Nuclear Magnetic Resonance Methods Research Articles

Cellulose-Based Polyurethane Foams of Low Flammability.

Decreasing oil resources creates the need to search for raw materials in the biosphere, which can be converted into polyols suitable for obtaining polyurethane foams (PUF). One such low-cost and reproducible biopolymer is cellulose. There are not many examples of cellulose-derived polyols due to the sluggish reactivity of cellulose itself. Recently, cellulose and its hydroxypropyl derivatives were applied as source materials to obtain polyols, further converted into biodegradable rigid polyurethane foams (PUFs). Those PUFs were flammable. Here, we describe our efforts to modify such PUFs in order to decrease their flammability. We obtained an ester from diethylene glycol and phosphoric(III) acid and used it as a reactive flame retardant in the synthesis of polyol-containing hydroxypropyl derivative of cellulose. The cellulose-based polyol was characterized by infrared spectra (IR) and proton nuclear magnetic resonance (1H-NMR) methods. Its properties, such as density, viscosity, surface tension, and hydroxyl numbers, were determined. Melamine was also added to the foamed composition as an additive flame retardant, obtaining PUFs, which were characterized by apparent density, water uptake, dimension stability, heat conductance, compressive strength, and heat resistance at 150 and 175 °C. Obtained rigid PUFs were tested for flammability by determining oxygen index, horizontal flammability test, and calorimetric analysis. Obtained rigid PUFs showed improved flammability resistance in comparison with non-modified PUFs and classic PUFs.

Research on Quantitative Diagnosis of Dendrites Based on Titration Gas Chromatography Technology

Lithium plating can cause capacity fade and thermal runaway safety issues in lithium-ion batteries. Therefore, accurately detecting the amount of lithium plating on the surface of the battery’s negative electrode is crucial for battery safety. This is especially crucial in high-energy-density applications such as battery energy storage systems or in electric vehicles (EVs). Early detection of lithium plating is crucial for evaluation of reliability and longevity. It also serves as a method for early diagnostics in practical industrial applications or infrastructure, such as EV transportation. This can enhance its impact on customers. This study validates the effectiveness of titration gas chromatography (TGC) technology in quantitatively detecting lithium plating on graphite negative electrodes in lithium-ion batteries. The results show that it can detect a minimum of 2.4 μmol of metallic lithium. Compared with the heating direct current resistance and reference electrode methods, which can be used to perform only qualitative dendrite detection, TGC has a wider range of detection. Compared with the nuclear magnetic resonance (NMR) method with higher quantitative detection accuracy, the maximum difference between the detection results of the two methods was only 7.2%, but the TGC method had lower cost and higher implementation convenience. In summary, among various dendrite detection methods, the TGC method can not only realize the effective quantitative detection of lithium plating, but also comprehensively consider its detection range, implementation convenience, cost, and detection accuracy, indicating that it is suitable for engineering applications and has the prospect of realizing large-scale quantitative detection of lithium plating in lithium-ion batteries.

NMR study of nitrate ionic liquids confined between micrometer-spaced plates

This review paper presents the results of a study conducted using nuclear magnetic resonance (NMR) methods to investigate the dynamic behaviour of ionic liquid-based compositions in micrometre-spaced confinement. Ethylammonium nitrate (EAN) and other ionic liquid (IL) systems with nitrate anion in glass or quartz spaced confinement demonstrate anomalous cation dynamics that differ from those observed in bulk and in nano-confinement. It was demonstrated that the principal axis of the nitrate anion exhibits preferential orientation to the surface, akin to that in liquid crystals. It was shown that the cation translational mobility reversibly changes during exposure to a static magnetic field. This phenomenon was interpreted as a result of intermolecular structure transformations occurring in the confined ILs. The mechanisms of these transformations were discussed.

Position-specific carbon stable isotope analysis of glyphosate: isotope fingerprinting of molecules within a mixture.

Glyphosate [N-(phosphonomethyl) glycine] is a widely used herbicide and a molecule of interest in the environmental sciences, due to its global use in agriculture and its potential impact on ecosystems. This study presents the first position-specific carbon isotope (13C/12C) analyses of glyphosates from multiple sources. In contrast to traditional isotope ratio mass spectrometry (IRMS), position-specific analysis provides 13C/12C ratios at individual carbon atom positions within a molecule, rather than an average carbon isotope ratio across a mixture or a specific compound. In this work, glyphosate in commercial herbicides was analyzed with only minimal purification, using a nuclear magnetic resonance (NMR) spectroscopy method that detects 1H nuclei with bonds to either 13C or 12C, and isolates the signals of interest from other signals in the mixture. Results demonstrate that glyphosate from different sources can have significantly different intramolecular 13C/12C distributions, which were found to be spread over a wide range, with δ13C Vienna Peedee Belemnite (VPDB) values of -28.7 to -57.9‰. In each glyphosate, the carbon with a bond to the phosphorus atom was found to be depleted in 13C compared to the carbon at the C2 position, by 4 to 10‰. Aminomethylphosphonic acid (AMPA) was analyzed for method validation; AMPA contains only a single carbon position, so the 13C/12C results provided by the NMR method could be directly compared with traditional isotope ratio mass spectrometry. The glyphosate mixtures were also analyzed by IRMS to obtain their average 13C/12C ratios, for comparison with our position-specific results. This comparison revealed that the IRMS results significantly disguise the intramolecular isotope distribution. Finally, we introduce a 31P NMR method that can provide a position-specific 13C/12C ratio for carbon positions with a C-P chemical bond, and the results obtained by 1H and 31P for C3 carbon agree with one another within their analytical uncertainty. These analytical tools for position-specific carbon isotope analysis permit the isotopic fingerprinting of target molecules within a mixture, with potential applications in a range of fields, including the environmental sciences and chemical forensics.

Cyclic Sesquiterpene-Flavanone [4+2] Hybrids, Syzygioblanes A-C, Found in an Indonesian Traditional Medicine, "Jampu Salo" (Syzygium oblanceolatum).

A plant used in an Indonesian traditional herbal medicine as a diabetes treatment and known locally as "Jampu Salo" was collected on Sulawesi Island, Indonesia. It was identified as Syzygium oblanceolatum (C. B. Rob.) Merr. (Myrtaceae) and found for the first time in Sulawesi; it was previously reported only in the eastern Philippines and Borneo. A phytochemical study of S. oblanceolatum led to the isolation of three unprecedented meroterpenoids, syzygioblanes A-C (1-3, respectively). These compounds might be biosynthesized through [4+2] cycloaddition of various germacrane-based cyclic sesquiterpenoids with the flavone desmethoxymatteucinol to form a spiro skeleton. The unique and complex structures were elucidated by microcrystal electron diffraction analysis in addition to general analytical techniques such as high-resolution mass spectrometry, various nuclear magnetic resonance methods, and infrared spectroscopy. Synchrotron X-ray diffraction and calculations of electronic circular dichroism spectra helped to determine the absolute configurations. The newly isolated compounds exhibited collateral sensitivity to more strongly inhibit the growth of a multidrug resistant tumor cell line compared to a chemosensitive tumor cell line.

Preparation of Single-Helical Curdlan Hydrogel and Its Activation with Coagulation Factor G.

β-1,3-glucans are a kind of natural polysaccharide with immunomodulatory, antitumor, and anti-inflammatory properties. Curdlan, as the simplest linear β-1,3-glucan, possesses a variety of biological activities and thermogelation properties. However, due to the complexity and variability of the conformations of curdlan, the exact structure-activity relationship remains unclear. We prepare a chemically crosslinked curdlan hydrogel with the unique single-helical skeleton (named S gel) in 0.4 wt% NaOH at 40 °C, confirmed by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). X-ray diffractometry (XRD) data show that S gel maintains the single-helical crystal structure, and the degree of crystallinity of the S gel is ~24%, which is slightly lower than that of the raw powder (~31%). Scanning electron microscopy (SEM) reveals that S gel has a continuous network structure, with large pores measuring 50-200 μm, which is consistent with its high swelling property. Using the 13C high-resolution magic angle spinning nuclear magnetic resonance (HRMAS NMR) method, we determine that most of the single-helical skeleton carbon signals in the swollen S gel are visible, suggesting that the single-helical skeleton of S gel exhibits fascinating mobility at room temperature. Finally, we reveal that the binding of S gel to coagulation Factor G from tachypleus amebocyte lysate increases and saturates at 20 μL tachypleus amebocyte lysate per mg of S gel. Our prepared S gel can avoid the transformation of curdlan conformations and retain the bioactivity of binding to coagulation Factor G, making it a valuable material for use in the food industry and the pharmaceutical field. This work deepens the understanding of the relationship between the single-helical structure and the activity of curdlan, promoting the development and application of β-1,3-glucans.

Estimation of unfrozen water content of saturated sandstones using nuclear magnetic resonance, mercury intrusion porosimetry, and ultrasonic tests

The unfrozen water content (UWC) is a crucial parameter that affects the strength and thermal properties of rocks in relation to engineering construction and geological disasters in cold regions. In this study, three different methods were employed to test and estimate the UWC of saturated sandstones, including nuclear magnetic resonance (NMR), mercury intrusion porosimetry (MIP), and ultrasonic methods. The NMR method enabled the direct measurement of the UWC of sandstones using the free induction decay (FID). The MIP method was used to analyze the pore structures of sandstones, with the UWC subsequently calculated based on pore ice crystallization. Therefore, the MIP test constituted an indirect measurement method. Furthermore, a correlation was established between the P-wave velocity and the UWC of these sandstones based on the mixture theory, which could be employed to estimate the UWC as an empirical method. All methods demonstrated that the UWC initially exhibited a rapid decrease from 0 °C to –5 °C and then generally became constant beyond –20 °C. However, these test methods had different characteristics. The NMR method was used to directly and accurately calculate the UWC in the laboratory. However, the cost and complexity of NMR equipment have precluded its use in the field. The UWC can be effectively estimated by the MIP test, but the estimation accuracy is influenced by the ice crystallization process and the pore size distribution. The P-wave velocity has been demonstrated to be a straightforward and practical empirical parameter and was utilized to estimate the UWC based on the mixture theory. This method may be more suitable in the field. All methods confirmed the existence of a hysteresis phenomenon in the freezing-thawing process. The average hysteresis coefficient was approximately 0.538, thus validating the Gibbs–Thomson equation. This study not only presents alternative methodologies for estimating the UWC of saturated sandstones but also contribute to our understanding of the freezing-thawing process of pore water.

Scavenging of Superoxide Radical Anion by Fluorinated Organosilicon Additives

We have explored a set of structurally related fluorinated and non-fluorinated organosilicon additives and quantified their rates of reaction with the superoxide radical anion O2 •−. using rapid-scan cyclic voltammetry. Absolute reaction rate measurements in acetonitrile solvent show that O2 •− reacts with the fluorinated OS compounds with bimolecular rate constants k BM more than 1000x larger than k BM for the reaction between O2 •− and ethylene carbonate. We further identified the products of reaction of a model OS compound using multiple nuclear magnetic resonance (NMR) methods and with gas chromatography/mass spectroscopy. Chemical analysis measurements show that addition of potassium superoxide KO2 to a model fluorinated OS compound produces only one product. Our results indicate that that OS compounds improve battery performance by rapidly scavenging O2 •− in a way that produces a stable product and reduces or eliminates the competing chemical pathways associated with carbonate breakdown. These results provide new insights into how chemical structure impacts critical chemical reactions and may guide the design of new additives that further improve battery safety and stability.

Radio frequency pulse marking of nuclear magnetization for magnetic flow metering: The impact of the flow profile

This study explores how magnetization manipulation occurs in a flowing medium over a pipe geometry using nuclear magnetic resonance methods. In particular, the experimental conditions on radio frequency pulsing and the signal detection are studied in an ultra-low frequency regime of a few kilohertz. An analytical model of the magnetization preparation is presented, which calculates the magnetization distribution of an excited flowing segment. The effective flip angle distribution is mapped to simulate the temporal development of the magnetization in the segment. The simulation results are compared to the experimental data from a flow metering setup. As a result, the quantitative impact of the flow profile on the magnetic signal is shown.

Rapid simulation of two-dimensional spectra with correlated anisotropic dimensions.

A new algorithm has been developed to simulate two-dimensional (2D) spectra with correlated anisotropic frequencies faster and more accurately than previous methods. The technique uses finite-element numerical integration on the sphere and an interpolation scheme based on the Alderman-Solum-Grant algorithm. This method is particularly useful for numerical calculations of joint probability distribution functions involving quantities with a parametric orientation dependence. The technique's efficiency also allows for practical least-squares fitting of experimental 2D solid-state nuclear magnetic resonance (NMR) datasets. The simulation method is illustrated for select 2D NMR methods, and a least-squares analysis is demonstrated in the extraction of paramagnetic shift and quadrupolar coupling tensors and their relative orientation from the experimental shifting-d echo 2H NMR spectrum of a NiCl2 · 2D2O salt.

Influence of Reservoir Microstructure on the State of Residual Oil According to Nuclear Magnetic Resonance (NMR) Spectroscopy

The influence of core properties on the state of residual oil in the process of oil displacement by water at the micro level is investigated. The pore size distribution, core permeability, dynamics and morphology of residual oil were studied. The analysis of the available experimental approaches to the study of the properties of the core and residual oil in the core samples showed that the existing methods do not provide complete information about the studied parameters. To solve these problems, it is proposed to use a combination of innovative relaxation-diffusion spectroscopy technology of nuclear magnetic resonance with traditional technology. A combination of mercury injection and nuclear magnetic resonance is used to measure the pore size distribution. The core permeability was determined using the nuclear magnetic resonance method. Two-dimensional nuclear magnetic resonance spectroscopy makes it possible to study the microscopic state of residual oil in an undisturbed core during the displacement process. With the help of the proposed methodology, a core study of the Shengli deposit in China was carried out. Pore size distributions were obtained, permeability and residual oil saturation at different stages of displacement were studied. Four types of residual oil are distinguished: strip-shaped (island), film, mesh, continuous. The influence of permeability on the fraction content of different types of residual oil in the process of displacement is shown. The research results demonstrate the influence of the pore space structure and wettability on the state of residual oil.

Ultrahigh Bifunctional Photocatalytic CO2 Reduction and H2 Evolution by Synergistic Interaction of Heteroatomic Pt-Ru Dimerization Sites.

Diatomic-site catalysts (DASCs) inherit the excellent performance of single-atom catalysts (SACs) by utilizing two adjacent atomic metal species to achieve functional complementarity and synergistic effects that improve the carbon dioxide reduction reaction (CO2RR) and H2 evolution reaction (HER) kinetics. Herein, we report a method to further improve the catalytic efficiency of Pt by using Pt and Ru single atoms randomly anchored on a g-C3N4 surface, yielding partial Pt-Ru dimers. The synthesized catalyst exhibits extraordinary photocatalytic activity and stability in both the CO2RR and HER processes. In-depth experimentation, the pH-dependent chemical exchange saturation transfer (CEST) imaging nuclear magnetic resonance (NMR) method, and theoretical analyses reveal that the excellent performance is attributed to orbital coupling between the Pt atoms and the neighboring Ru atoms (mainly dxy and dxz), which decreases the orbital energy levels and weakens the bond strength with intermediates, resulting in improved CO2RR and HER performance. This study successfully applies the pH-dependent CEST imaging NMR method to catalytic reactions, and CO2 adsorption is directly observed using CEST 2D imaging maps. This work presents significant potential for a variety of catalytic reaction applications by systematically designing bimetallic dimers with higher activity and stability.

Physicochemical and structural evaluation of natural products as a potential source for viral disease treatment

This research article aims to investigate six selected medicinal plants of Achillea millefolium (Yarrow), Alkanet, Rumex patientia (Patience dock), Dill, Tarragon, and Sweet fennel including some principal chemical compounds of achillin, alkannin, cuminaldehyde, dillapiole, estragole and fenchone. The definitive roles of these medicinal plants in Omicron treatment have been investigated through quantum mechanics and molecular mechanic methods. However, given the unprecedented challenges faced should be given a fair amount of consideration for contribution during this pandemic. In this work, it has been investigated the compounds of achillin, alkannin, cuminaldehyde, dillapiole, estragole and fenchone as a probable anti pandemic Omicron receptor derived from medicinal plants. Anti-Omicron drugs through the hydrogen bonding through physico-chemical properties of medicinal ingredients bound to the database amino acids fragment of Tyr-Met-His as the selective zone of the Omicron have been estimated with infrared (IR) and nuclear magnetic resonance (NMR) methods. A comparison of these structures has provided new insights for the design of substrate-based anti-targeting Omicron. Finally, five medicinal ingredients of achillin, alkannin, cuminaldehyde, dillapiole, and estragole bound to TMH have conducted to a Monte Carlo (MC) simulation for evaluating the absorbance of these inhibitor-active site complexes. Here, we used the network pharmacology, metabolite analysis, and molecular simulation to figure out the biochemical basis of the health-raising influence of medicinal plants. This research article peruses the drug ability, metabolites and potential interaction of some medicinal plants with Coronavirus-induced pathogenesis.

A Facile NMR Method for Pre-MRI Evaluation of Trigger-Responsive T1 Contrast Enhancement.

There is a growing interest in developing paramagnetic nanoparticles as responsive magnetic resonance imaging (MRI) contrast agents, which feature switchable T1 image contrast of water protons upon biochemical cues for better discerning diseases. However, performing an MRI is pragmatically limited by its cost and availability. Hence, a facile, routine method for measuring the T1 contrast is highly desired in early-stage development. This work presents a single-point inversion recovery (IR) nuclear magnetic resonance (NMR) method that can rapidly evaluate T1 contrast change by employing a single, optimized IR pulse sequence that minimizes water signal for "off-state" nanoparticles and allows for sensitively measuring the signal change with "switch-on" T1 contrast. Using peptide-induced liposomal gadopentetic acid (Gd3+ -DTPA) release and redox-sensitive manganese oxide (MnO2 ) nanoparticles as a demonstration of generality, this method successfully evaluates the T1 shortening of water protons caused by liposomal Gd3+ -DTPA release and Mn2+ formation from MnO2 reduction. Furthermore, the NMR measurement is highly correlated to T1 -weighted MRI scans, suggesting its feasibility to predict the MRI results at the same field strength. This NMR method can be a low-cost, time-saving alternative for pre-MRI evaluation for a diversity of responsive T1 contrast systems.

Predicting the Electrical Conductivity of Partially Saturated Frozen Porous Media, a Fractal Model for Wide Ranges of Temperature and Salinity

AbstractThe quantitative determination of liquid water content and salinity in soils is crucial for the preservation of hydrological environments and engineering infrastructures, especially in frozen regions. Electrical conductivity, as a fundamental physical parameter in electrical and electromagnetic non‐destructive techniques, varies significantly with the physical and chemical properties, such as pore water conductivity, salinity, water saturation, and temperature. In this study, accounting for pore size and tortuous length following fractal distributions, we develop a new capillary bundle model for variation of electrical conductivity as a function of temperature in broad water saturation and salinity ranges. In this new model, we consider the contributions of bulk and surface conductivities to the total electrical conductivity. To test this model, a series of laboratory experiments were carried out for different initial water saturations and salinities using an electrical resistance apparatus and a nuclear magnetic resonance method. The experimental results show that unfrozen water saturation and ionic concentration affect the electrical conductivity of unsaturated frozen soils. Furthermore, the proposed model is capable of fitting the main trends of the experimental data from the literature and acquired in this study in unfrozen‐frozen conditions for different water contents. Relying on the proposed model, we also determine the expression of the apparent formation factor, which is significantly sensitive to porosity, water saturation, and temperature. The predicted values of the apparent formation factor also agree very well with the experimental data. This new capillary bundle model provides a new perspective in interpreting electrical monitoring to easily deduce changes in key variables in the cryosphere such as liquid water content and moisture gradients.

A review of 17O isotopic labeling techniques for solid-state NMR structural studies of metal oxides in lithium-ion batteries

Recent advances in utilizing 17O isotopic labeling methods for solid-state nuclear magnetic resonance (NMR) investigations of metal oxides for lithium-ion batteries have yielded extensive insights into their structural and dynamic details. Herein, we commence with a brief introduction to recent research on lithium-ion battery oxide materials studied using 17O solid-state NMR spectroscopy. Then we delve into a review of 17O isotopic labeling methods for tagging oxygen sites in both the bulk and surfaces of metal oxides. At last, the unresolved problems and the future research directions for advancing the 17O labeling technique are discussed.

Features of a Low-Temperature Charge Density Wave in the Monoclinic Phase of NbS3 Manifested in the NMR and in Transport Properties

The relaxation of the transverse nuclear magnetization in the monoclinic phase of NbS3 has been studied by the 93Nb nuclear magnetic resonance method near the temperature TP2 = 150 K, at which a low-temperature charge density wave is formed. It has been shown that the critical slowing down of one of the vibrational modes of the lattice, which is quite slow even above TP2, occurs slightly below TP2. The transition at TP2 occurs not only in low-resistance samples, as thought previously, but also in high-resistance ones, and involves Nb atoms in the bulk of a sample. The transport properties of high-resistance samples, namely, the smearing of the depinning threshold for the charge density wave below TP2, confirm that the phase transition in them occurs at TP2. It has been concluded that the distortion of the lattice at TP2 is not due to the Peierls mechanism and can be attributed to the Keldysh–Kopaev transition. Another possible mechanism is the fluctuation distortion of the lattice above TP2 that prevents the sliding of the charge density wave.

Selective Detection of Intermediate-Amplitude Motion by Solid-State NMR.

The coexistence of rigid and mobile molecules or molecular segments abounds in biomolecular assemblies. Examples include the carbohydrate-rich cell walls of plants and intrinsically disordered proteins that contain rigid β-sheet cores. In solid-state nuclear magnetic resonance (NMR) spectroscopy, dipolar polarization transfer experiments are well suited for detecting rigid components, whereas scalar-coupling experiments are well suited for detecting highly mobile components. However, few NMR methods are available to detect the segments that undergo intermediate-amplitude fast motion. Here, we introduce two NMR experiments, a two-dimensional T2H-filtered CP-hCH correlation and a three-dimensional J-INADEQUATE CCH correlation, to observe this intermediate-amplitude motion. Both experiments involve 1H detection under fast magic-angle spinning (MAS). By combining 1H transverse relaxation (T2H) filters with dipolar polarization transfer, we suppress the signals of both highly rigid and highly mobile species, thus revealing the signals of intermediate mobile species. 1H detection under fast MAS is crucial for distinguishing the different motional amplitudes. We demonstrate these techniques on several plant cell wall samples and show that they allow the selective detection and resolution of certain hemicellulose and pectin signals, which are usually masked by the signals of the rigid cellulose and the highly dynamic pectins in purely dipolar and scalar NMR spectra.

The setting and hardening of geopolymer concrete based on low-field nuclear magnetic resonance and cyclic voltammetry methods

The hydration process has an important influence on the various properties of geopolymer concrete. However, current testing methods for hydration degree are complex and inconvenient, which limits the wide application of geopolymer concrete. For this reason, this study innovatively proposes new methods for non-destructive characterisation of the hydration degree based on low-field nuclear magnetic resonance and cyclic voltammetry techniques. Meanwhile, the setting and hardening characteristics of red mud-coal metakaolin geopolymer concrete with water-binder (W/B) ratios of 0.50, 0.55, 0.60 and 0.65, respectively, was systematically and comprehensively evaluated. The reaction mechanism of geopolymer concrete was revealed using a variety of testing methods such as SEM-EDS, thermogravimetric, and heat of hydration. The results show that the degree of hydration is significantly correlated with the intensity-weighted relaxation time and specific capacitance value, which can be expressed by pertinent equations. In addition, it is found that the hydration process of geopolymer concrete is divided into different stages, forming two gel phases, C-A-S-H and N-A-S-H. Increasing the W/B ratio promotes the generation of C-A-S-H gels but severely hinders the generation of N-A-S-H gels, overall adversely affecting the hydration process. This work will facilitate non-destructive monitoring of the status of geopolymer concrete during actual projects to ensure construction safety.

Studies of the Physical Structure of Cured Epoxy Resin Composite Modified with Silicon-Containing Additives

Abstract The possibility of regulating the structure and reducing its defectiveness opens great possibilities for controlling the properties of epoxy composite materials. This article reports the results of investigation by X-ray scattering and nuclear magnetic resonance methods and the microstructural changes that occur when silicon-containing additives such as polydimethyl siloxane (PDMS-5) and pyrogenic silica (HDK) are introduced into epoxy resin ED-20. The mechanism of formation of the structure of epoxy binder ED-20 with L-20 curing agent in the presence of complex additives is found. The modifying additive (PDMS-5 + HDK) is located in the epoxy binder because of the chemical interaction of functional polar groups and the developed surface. The additives increase the mobility of the reaction mixture and also facilitate and regulate the spatial orientation of macromolecules during polymerization. This contributes to the formation of a more regular and less defective spatial structure. The epoxy binder is a heterogeneous two-component system, one of which corresponds to a pseudo-crystalline region in which the movement of molecules is suppressed, and the second is found at lower volume fractions and is amorphous. The only maximum in the wide-angle X-ray diffraction pattern of the binder without additives is attributable to the distribution of molecular chains in the para-crystalline lattice. The addition of the HDK additive leads to ordering of the supramolecular structure, in which linear clusters consisting of 5–7 spheres appear. The average size of the spheres is from 8 to 26 nm. The addition of additives in the samples leads to the formation of a more regular and less defective spatial structure because of the interaction of functional polar groups and the surface, which regulate the spatial orientation of macromolecules during polymerization.