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MOX (uranium-plutonium mixed oxide) nuclear fuels are generally manufactured using a MIMAS (micronized master blend)-type process resulting in ceramics presenting a microstructure composed of agglomerates of different plutonium contents. To allow for phase-dependent grain size analysis, we developed an SEM (scanning electron microscopy) method based on simultaneously collected EDS (energy dispersive X-ray spectroscopy) and EBSD (electron backscattered diffraction) maps. Posttreatment of the EDS/EBSD data allows constructing maps of plutonium-rich agglomerates, grain boundaries, and porosities, which are then combined in a single dataset. We then propose and discuss a criterion that can be applied for the attribution of each grain to the plutonium-rich or uranium-rich agglomerates. To validate this criterion, the EDS/EBSD results are compared to better chemically resolved mapping that can be obtained through EPMA (electron probe microanalyzer). Compared to the EPMA-/EBSD-based method previously reported in the literature, the EDS/EBSD method we present offers a simple and convenient way to gain insights about the interdependence between microstructural and chemical features, such as measuring grain size in the different phases present in MIMAS-type MOX fuels.

In this study, we aimed to elucidate the functional significance of transforming growth factor-β (TGF-β)-regulated SLC9A5 (NHE5) in enamel formation. Mouse ameloblast-derived mHAT9d cells were treated with TGF-β1, TGF-β2, or TGF-β3, and the expression of Slc9a family members was analyzed via RNA sequencing (RNA-seq) and quantitative PCR (qPCR). Slc9a5-deficient mice were generated to examine enamel morphology. Enamel volume, mineral density, and structure were assessed using micro-computed tomography (μCT), scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). Protein expression was analyzed via SDS-PAGE, western blotting, and immunohistochemistry. RNA-seq and qPCR analyses revealed that TGF-β1 and TGF-β3 strongly induced Slc9a5 in a dose-dependent manner; however, TGF-β2 had a minimal effect. In Slc9a5-deficient mice, incomplete crown formation and pit-like defects were evident on postnatal day 5; however, enamel protein profiles and thickness formation at day 11 were comparable to those in wild-type mice. In contrast, by day 70, μCT revealed marked thinning of enamel and reduced mineral density, SEM showed cracks and surface defects, and EPMA demonstrated significantly lower calcium-to-phosphorus (Ca/P) molar ratios than in wild-type mice. These findings indicate that loss of Slc9a5 slightly affects protein secretion but causes defective mineral maturation and enamel fragility. SLC9A5 is a downstream target of TGF-β signaling, which is indispensable for enamel maturation because it maintains ion transport and extracellular pH homeostasis in ameloblasts. Its deficiency leads to reduced mineral density, altered Ca/P composition, and progressive enamel loss. These findings underscore the essential role of SLC9A5 in the long-term structural stability of enamel.

Doxorubicin (DOX), an anthracycline chemotherapeutic agent, induces significant male reproductive toxicity, however, its molecular mechanisms remain incompletely defined. Although oxidative stress is implicated in DOX-induced testicular injury, the roles of iron dysregulation and antioxidant suppression have not been fully characterized in the testis. We investigated time-dependent effects of DOX on testicular morphology, iron homeostasis, and oxidative stress, and evaluated the potential protective effects of (4-(methylthio)phenylthio) methane bisphosphonate (MPMBP), an iron-chelating and antioxidant compound. Male ICR mice received a single intraperitoneal injection of DOX (5 mg/kg). In Experiment 1, testes were collected at 24 h, 48 h, and 1-5 weeks to assess morphological changes, germ cell counts, transcriptional alterations in apoptosis-, antioxidant-, and iron metabolism-related genes, and iron deposition using electron probe microanalysis (EPMA). In Experiment 2, MPMBP (10 mg/kg) was administered either concomitantly with DOX or starting 5 days later, and testicular endpoints were evaluated at 5 weeks. DOX induced progressive testicular atrophy and depletion of early-stage germ cells. Apoptosis-related genes exhibited biphasic upregulation, accompanied by iron accumulation and downregulation of Gpx4 and mitochondrial ferritin (Ftmt). EPMA confirmed iron deposition within seminiferous tubules and interstitial regions. MPMBP co-administration was associated with partial preservation of testicular architecture, reduced iron accumulation, and modest restoration of Gpx4 and Ftmt expression, although these effects were incomplete under the present experimental conditions. These findings associate iron dysregulation and impaired antioxidant defense with DOX-induced testicular injury and support further preclinical investigation of iron-chelating and antioxidant strategies aimed at mitigating chemotherapy-associated reproductive toxicity.

To delve into the intrinsic mechanism of mineral liberation during the grinding process, this study systematically analyzed the coal petrographic composition and mineral occurrence forms in coking middling coal using electron probe microanalysis (EPMA) and X-ray diffraction (XRD) techniques. Results showed that quartz occurred primarily as coarse granules embedded in organic matter, kaolinite was mostly lumpy and disseminated, and calcite mainly filled fractures. The mechanical properties of minerals can significantly influence the grinding efficiency. The elastic constants of major minerals such as quartz, kaolinite, and calcite were calculated through density functional theory (DFT) and molecular dynamics (MD) simulations. On the basis of these calculations, their mechanical properties were deduced, and a connection was established between the mechanical properties of minerals and their liberation during the grinding process. Quartz exhibited remarkable resistance to compressive deformation and shear fracture owing to its ultrahigh stiffness (C11 = C22 = 245.47 and C33 = 221.66 GPa) and macroscopic moduli (K = 166.24, G = 69.61, and E = 183.25 GPa). Kaolinite exhibited high stiffness within its layers but weak interlayer shear properties (C11 = 161.38 and C44 = 23.14 GPa), which made it prone to interlayer dissociation. Calcite, due to its significant stiffness anisotropy (with C11 = C22 = 196.9 and C33 = 79.79 GPa), demonstrated strong anisotropy and cleavage-dominated fragmentation behavior during the process. Coal, characterized by weak bedding stiffness and extremely low moduli, is susceptible to brittle fracture. Broken resistance decreased in the order of quartz > kaolinite > calcite > coal. Excellent agreement existed between the elastic constant calculations and the mineral size distributions after grinding. This study innovatively correlates the mechanical properties of minerals with liberation behaviors during macroscopic grinding processes, providing significant insights into the selective liberation mechanisms of minerals in middling coking coal.

Pyrometallurgical production of non-ferrous metals generates substantial slag volumes, yet potential metal(loid) leaching remains a critical barrier to sustainable valorisation. In principle, appropriate control of metallurgical processing can tailor slag characteristics to achieve acceptable leachability and reduce environmental risk. Understanding metal(loid) leaching behaviour requires systematic consideration of slag chemistry, mineralogy, and microstructure. This is explored herein in synthetic Fe,Al-silicate slags, representative of those produced in non-ferrous metallurgy. Chemistry, oxygen partial pressure, and cooling rates were varied to assess their influence on the distribution and leaching of As, Sb, and Mo. Slags were characterised by XRF, ICP-OES, QXRD, FTIR, SEM/EDX, and EPMA, while leaching was evaluated (EN 12457-2 test) to establish processing-leaching relationships. Rapid cooling was found to promote the formation of amorphous Fe-Si matrices , immobilising As and Sb, whereas slower cooling favoured fayalite crystallisation, resulting in increased leaching of these elements. Mo exhibited the lowest leaching in slowly cooled slags, likely due to the formation of Mo-rich phases. Arsenic and Sb were predominantly associated with the amorphous phase, independent of the Fe/Si ratio; however, higher Fe/Si ratios depolymerise the glass, diminishing its stabilising capacity and increasing the leaching of As and Sb. Oxygen partial pressure played a critical role in elemental partitioning: higher pO2 (10⁻10 atm) favoured the retention of As, Sb, and Mo within the glass, whereas lower pO2 (10⁻12 atm) promoted the formation of metallic Fe particles enriched in these elements, leading to elevated leaching. Overall, the findings herein provide insights into how to steer process parameters during slag formation and effectively minimise leaching.

Increased alloying content in advanced Ni-based superalloys for large disc forgings intensifies microsegregation and promotes the formation of detrimental secondary phases, challenging the cast-and-wrought processing route. This study investigates the effects of Ta addition on the solidification and homogenization behaviors of a high-alloyed GH4065A superalloy by comparing the base alloy with a variant containing 5 wt.% Ta (5Ta alloy). As-cast and homogenized microstructures were characterized using SEM and EPMA, solidification behavior was analyzed via DSC, and homogenization kinetics were modeled. Results demonstrate that Ta addition stabilizes the η phase, increasing its solidification temperature and fraction in the as-cast microstructure, but does not alter the solidification sequence. During homogenization, Nb remained the most segregated element and governed the homogenization kinetics, whereas Ta preferentially partitioned into MC carbides and the η phase. The diffusion activation energy for Nb in the 5Ta alloy was determined, and a diffusion model was established to describe the elimination of microsegregation. Optimum homogenization parameters were determined to completely dissolve the η phase and eliminate microsegregation. The results indicate that strategic Ta addition for enhanced performance does not compromise ingot manufacturability, providing valuable guidance for the processing and composition design of advanced disc superalloys.

To address the high-salinity and hyper-humid thermal environment of tropical oceans and meet industrial demands for high strength and lightweight, austenitic low-density steel was developed as a novel corrosion-resistant steel. A 3.5 wt.% NaCl solution was used to simulate the marine environment to study the effect of Si on the corrosion behavior of this steel. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and electron probe microanalysis (EPMA) were employed to characterize the microstructures and corrosion behaviors of two test steels, as well as the phase compositions and element distributions of corrosion products after polarization and cyclic immersion accelerated corrosion tests. The results show that a dense oxide film initially forms on the steel surface in 3.5 wt.% NaCl solution at the early corrosion stage. Si addition induces SiO2 formation and promotes Al conversion to Al2O3, enhancing oxide film compactness and inhibiting matrix atom outward diffusion and Cl- inward penetration. With prolonged corrosion, the oxide film is dissolved or broken, forming a dense rust layer dominated by Fe3O4, Fe2O3 and FeOOH. Si enriches in the inner rust layer adjacent to the matrix and pitting cavities, inhibiting pitting deepening and promoting γ-FeOOH to α-FeOOH transformation, thus improving the steel's corrosion resistance.

Titanium-bearing blast furnace slag is rich in high-melting-point titanium-containing minerals including perovskite, melilite and spinel, which result in the loss of titanium resources and hinder the comprehensive utilization of such slag. On this basis, combined with process mineralogy theories, this study adopted multiple characterization methods, including a polarized light microscope with transmitted and reflected light, XRD and EPMA. These simulations reveal that the bulk SiO2 content dictates titanium distribution among the mineral phases, thereby laying a solid foundation for the subsequent experiments. Meanwhile, quantitative analyses were performed on the microstructure, mineral composition and perovskite grain size of the slag. The occurrence state and migration law of titanium in the slag were systematically investigated. The results show that the microstructure of titanium-bearing blast furnace slag presents a porphyritic structure at different SiO2 levels. Its main mineral phases include perovskite, pyroxene, spinel and glass. Titanium is predominantly hosted in perovskite, with small amounts distributed in the pyroxene, spinel and glass phases. Reducing the SiO2 content facilitates the formation and grain coarsening of perovskite and promotes the migration of titanium from pyroxene and glass into perovskite. When the SiO2 content is 20%, the perovskite content reaches 44.3%. Among them, the proportion of grains larger than 40 μm is 59.94%, and the distribution ratio of titanium in perovskite is 86.78%. Under the experimental conditions of this study, 20% SiO2 is the optimal level. These findings can provide a theoretical reference for the efficient separation and recovery of titanium from titanium-bearing blast furnace slag.

Surface nanocrystallization is a critical approach for improving mechanical and functional properties of materials. Beyond conventional mechanical routes, chemical loading presents a promising pathway for nanocrystallization via interstitial-driven phase transformation. However, the characteristics and mechanisms underlying chemical load-induced nanostructuring remain insufficiently elucidated. This work investigates the surface nanocrystallization of 17-4 PH martensitic stainless steel during low-temperature plasma nitriding at 350 °C. Microstructural characterization combining XRD, EPMA, and TEM revealed a nitrogen-saturated layer with a maximum hardness of 13.5 GPa. The modified layer consists of nanoscale domains formed via a diffusionless martensite-to-austenite transformation, as evidenced by broadened FCC peaks, dark-field images, and the absence of elemental partitioning in EDX maps. This process is driven by the cyclic accumulation of chemical and elastic-strain energy at the advancing nitrogen diffusion front, triggering a self-sustaining, periodic transformation. This study introduces a chemical-driven nanocrystallization mechanism for novel design of surface-nanostructured steels via controlled thermochemical processing.

The Li K-L emission spectra of lithium metal and its binary compounds (Li3N, Li2O, and LiF) were measured by using a soft X-ray emission spectrometer (SXES), which was equipped with a newly developed high-efficiency diffraction grating (JS35BC) and attached to an electron probe microanalyzer (EPMA). The new grating enables the observation of the entire intensity profile of both Li K-L and Mg L2,3-M emission spectra. The systematic energy shift of the Li K-L spectra to the lower energy side with an increasing electronegativity (or the ionization tendency) of elements of N, O, and F bonded with the Li atom was clearly detected. This shift was reproduced by theoretical calculations and was assigned mainly due to the change of the binding energy of the valence band of those materials. The main peak and its distinct shoulder structure observed in Li K-L spectrum of LiF were assigned as 2p dominated and 2 s + 2p mixed states, respectively, from the comparison with theoretical calculations.

This study investigates the influence of strontium (Sr) salt chemistry (Sr(OH)2·8H2O, SrCO3, Sr(NO3)2, and SrSO4) on the nanostructural evolution of potassium silicate-activated geopolymers. High-field multinuclear (27Al, 29Si, 39K, and 87Sr) MAS NMR, synchrotron XANES, EPMA, XRD, and FTIR showed that while the primary binding phase in all samples is a disordered, highly cross-linked K-A-S-H gel, the Sr immobilisation mechanism is governed by salt solubility. Soluble nitrate and hydroxide salts release Sr2+ ions that are chemically incorporated into the K-A-S-H gel framework in brewsterite-type pseudo-zeolitic environments. In contrast, insoluble carbonate and sulfate salts act primarily as physical fillers, and are encapsulated as discrete particles within the geopolymer matrix, though sulfate additionally reacts to form secondary crystalline kalistrontite (K2Sr(SO4)2). Sr2+ adsorption on metakaolin surfaces is found to inhibit early-stage Al dissolution, resulting in a Si-rich K-A-S-H gel that transitions to an Al-rich K-A-S-H gel over 28 days. These results provide new insight into the mechanisms of immobilisation of Sr in geopolymers, and highlight their potential as wasteforms for long-term management of 90Sr radioactive waste.

In recent years, economically significant sandstone-hosted uranium mineralization has been identified in the Louzhuangzi area along the southern margin of the Junggar Basin. However, the controls on uranium enrichment and their links to depositional architecture and post-depositional fluid processes remain insufficiently constrained. This study integrates field geological investigations, drill-core lithofacies logging, and systematic sampling with petrographic and micro-analytical techniques, including optical microscopy, scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and transmission electron microscopy (TEM). The objective is to elucidate the depositional characteristics, alteration processes, and uranium occurrence mechanisms of the ore-bearing sandstones within the Toutunhe Formation (J2t). Results show that the upper member (J2t2) represents meandering-river deposits, whereas economically significant uranium mineralization is hosted in the lower member (J2t1), characterized by braided-river sandstone units with high permeability. The sandstones of the Toutunhe Formation (J2t) exhibit intense oxidation by surficial fluids, overprinted by post-mineralization hydrothermal alteration and sulfide-forming alteration associated with reducing fluids. Uranium is closely associated with pyrite, organic matter, and clay minerals. Uranium minerals are dominated by coffinite and pitchblende (~68%), with UO₂ contents of 52.89-86.07%. Minor Ti-bearing uranium phases (~16%), interpreted as possible brannerite, contain 38.01-41.46% UO₂ and 31.67-36.09% TiO₂, while nanoscale uranium minerals (~16%) show UO₂ contents of 9.15-60.28%. These results indicate that uranium mineralization was controlled by the coupling of braided-channel architecture and multi-stage fluid processes. Uranium was initially precipitated from oxidized fluids and subsequently modified and preserved by later thermal and reducing fluids, highlighting the importance of multi-fluid interactions in sandstone-hosted uranium systems.

Extractive pyrometallurgy is an established process for recycling lithium-ion batteries (LIB). One approach to recover lithium from slags produced by pyrometallurgical recycling of LIB involves accumulating lithium in an engineered artificial mineral (EnAM) facilitating recovery. &#x3b2;-Eucryptite (LiAlSiO4) is a promising EnAM-candidate as it is chemically similar to the primary lithium ore spodumene (LiAlSi2O6) making co-processing a viable option. However, for economic recycling the &#x3b2;-eucryptite must have a high lithium content, a high purity, and display a favorable microstructure. The presented work aims to quantify all three parameters. An industrial pyrometallurgical slag was analyzed using scanning electron microscopy (SEM), electron probe microanalysis (EPMA) and laser ablation inductively coupled plasma mass spectroscopy (LA-ICP-MS). The analyzed &#x3b2;-eucryptite shows a high lithium content of 5.45 mass % while containing only low amounts of iron (0.64 mass %) and calcium (0.2 mass %). However, small mean grain sizes (< 21 &#xb5;m) and unfavorable grain shapes impede the separation of &#x3b2;-eucryptite. It was discovered that chromium and vanadium were accumulated in spinel phases of the chromite-coulsonite solid solution series. Producing a Cr, V-bearing spinel concentrate would enable the recycling of both metals as well as improving the quality of the residual lithium-depleted slag as a by-product.

The influence of tempering temperature within the range of 520 &#xb0;C to 640 &#xb0;C on the microstructure and mechanical properties of 04Cr13Ni5Mo maraging stainless steel was systematically studied. The evolution of crystallographic orientation information, such as phase ratio and grain boundary ratio of the studied steel at different tempering temperatures, was studied by utilizing the electron backscatter diffraction (EBSD) technique. Furthermore, the element distribution at typical tempering temperatures was quantitatively analyzed by utilizing the electron probe microanalysis (EPMA) technique. Results indicated that the microstructure of the studied steel at different tempering temperatures is mainly composed of tempered sorbite. As the tempering temperature increased from 520 &#xb0;C to 640 &#xb0;C, the proportion of low-angle grain boundaries gradually increased while the proportion of large-angle grain boundaries decreased. The content of reversed austenite showed a sharp increase with the elevation of tempering temperature and peaked at approximately 9.0% at a tempering temperature of 640 &#xb0;C. With the tempering temperature increasing from 520 &#xb0;C to 640 &#xb0;C, the strength of the studied steel showed a trend of first decreasing, then stabilizing, and then decreasing again, while the plasticity showed a stable upward trend. When the tempering temperature was 610 &#xb0;C, the strength, plasticity, and toughness of the studied steel achieved the optimal match. The enrichment of the Ni element during the austenite reverse phase transformation process was confirmed as the predominant factor ensuring the stability of the reverse austenite to room temperature.

Diffusion-controlled processes exert an indispensable influence on the thermal processing and microstructural homogenization of &#x3b2;-titanium alloys containing multiple &#x3b2;-stabilizing elements. However, credible multicomponent diffusion kinetic data corresponding to the &#x3b2;-phase within the Ti-Zr-Ta ternary system remain inadequate. In this work, diffusion characteristics within the &#x3b2; single-phase domain of the Ti-Zr-Ta system were investigated using solid-state diffusion couples combined with a numerical inverse method. Twelve diffusion couples in total were synthesized and subjected to annealing treatments at 1373, 1423, and 1473 K, with the corresponding composition-distance distributions quantified by electron probe microanalysis (EPMA). The composition-dependent main interdiffusion coefficients were measured via the numerical inverse method embedded in the HitDIC computational platform, while the atomic mobility parameters corresponding to the &#x3b2;-phase were refined to replicate the experimental concentration distributions and diffusion trajectories across the studied temperature and composition intervals. The results reveal pronounced temperature and composition dependence of the main interdiffusion coefficients, and the diffusion rate of Zr is faster than that of Ta in the &#x3b2; phase.

In the context of spent fuel recycling and the valorization of plutonium, (U,Pu)O2 mixed oxides (MOX) have been developed for use in French Pressurized Water Reactors (PWR). They are also leading candidates for some GEN IV reactor concepts, such as sodium-cooled fast reactors (SFR). One of the critical challenges in the nuclear industry is the mastery of the nuclear fuel cycle, specifically plutonium multirecycling. In order to achieve this goal, it is crucial to identify the secondary phases created during irradiation. In this work, (U,Pu)O2 MOX have been doped with 11 stable fission products (FP) (Sr, Y, La, Nd, Ce, Zr, Mo, Pd, Rh, Ru, Ba) to reproduce FP-based precipitates existing in the real spent fuel. The structural and microstructural properties of these secondary phases were characterized by coupling scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), Electron Probe MicroAnalysis (EPMA), and synchrotron techniques such as X-ray Absorption Spectroscopy (XAS) and Synchrotron Powder X-ray Diffraction (SP-XRD). This analysis highlights the relationship between the partial segregation among metallic FP (Mo, Pd, Rh, Ru) and their crystallographic structures, as well as the speciation shift of several FP induced by the addition of Ba. The synthesized SIMMOX samples present a secondary phase representative of irradiated MOX and can be used as an effective model material to study spent nuclear fuel and its reprocessing.

The Gallows Hill Phonolite is a Triassic, fine-grained subvolcanic sill outcropping within the Upper Devonian Mansfield Basin, in Victoria (Australia), containing elevated concentrations of Zr-Nb-RE elements (&#x223c;0.26-0.28 wt%), and was recently assessed for critical mineral potential by the Geological Survey of Victoria (Andrews et al., 2025). This study found the bulk rock chemistry is homogeneous, however fine-grained mineralogy which is very complex was observed warranting further study. Here, we performed hyperspectral X-ray and cathodoluminescence (CL) mapping in an electron probe microanalyzer (EPMA), coupled with an automated cluster analysis combined with quantitative analysis of clustered X-ray spectra of discrete phases. This approach identified and quantified over 35 phases from Gallows Hill phonolite, including several unexpected rare phases. A standards-based energy dispersive X-ray spectrometry (EDS) quantification method measured compositions in agreement with expected mineral stoichiometry, with elemental detection limits in the range of <&#x223c;20-1,000&#x2005;ppm, depending on phase abundance, and proved reliable even for challenging mineral species, such as Zr-Nb-Ti and multi-rare earth element (REE)-bearing minerals. The mineral identification and clustering procedure revealed compositional variations across different minerals, as well as distinct CL signals, indicating that the rock samples recorded overprinting of the original mineralogy. Our results show that the rocks' textures indicate late-stage magmatic crystallization of Zr-Nb-Ti silicate phases together with REE-mineralogy like worldwide reported alkali igneous Zr-Nb-REE deposits (analogous Toongi-Dubbo Zr-Nb-Hf-REE deposit in New South Wales, Australia). Secondary overprints altered the rocks, leading to the dissolution of feldspathoids, as well as remobilization and locally redepositioning of various Zr-Nb-REE phases.

Weathering of sulfide-bearing mine waste poses long-term environmental risks through coupled acid generation and release of toxic elements, notably thallium (Tl) and arsenic (As). Despite their high toxicity, the mineralogical controls on Tl and As sequestration during progressive weathering remain poorly constrained. Here, we elucidate the divergent migration and attenuation pathways of Tl and As by identifying their dominant hosts across distinct weathering stages. In unweathered mine waste, LA-ICP-MS reveals enrichment of Tl and As in pyrite structural defects and grain margins, rendering them susceptible to preferential release during oxidative dissolution. In weakly weathered layers, Tl and As concentrations reach up to 710 and 2090&#x202f;mg&#x202f;kg-1, respectively, with both elements predominantly retained in the residual fraction. Combined XRD, SEM-EDS, and EPMA confirm that jarosite serves as the dominant host for Tl and As, with their association consistent with structural incorporation via Tl+-K+ and arsenate-sulfate substitution. During advanced weathering, rising pH initiates gradual jarosite dissolution. In contrast to Tl, which is efficiently scavenged by pedogenic Mn oxides in the regolith, As undergoes progressive depletion, reflecting its limited retention by Fe-(hydr)oxides under near-neutral pH conditions. These findings demonstrate that the dynamic evolution of secondary mineral assemblages governs the decoupling of Tl and As cycling during weathering, providing a predictive mineralogical framework for stage-specific remediation strategies to mitigate their release.

Breast cancer (BC) is the most commonly diagnosed malignancy in women (&#x223c;25% of new cases). Plants adapted to specific niches accumulate secondary metabolites with bioactivity, including anticancer effects. The objective of this study was to evaluate the chemopreventive and treatment potential of Vaccinium myrtillus (bilberry) peel-enriched pomace powder in BC models, hypothesizing system-level effects and synergy with standard therapy. Chemistry was profiled by liquid chromatography with diode-array detection-mass spectrometry (LC-DAD-MS)/liquid chromatography with diode-array detection (LC-DAD) from 2 extracts: BILHEX (hexane) and BILMeOH (methanol). Biology was tested in the following: 1) 4T1 triple-negative mouse model (treatment); 2) NMU rat mammary carcinogenesis (chemoprevention); and 3) in vitro assays with MCF-7 and MDA-MB-231, including 3D spheroids and cisplatin combinations. BILMeOH was enriched for phenolics; BILHEX for unsaturated triacylglycerols/triterpene acids. Compared with control, bilberry diet reduced 4T1 tumor volume by 51% and 91% (low/high dose; P < 0.05/0.001), lowered mitotic index (P < 0.001), and reduced necrosis:tumor ratio (P < 0.05). In NMU rats, chemoprevention increased cleaved caspase-3 (P < 0.05) and Bax/Bcl-2 (P < 0.001), and decreased Ki-67 (P < 0.05), MDA, and CD133 (P < 0.01). Histone marks shifted (&#x2193;H3K4me3 P < 0.05; &#x2191;H4K20me3 P < 0.01; &#x2191;H4K16ac P < 0.001). Promoter methylation was gene-specific (e.g., RASSF1 +12% absolute, P < 0.05); low-baseline loci were treated as low magnitude. miRNA profiling (758 features) identified significant dysregulation (|FC| &#x2265; 2) of let-7d-5p, let-7i-5p, miR-1224-3p, miR-494-3p, and miR-6216. TGF-&#x3b2; and IL-10 increased (both P < 0.001), IL-6 rose (P < 0.05), indicating selective immunomodulation. Metabolomics showed shifts in lactate (P < 0.05), branched-chain ketoacids (P < 0.05/0.01), and histidine (P < 0.001). In vitro, BILHEX suppressed proliferation, induced G2/M arrest, activated intrinsic apoptosis (cytochrome-c &#x2192; caspase-9 &#x2192; caspase-3/7 &#x2192; PARP), and synergized with cisplatin in 3D spheroids (Bliss). Bilberry pomace shows multitarget anticancer activity across BC models; translational studies should confirm mechanisms, refine dosing, and explore biomarker-guided use.