Helium Ion Microscopy Research Articles

Isolation and characterization of bacteriophages specific to Streptococcus equi subspecies zooepidemicus and evaluation of efficacy ex vivo.

Streptococcus (S.) equi subspecies (subsp.) zooepidemicus is an important facultative pathogen in horses and can cause severe infections in other species including humans. Facing the post-antibiotic era, novel antimicrobials are needed for fighting bacterial infections. Bacteriophages (phages) are the natural predators of bacteria and discussed as a promising antimicrobial treatment option. The objective of this study was to isolate and characterize S. equi subsp. zooepidemicus-specific phages for the first time and to evaluate their efficacy in vitro and ex vivo. In total, 13 phages with lytic activity were isolated and host ranges were determined. Two phages with broad host ranges and high efficiency of plating (vB_SeqZP_LmqsRe26-2 (lytic activity: 30/37 bacterial isolates) and vB_SeqZP_LmqsRe26-3 (lytic activity: 29/37 bacterial isolates)) and one phage with relatively low efficiency of plating (vB_SeqZP_LmqsRe26-1) were selected for further characterization, including electron microscopy and whole genome sequencing. In in vitro planktonic killing assays at two tested multiplicities of infection (MOI 1 and MOI 10), significant bacterial growth reduction was observed when the phages vB_SeqZP_LmqsRe26-2 and vB_SeqZP_LmqsRe26-3 were added. These phages were subsequently co-incubated with clinical S. equi subsp. zooepidemicus isolates in an equine endometrial explant model but did not achieve bacterial growth reduction at MOI 1 and MOI 10. However, helium ion microscopy revealed presence of particles adherent to the bacteria on the explant after incubation (25 h), suggesting possible phage-bacteria interactions. In conclusion, phages against S. equi subsp. zooepidemicus were successfully isolated and characterized. Promising results were observed in in vitro but no significant reduction was detected in ex vivo experiments, requiring additional investigations. However, after further adaptations (e.g., optimization of MOIs and phage administration or use of phage-antibiotic combination), phages could be a potential antimicrobial tool for future therapeutic use in S. equi subsp. zooepidemicus infections, although the available results do not currently support the therapeutic usage.

Surface plasmons on silver gratings transform pyrolytic carbon into luminescent graphitized carbon dots.

Plasmonic catalysis holds the promise of opening new reaction pathways that are inaccessible thermally or via direct UV-vis electronic transitions. Here, energetic carriers produced via the decay of surface plasmons excited by visible light at 532nm (2.33eV, green) on a Ag-grating-bearing pyrolytic carbon residue drive its transformation into light-emitting graphitized carbon dots. The pyrolytic carbon residue is detectable via high-magnification surface-enhanced Raman scattering but cannot be directly observed using optical, electron, atomic force, or helium ion microscopy. When a Ag-grating-bearing pyrolyzed residue is introduced into a high-purity O2-depleted gas environment (Ar, N2, and CO2) and excited with 532nm light, bright yellow luminescence emerges and is readily observed. Light emission is not observed without the pyrolytic carbon, without the excitation of plasmons, or in air or an Ar/O2 gas mixture. This process, driven by visible light and a nanostructured Ag surface bearing pyrolytic carbon, will be of interest to researchers involved in plasmonic catalysis, catalytic processes involving carbon, and luminescent plasmonic surfaces.

Doped multi-walled carbon nanotubes and nanoclay based-geopolymer concrete: An overview of current knowledge and future research challenges

This in-depth review aims to shed light on the application of nanoclay and multi-walled carbon nanotubes in geopolymer concrete. It comprehensively examines the profound impact of these nanomaterials on the physical, chemical, and mechanical properties of geopolymer concrete. The review delves into the intricate details of the properties exhibited by nanoclay and multi-walled carbon nanotubes, providing valuable insights into their unique physical and chemical characteristics. It also explores the methodologies adopted for their dispersion and the underlying functionalities within geopolymer composite. The review highlights advanced imaging and characterization techniques essential for understanding surface and mechanical properties. The review compares imaging techniques (scanning electron microscopy, transmission electron microscopy, helium ion microscopy, and atomic force microscopy), emphasizing their importance in characterizing mechanical properties of nanocomposites. A detailed discussion on the fresh and hardened mechanical properties, specifically compressive and flexural strength, of geopolymer concrete incorporating nanoclay and multi-walled carbon nanotubes is also included. Addressing key challenges and offering perspectives on future developments in the realm of geopolymer concrete, this review serves as a comprehensive exploration of the subject.

Shifting shapes: Density variations and physicochemical characteristics from spheres to rods

This work extensively explores purifying cetyltrimethylammonium bromide (CTAB)-stabilized gold nanorods, focusing on efficiently separating spheres and rods to achieve a rod-rich suspension in one cycle. Utilizing UV–vis spectroscopy and Helium ion microscopy, the study delves into nanorods' spectral traits across different aspect ratios (AR 3–6). Results show centrifugation greatly influences gold nanorods' spectral features, indicating a link between CTAB-coated nanorod density and absorbance levels post-centrifugation. This quantitative evaluation enhances understanding of purification dynamics, highlighting effects on purity and density while offering insights for future refinements. Emphasizing centrifugation's role in reducing byproducts, nanoparticle density changes, and absorbance variations, the study's consistent spectral profiles affirm the effectiveness of purification parameters for stability and nanoparticle density maintenance. By quantitatively analyzing centrifugation duration's impact on spectral properties and shape separation dynamics, the research provides an empirical foundation for optimizing gold nanorod suspension purification processes. Additionally, a clear correlation between AR and absorbance-to-density ratios pre- and post-centrifugation underscores AR's relevance in comprehending nanorods' optical traits amidst centrifugation, benefiting purification strategies.

Theoretical and experimental perspectives on localized plasmons in gold nanospheroids

Theoretical frameworks play a pivotal role in comprehending the optical characteristics of gold nanorods, providing valuable perspectives on the factors that impact their optical properties. These frameworks play a key role in anticipating how nanorods will perform under different circumstances and in validating experimental findings against theoretical projections. Through the utilization of theoretical frameworks, scientists can efficiently delve into creative nanostructure designs, ultimately enriching our understanding of how gold nanorods react optically for both academic research and practical implementations. The optical behavior of elongated gold spheroids was extensively analyzed using both the quasi-static approximation (QSA) and the Modified Long Wavelength Approximation (MLWA) to gauge their effectiveness in projecting experimental results. While the QSA proves beneficial in specific scenarios, its accuracy tends to be overshadowed by empirical data obtained from UV–visible spectroscopy and helium ion microscopy (HIM). In contrast, the MLWA exhibits a stronger alignment with empirical findings, thus providing a more accurate theoretical groundwork. This alignment implies that the MLWA considers intricacies and variables overlooked by the QSA, establishing it as a more dependable approach for envisaging the optical conduct of such nanostructures. The juxtaposition emphasizes the significance of selecting appropriate theoretical frameworks in the realm of nanoscale optics, with the MLWA emerging as the preferred option for investigations concerning elongated gold spheroids.

Gold nano densities: Relationship with drying parameters

Gold nanorod stain deposits have been studied using helium ion microscopy (HIM). The multilayer thick deposits can become well-organized monolayers when the density drops, as demonstrated by the density fluctuation of nanosuspension. However, once the density of nanoparticles approaches certain extremely low values, this tendency has disappeared. The difference in density associated with the liquid crystalline (LC) phases that have developed on the surface. There is a correlation between the density of nanoparticles in suspension and the relationship between droplet volume and UV-Vis absorbance. The physical characteristics that affect and generate such LC phases are contrasted and examined with the assembly method. To highlight noteworthy aspects, a quantitative comparison between the HIM analysis and the SEM is also made. Analyzing the correlation between the coffee stain range, nanoparticle density, and droplet contact angle is essential. It is possible to quantify the difference in the ring stains from the outside to the midle and from the midle to the inner boundary. HIM is typically useful when attempting to determine the true composition of surface deposits. The aim of this work is to investigate the effects of particle density on liquid crystalline superstructures and the coffee stain effect.

Studies of the Morphology of Hematite Synthesized from Waste Iron Sulfate.

Microwave-based reactions have gained traction in recent years due to their ability to enhance reaction rates and yield while reducing energy consumption. Also, according to the conception of 'waste to materials', various waste feeds are intensively sought to be tested. The experimental setup of this study involved varying pH levels, oxidation agents, and precipitation agents to optimize the synthesis process of iron red based on waste iron sulfate. The selection of oxidation and precipitation agents was found to significantly influence the pigment synthesis process. Various oxidizing agents, including hydrogen peroxide and atmospheric air, were evaluated for their effectiveness in promoting the oxidation of ferrous ions to ferric ions, essential for pigment formation. Additionally, different precipitation agents such as sodium hydroxide and ammonia solution were assessed for their ability to precipitate iron hydroxides and facilitate pigment particle formation. The characterization of synthesized pigments revealed promising results in terms of quality and color properties. Helium Ion Microscopy (HIM) analysis confirmed the formation of well-defined pigment particles with controlled morphology. X-ray diffraction (XRD) studies provided insights into the crystalline structure of the pigments, indicating the presence of characteristic iron oxide phases. By improving this technology, waste iron sulfate can be efficiently transformed into valuable iron pigments, offering a sustainable solution for waste management while meeting the growing demand for high-quality pigments.

Shot noise-mitigated secondary electron imaging with ion count-aided microscopy

Modern science is dependent on imaging on the nanoscale, often achieved through processes that detect secondary electrons created by a highly focused incident charged particle beam. Multiple types of measurement noise limit the ultimate trade-off between the image quality and the incident particle dose, which can preclude useful imaging of dose-sensitive samples. Existing methods to improve image quality do not fundamentally mitigate the noise sources. Furthermore, barriers to assigning a physically meaningful scale make the images qualitative. Here, we introduce ion count-aided microscopy (ICAM), which is a quantitative imaging technique that uses statistically principled estimation of the secondary electron yield. With a readily implemented change in data collection, ICAM substantially reduces source shot noise. In helium ion microscopy, we demonstrate 3[Formula: see text] dose reduction and a good match between these empirical results and theoretical performance predictions. ICAM facilitates imaging of fragile samples and may make imaging with heavier particles more attractive.

Recovery of rare earth elements from mining wastewater with aminomethylphosphonic acid functionalized 3D-printed filters

Herein we report the use of nylon-12-based 3D-printed filters incorporating α-aminomethylphosphonic acid as an active additive for the recovery of Y, Nd, and Dy from the mining waste solution containing Al, K, Ca, Sc, Fe, Co, Cu, Zn, Y, Nd, Dy, and U. Nylon-12 was chosen for the polymer matrix of the filter due to its inactivity towards the studied metals. The micrometer-level structure of the filters was studied with a scanning helium ion microscope and X-ray tomography to reveal the porosity, pore size, and active additive distribution in the filters. Furthermore, FTIR spectroscopy was used to analyze the compositional changes in the 3D-printed filters after the printing and adsorption processes. Adsorption of the metals was studied at a pH range of 1–4, and the following adsorption trend Sc > Fe > U > Y, Nd, Dy > Al, Cu, Zn > K, Ca, Co was observed in each of the studied pH values. The sequential recovery process for metals was studied at pH 2, and desorption of the metals from the filters was performed with 6 M HNO3. 100 % adsorption of REEs, Fe, and U was achieved during the recovery process, and on average, over 88 % of the adsorbed Y, Nd, and Dy were desorbed from the filters. In contrast to Y, Nd, and Dy, the desorption of Sc, Fe, and U was minimal (Fe and U) or negligible (Sc) with 6 M HNO3 due to their strong coordination to the active additive. Maximum adsorption capacities for Y, Nd, Dy, and U were determined by using linear Langmuir adsorption isotherm. The best maximum adsorption capacity was determined for Sc, Qmax = 0.51 mmol/g followed by U, Nd, Dy, and Y with capacities of 0.47, 0.24, 0.23, and 0.17 mmol/g, respectively. Overall, this study achieved a complete removal of Sc, Fe, and U from the simulated mining waste solution leaving a final eluate that mainly contained Y (320 μg), Nd (350 μg), Dy (330 μg), and Al (710 μg) demonstrating the applicability of the 3D-printed filters in the recovery of Y, Nd, and Dy from the multimetal solution.

Controllable Fabrication of Sub-10 nm Graphene Nanopores via Helium Ion Microscopy and DNA Detection.

Solid-state nanopores have become a prominent tool in the field of single-molecule detection. Conventional solid-state nanopores are thick, which affects the spatial resolution of the detection results. Graphene is the thinnest 2D material and has the highest spatial detection resolution. In this study, a graphene membrane chip was fabricated by combining a MEMS process with a 2D material wet transfer process. Raman spectroscopy was used to assess the quality of graphene after the transfer. The mechanism behind the influence of the processing dose and residence time of the helium ion beam on the processed pore size was investigated. Subsequently, graphene nanopores with diameters less than 10 nm were fabricated via helium ion microscopy. DNA was detected using a 5.8 nm graphene nanopore chip, and the appearance of double-peak signals on the surface of 20 mer DNA was successfully detected. These results serve as a valuable reference for nanopore fabrication using 2D material for DNA analysis.

Contribution of black carbon and desert dust to aerosol absorption in the atmosphere of the Eastern Arabian Peninsula

Discriminating the absorption coefficients of aerosol mineral dust and black carbon (BC) in different aerosol size fractions is a challenge because of BC's large mass absorption cross-section compared to dust. Ambient aerosol wavelength dependent absorption coefficients (babs) in supermicron and submicron size fractions were determined with a high time resolution. The measurements were performed simultaneously using identical systems at an urban and a regional background site in Qatar. At each site, measurements were taken by co-located Aethalometers, one with a virtual impactor (VI) and the other with a PM1 cyclone to respectively collect super-micron-enhanced and submicron fractions. The combined measurement of aerosol absorption and scattering coefficients enabled the particles to be classified based on their optical properties' wavelength dependence. The classification reveals the presence of BC internally/externally mixed with different aerosols. Helium ion microscopy images provided information concerning the extent of mineral dust in the submicron fraction. The determination of absorption coefficients during dust storms and non-dust periods was used to establish the absorption Ångström exponent for dust and BC. Non-parametric wind regression, potential source contribution function and back-trajectory analysis reveal major regional sources of desert dust associated with north-westerly winds and a minor local dust contribution. In contrast, major BC sources found locally were associated with south-westerly winds with a smaller contribution made by offshore emissions transported by north-easterly and easterly winds. The use of a pair of Aethalometers with VI and PM1 inlets separates contributions of BC and dust to the aerosol absorption coefficient.

Contributions of Chinese hamster ovary cell derived extracellular vesicles and other cellular materials to hollow fiber filter fouling during perfusion manufacturing of monoclonal antibodies.

Hollow fiber filter fouling is a common issue plaguing perfusion production process for biologics therapeutics, but the nature of filter foulant has been elusive. Here we studied cell culture materials especially Chinese hamster ovary (CHO) cell-derived extracellular vesicles in perfusion process to determine their role in filter fouling. We found that the decrease of CHO-derived small extracellular vesicles (sEVs) with 50-200 nm in diameter in perfusion permeates always preceded the increase in transmembrane pressure (TMP) and subsequent decrease in product sieving, suggesting that sEVs might have been retained inside filters and contributed to filter fouling. Using scanning electron microscopy and helium ion microscopy, we found sEV-like structures in pores and on foulant patches of hollow fiber tangential flow filtration filter (HF-TFF) membranes. We also observed that the Day 28 TMP of perfusion culture correlated positively with the percentage of foulant patch areas. In addition, energy dispersive X-ray spectroscopy-based elemental mapping microscopy and spectroscopy analysis suggests that foulant patches had enriched cellular materials but not antifoam. Fluorescent staining results further indicate that these cellular materials could be DNA, proteins, and even adherent CHO cells. Lastly, in a small-scale HF-TFF model, addition of CHO-specific sEVs in CHO culture simulated filter fouling behaviors in a concentration-dependent manner. Based on these results, we proposed a mechanism of HF-TFF fouling, in which filter pore constriction by CHO sEVs is followed by cake formation of cellular materials on filter membrane.

Focused Helium Ion and Electron Beam-Induced Deposition of Organometallic Tips for Dynamic Atomic Force Microscopy of Biomolecules in Liquid.

We demonstrate the fabrication of sharp nanopillars of high aspect ratio onto specialized atomic force microscopy (AFM) microcantilevers and their use for high-speed AFM of DNA and nucleoproteins in liquid. The fabrication technique uses localized charged-particle-induced deposition with either a focused beam of helium ions or electrons in a helium ion microscope (HIM) or scanning electron microscope (SEM). This approach enables customized growth onto delicate substrates with nanometer-scale placement precision and in situ imaging of the final tip structures using the HIM or SEM. Tip radii of <10 nm are obtained and the underlying microcantilever remains intact. Instead of the more commonly used organic precursors employed for bio-AFM applications, we use an organometallic precursor (tungsten hexacarbonyl) resulting in tungsten-containing tips. Transmission electron microscopy reveals a thin layer of carbon on the tips. The interaction of the new tips with biological specimens is therefore likely very similar to that of standard carbonaceous tips, with the added benefit of robustness. A further advantage of the organometallic tips is that compared to carbonaceous tips they better withstand UV-ozone cleaning treatments to remove residual organic contaminants between experiments, which are inevitable during the scanning of soft biomolecules in liquid. Our tips can also be grown onto the blunted tips of previously used cantilevers, thus providing a means to recycle specialized cantilevers and restore their performance to the original manufacturer specifications. Finally, a focused helium ion beam milling technique to reduce the tip radii and thus further improve lateral spatial resolution in the AFM scans is demonstrated.

Preparation of Borrelia-Infected Mammalian Cells for Helium Ion Microscopy.

Preparation of mammalian cells for a Borrelia burgdorferi infection can be cumbersome especially if investigating possible cell entry processes. The initial steps of infection or entry into cells by a pathogen often involve attachment to the cell surface and plasma membrane changes. To topologically investigate with great resolution and detail these interactions of the pathogen and the mammalian cell, helium ion microscopy (HIM) can be employed. Here we describe a protocol used to define a specific multiplicity of infection (MOI) of Borrelia burgdorferi on a human chondrosarcoma cell line (SW1353) so that fine detail structures on the mammalian cell can be observed and quantified by HIM.

Scanning Ion Microscopy and Its Application in Microbiology

Helium ion microscopy, a scanning microscope operating with ions rather than electrons, is one of the best equipment to analyze the surface of cells and the surface of intracellular compartments exposed by different methods. This short review aims to show the advantages of resolution and depth of focus in some microorganisms such as viruses, bacteria, fungi and parasitic protists.

Defects distribution and evolution in selected-area helium ion implanted 4H–SiC

An experimental demonstration of the generation of VSi, CSiVC, and NCVSi color centers in 4H–SiC using helium ion microscope irradiation of 5 × 5 μm2 areas with subsequent annealing treatment is presented. With the aid of transmission electron microscopy (TEM), photoluminescence (PL) and cathodoluminescence (CL) spectroscopy and Raman stress analysis, the evolution and distribution of color centers were thoroughly investigated. Cross-sectional TEM revealed the presence of helium bubbles in the center of the regions implanted with high doses which account for the observed quench of PL emission in the center of the implanted regions in both PL and CL measurements. PL spectra from the virgin, implanted and annealed samples proved the appearance of VSi after implantation and the transformation from VSi to CSiVC and NCVSi centers after annealing at 1000 °C. Moreover, with the increase of the implantation dose, the area of NCVSi centers increases whereas that of CSiVC decreases, which provide the first evidence of the competitive relationship between the formation of CSiVC and NCVSi defects. The comparison between stress distribution and CSiVC defect distribution illustrated that CSiVC centers predominantly distributed around the surface rupture region after thermal annealing where significant stress repair occurred. The results show that focused helium ion implantation holds promise for the precise coupling of VSi, CSiVC and NCVSi centers in predefined locations in integrated photonics applications.

Assembly of nanoparticles at symmetric coffee stain locations

The precise picture of the nanoparticle array deposits on the substrate surface is crucial since many uses for nanostructures are dependent on how the assembled array's collective behavior responds to various physicochemical properties. The well-known seed-mediated approach was used to synthesize gold nanorods stabilized by CTAB molecules. Due to the Helium Ion Microscope’s (HIM) remarkable ability to reveal the real nature of the deposited entities, gold nanorod arrays at symmetrical parts of the coffee-stain ring have been studied using this technique. The object of this study is to evaluate three different positions within the coffee-stain ring at the convective symmetric locations. In the context of the self-assembled mechanism, the formation of various liquid crystalline phases induced by the evaporating symmetric convective flow inside the sessile droplet have been examined and compared at the symmetric positions within the ring.

Well-Tunable, 3D-printable, and Fast Autonomous Self-Healing Elastomers

Self-healing elastomers provide extended longevity of functional materials, due to their unique adaptability and durability. However, a major scientific challenge remains in developing materials with a rapid healing process combined with decent mechanical properties, that can be prepared by a relatively simple synthesis approach. Herein, we report a versatile design approach on self-healing elastomers by incorporating two different hydrogen bonding containing monomers, i.e., 2-[[(butylamino)carbonyl]oxy]ethyl acrylate (BCOE) and 2-ureido-4[1H]pyrimidinone (UPy) functionalized ethyl methacrylate. Poly(BCOE-r-UPy)s are synthesized by reversible addition−fragmentation chain-transfer (RAFT) polymerization, and controlling the ratio of two monomers enables well-tunable mechanical properties with tensile strength ranging from 0.04 to 6.3 MPa and tensile strain up to 3,000 %. The characteristic dissociation energy is calculated from a temperature dependence of terminal relaxation followed by subtracting the segmental relaxation. The rapid autonomous self-healing is achieved when the molar composition of Poly(BCOE-r-UPy) is tailored to BCOE/UPy = 99/1. The self-healing process is monitored in situ by a helium-ion microscope, and its macroscopic study using tensile tests indicates that Poly(BCOE-r-UPy1) with 1 % molar ratio of UPy recovers 70 % of its original toughness at ambient temperature within 10 mins. 3D printing of Poly(BCOE-r-UPy) affords a self-healable 3D structure, demonstrating the adaptability of Poly(BCOE-r-UPy) for on-demand fabrication. The simplicity of synthesis, well-tunable mechanical properties, unique self-healability, and 3D printing capability of Poly(BCOE-r-UPy)s indicate their potential for a range of applications.

LixCoyOz thin-films deposition through thermal atomic layer deposition

3D-Li ion batteries are identified as one of the most promising technologies for improving portable and safe energy storage devices. One of the main remaining challenges to be tackled in that regard is the manufacture of efficient nanostructured electrode materials. In this paper, we report on the first realization of an electrochemically active cathodic LixCoyOz material grown via a thermal atomic layer deposition process based on the combination of Co(thd)2 and Li(thd) organometallic ligands and O3 as an oxidizing agent. Comprehensive characterizations comprising XPS, Raman, HIM (helium ion microscopy)-SIMS, and the first ever SEM images of a thermal-atomic layer deposition (ALD) deposited LixCoyOz material are shown and discussed as well and the very first electrochemical results to attest the electrochemical activity of the deposited material. Those results act as the first demonstration that lithiated materials and more precisely, LixCoyOz, can be grown via an advanced thermal ALD.

Characterization of mineral precipitation in artificially fractured chalk during flooding experiments for IOR research

Natural fractures in carbonate reservoirs are essential to effectively transport hydrocarbon in an otherwise low permeable matrix. However, they can reduce the wanted effect of water injection and Improved Oil Recovery (IOR), as the injected water mainly runs through the fractures. We have investigated chemical and textural alteration in and adjacent to an artificial fracture with an aperture of 2.25 (±0.05) mm in Upper Cretaceous chalk from the St. Vaast Formation (Mons Basin, Belgium). The sample has been injected mainly with 0.219 M MgCl₂ under reservoir conditions over two months. The fracture aperture reduced averagely by 76%. The analysis performed by Transmission Electron Microscopy (TEM) and X-ray Diffraction (XRD) show that, magnesite is the dominating precipitate in the fracture with sizes ranging from 0.5 to 5 μm. The abundance of magnesium phases in the fracture fill was also confirmed by Scanning Electron Microscopy (SEM) coupled with Energy-dispersive X-ray spectroscopy (EDS) and bulk geochemistry (Inductively Coupled Plasma Mass Spectrometry ICP-MS). Besides magnesite, phyllosilicates were observed by TEM and Helium Ion Microscopy combined with Secondary Ion Mass Spectrometry (HIM-SIMS). The newly formed material, precipitates, and possible reworked minerals are characterized by magnesite crystals being covered occasionally by phyllosilicates. This material has formed a distinct area bounded to the surrounding matrix. The final diameter of the precipitate measures about 2.75 (±0.15) mm, which indicates an incremental widening of the original fracture aperture. Calcite along fracture wall dissolved. Effluent concentration supports dissolution by an increase in Ca2⁺ and precipitation of magnesite by the loss of Mg2+. As either silica or aluminium is a component of the fluids, the origin of these elements is necessarily from the matrix of the chalk. It is yet unknown if phyllosilicates precipitated or was reworked, or both. Formation and concentration of magnesite and phyllosilicates in reservoir fractures can reduce fracture permeability over time and lead to subsequent propagation through the matrix of the reservoir rock. This in-depth mineralogical study of artificial fracture changes has the utmost importance for the implementation of techniques in fractured reservoirs.