus and high stability, we suggest NVP as a reference material for cathode and anode materials. For example, NVP can serve as a reliable anode material for testing the stability of different cathode materials. NVP as a cathode may be used to test anode materials or as a benchmark for other cathode materials [5].Acknowledgements:This work contributes to the research performed at CELEST (Center for Electrochemical Energy Storage Ulm-Karlsruhe) and was funded by the German Research Foundation (DFG) under Project ID 390874152 (POLiS Cluster of Excellence, EXC 2154).Literature:[1] C. Vaalma et al., Nature Reviews Materials 2018, 3, 4, 1-11.[2] M. A. Sawhney et al., ChemPhysChem 2022, 23, 5, 1-19.[3] Z. Choi et al., Journal of Power Sources 2013, 240, 245-251.[4] J. M. De Ilarduya et al. Electrochimica Acta 2019, 321, 134693.[5] T. Akçay et al., ACS Applied Energy Materials 2021, 4, 11, 12688-12695.

A novel diagnostic for dust particle size in a low-pressure nanodusty plasma based on the decay of the electron density released by laser-induced photodetachment

One of the key parameters in low-pressure nanodusty plasmas is the dust particle size. In this work, we introduce a new method for the determination of the dust particle size in a nanodusty plasma, created in a mixture of argon and hexamethyldisiloxane. To this end, an ultraviolet (λ=266 nm) pulsed laser was used to release plasma-collected electrons from the nanoparticles. Subsequently, the response of the free electron density of the plasma was measured using microwave cavity resonance spectroscopy. Using a stochastic model for particle charging using orbital-motion limited (OML) theory, the predicted charging timescale can be directly compared to the experimentally measured decay timescale of the photo-released electron density. Good agreement was found between the experimentally predicted dust particle size and ex situ scanning electron microscopy (SEM) measurements. Furthermore, the sensitivity of the OML model to its input parameters was assessed. Finally, reversing the method can yield an estimate for the positive ion density based on the dust particle size from SEM.

In Situ SEM Compression Study on Micro-mechanical Behavior of Electron Beam Melted Ti-6Al-4V Alloy

To investigate the mechanical properties of electron beam melted (EBM) Ti-6Al-4V alloy at the microscale, a series of in situ scanning electron microscope (SEM) compression experiments were performed in the current study. Firstly, a reconstruction of the original β phase of Ti-6Al-4V alloy was conducted using electron backscattering diffraction (EBSD) analysis. Micro-pillars were subsequently fabricated with a diameter of 2 μm within the same original β phase grain, and yield strength was measured using an in-situ mechanical compression device. The mechanical response of each micro-pillar was found to vary, and potential reasons for this phenomenon were discussed, including the impact of α-phase and β-dispersion on the material’s mechanical properties. Moreover, a clear size effect was observed when comparing the yield strength of the bulk material. Furthermore, the plastic deformation behavior of Ti-6Al-4V alloy was also investigated through compression tests on the micro-pillars.

Classification of the acquisition conditions driving the accuracy of strain measurements during in situ DIC with scanning electron microscope

AbstractPerforming in situ scanning electron microscope (SEM) tests is an interesting way to visualise strain heterogeneities under mechanical loading. An essential step before performing the tests is to define the acquisition conditions. The aim of this paper is to propose a classification of the acquisition conditions that are most important for the accuracy of strain measurements using digital image correlation (DIC) in in situ SEM tests. More than 200 image pairs were acquired using a field emission gun SEM. The influence of different acquisition conditions was investigated: acceleration voltage, probe current, working distance, magnification, number of integrated images, image resolution, integration and number of integrated images, scan speed, contrast, brightness and exposure time of the sample in a given area. The methodology implemented in this work is an interesting tool for detecting scan line shift, drift distortion, spatial distortion and rastering artefacts. It allows the optimization of SEM acquisition conditions for strain measurements. Finally, optimal acquisition conditions for in situ testing are proposed and used to perform a tensile test on pure copper. The main factors highlighted include the size of the subset used in the DIC, the beam stabilisation time before image acquisition and the size of the images, which play a significant role in the results. It is recommended to apply the methodology to each device to optimise the acquisition conditions.

Evaluating Residual Stress in Carbon Fiber-Reinforced Polymer (CFRP) at Microscale Using Fiber Push-Out Experiment and Finite Element Modeling.

Microscale residual stress may develop during the manufacturing of Carbon Fiber-Reinforced Polymer (CFRP) composites and negatively affect apparent macroscale mechanical properties. Accordingly, accurately capturing residual stress may be essential in computational methods used for composite material design. This work presents a new data-driven methodology for the evaluation of microscale residual stress in CFRPs using fiber push-out experiments with in situ scanning electron microscopy (SEM) imaging. SEM images reveal significant through-thickness matrix sink-in deformation in resin-rich areas after nearby fibers are pushed out, which is attributed to the release of microscale process-induced residual stress. The sink-in deformation is measured experimentally, and a Finite Element Model Updating (FEMU) method is used to retrieve the associated residual stress. The finite element (FE) analysis includes simulation of the curing process, test sample machining, and fiber push-out experiment. Significant out-of-plane matrix deformation larger than 1% of the specimen thickness is reported and associated with a high level of residual stress in resin-rich areas. This work emphasizes the importance of in situ data-driven characterization for integrated computational materials engineering (ICME) and material design.

The influence of recrystallization annealing time on high cycle fatigue behavior of high-Mn austenitic steel at 77 K

Three high manganese austenitic steels were prepared by different recrystallization annealing time (0, 32, and 128 min) to investigate the effect of recrystallization annealing time on high-cycle fatigue behavior at 77 K. The microstructure was characterized by means of quasi in situ scanning electron microscope (SEM). When fatigue life is about 5.0 × 106 loading cycles, the fatigue strength at 77 K increases from 512 MPa to 625 MPa with the decrease in recrystallization annealing time (RAT). Decrease in RAT leads to grain refinement and the increase in density of dislocation. Grain refinement can delay crack initiation, prevent crack propagation, and hardly hinders the formation of deformation twins. In addition, it is surprising that the grain refinement and the increase in dislocation density promote the formation of nanoscale voids, which leads to stress relaxation and thus improve the fatigue performance.

Effect of Fiber–Matrix Interface Friction on Compressive Strength of High-Modulus Carbon Composites

Carbon-fiber-reinforced polymers (CFRPs) enable lightweight, strong, and durable structures for many engineering applications including aerospace, automotive, biomedical, and others. High-modulus (HM) CFRPs enable the most significant improvement in mechanical stiffness at a lower weight, allowing for extremely lightweight aircraft structures. However, low fiber-direction compressive strength has been a major weakness of HM CFRPs, prohibiting their implementation in the primary structures. Microstructural tailoring may provide an innovative means for breaking through the fiber-direction compressive strength barrier. This has been implemented by hybridizing intermediate-modulus (IM) and HM carbon fibers in HM CFRP toughened with nanosilica particles. The new material solution almost doubles the compressive strength of the HM CFRPs, achieving that of the advanced IM CFRPs currently used in airframes and rotor components, but with a much higher axial modulus. The major focus of this work has been understanding the fiber-matrix interface properties governing the fiber-direction compressive strength improvement of the hybrid HM CFRPs. In particular, differences in the surface topology may cause much higher interface friction for IM carbon fibers compared to the HM fibers, which is responsible for the interface strength improvement. In situ Scanning Electron Microscopy (SEM)-based experiments were developed to measure interface friction. Such experiments reveal an approximately 48% higher maximum shear traction due to interface friction for IM carbon fibers compared to the HM fibers.