This preliminary study introduces the incorporation and chemical stabilization of sulfur waste into geopolymers matrix and explores the concept of material production for further environmental and engineering solutions. Geopolymers were synthesized by dissolving sulfur in the alkaline activator of sodium hydroxide and sodium silicate in different proportions. The Alkaline solution was then mixed with metakaolin to synthesize the geopolymer matrix. Adding sulfur from 0 wt.% to 5 wt.%, compared with metakaolin, was found to lead to an increase in the compressive strength of the geopolymer from 22.5 MPa to 29.9MPa. When sulfur is between 5 wt.% and 15 wt.%, a decrease in compressive strength was observed to 15.7 MPa, which can be explained by defects and voids in the geopolymer microstructure through the solubility of excess sulfur and thus the formation of defects and voids in the geopolymer microstructure. Because of the incorporation of sulfur into the geo-polymer, a compact and dense microstructure is formed as reported in the SEM analysis. XRD analysis shows that besides quartz and Analcime, a new phase, Al2·H10·O17·S3, is also formed as a result of sulfur dissolution in alkaline activator of geopolymer.

In this work a new method is proposed to tackle down the multiple objective optimization problem of the calculation of cation distribution in spinels structure, through the difference of intensity ratios between experimental and calculated intensities of cation sensitive Bragg planes, by introducing a new factor, Rabs, in Bertaut method. This factor is introduced as the sum of absolute R factors, and it is minimized by varying cation distribution. To test this method aluminate manganese spinel where synthesized though modified Pechini method and characterized though XRD. The results show to be in agreement with literature for the aluminum inversion in tetrahedral sites, which is near to the reported value of 10%. Also, it was noticed that the manganese atoms are present in octahedral sites with a mixed valence state of +2 and +3. Which might be an indicator that oxygen vacancies are present in the structure, so the vacancies value of oxygen is proposed considering the total charge of cations and thus proposing the value of 3.678 mol per formula unit of the spinel, thus having the next stoichiometry considering normalized Al and Mn, MnAl2O3.678. Finally, the last cation distribution proposed was [Mn0.867^(+2) Al0.129^(+3) ][Mn0.034^(+2) Mn0.098^(+3) Al1.871^(+3) ] O3.678 with a Rabs factor value of 0.6466, which considers the cation distribution and oxygen vacancies.

In this contribution we present work on rapid thermal annealing of as-electrodeposited thin films of Cu2ZnSnS4. The treatment was carried out in cold wall tubular reactor in dynamic conditions with variations of temperature, speed and time of the specific elements of the process. The effect of annealing was investigated by X-ray diffractometry, Raman scattering and Scanning Electron Microscopy (SEM). The phase composition of the films in dependence on conditions of treatment was analysed and have been shown that in slow and prolonged high-temperature process the low temperature binaries react completely and only Kesterite and ZnS is left. In addition, structural investigations by XRD have shown gradual decrease of crystallite sizes when the temperature level and duration of the high-temperature segment increases and respectively increase in the strain, due to formation of the phases in non-equilibrium conditions. In opposite, when the speed of dynamic segments in the process decreases the both crystallite size and strain of the Kesterite decreases non-monotonically. The grain sizes of Kesterite, presented by SEM investigations, have shown increase when the temperature and the duration increase, respectively the speed decreases with exemption at higher temperature near 750 C. The set of experiments gave idea by scrupulous analysis of Raman data to elucidate the track for fine manipulating of the defects in the structure of CZTS thin films having in mind the dependences of the ratios of Q = I287/I303 and Q’= I338/(I366+I374) on the process variables.

Four new unusual pentacyclic triterpenoids (1-4) were isolated from the roots of Jasminum sambac (L.) Ait. Their structures were elucidated by 1D and 2D NMR analysis, single crystal X-ray diffraction and HRESIMS.

In the present work, doped ZnO (ZnO:Al) thin film has been grown on Silicon (Si) substrate by DC sputtering. The obtained thickness of the film is 230 ± 5 nm. The films were subjected to swift heavy ion (SHI) irradiation 120 MeV, Ag⁹⁺ with different fluences ranging from 3 × 10¹¹ to 3 × 10¹³ ions/cm². To study the impact of SHI, both pristine and irradiated samples were characterized to obtain the structural, surface morphological and electrical properties using X-ray diffractometry (XRD), atomic force microscopy (AFM) and hall effect measurement system respectively. From XRD results it is observed that there is change in crystallinity of the film with increase in irradiation fluence. The surface morphological studies through AFM shows the increase in surface roughness with increase in fluence. A significant change is also observed in electrical parameters viz conductivity, mobility and carrier concentration. Conductivity, mobility and carrier concentration decreases with increasing fluence.

Carburizing of stainless steels at low temperatures (below 500°C) develops a high content carbon layer, known for its high hardness. X-ray Diffraction investigation indicates that carburization treatment does not impact the structure of substrate; however, introduced carbon causes expansion in the carburized layer through the increase in d-spacing. Characterization of carbon concentration and hardness profiles indicate that carbon content gradually decreases while moving further into the substrate; and the origin of the increased hardness of the expanded layer arises from the super-saturated carbon content, following the solid solution strengthening theory. An area that is not well understood is in regard to the carburized layer’s relation to the substrate and the significance in their differences. Using two grades of stainless steel, AISI 316L and PH 17-4, it was observed that the carburized layer is not a separate layer, but a higher carbon content version of the substrate,

The thermal degradation behaviour of 10:90 and 90:10 blends of Polyethylene Terephthalate (PET) and petroleum coke has been investigated using mechanical alloying (milling) at 300 rpm and for periods up to 1-10 hours. Milled specimens were characterised using SEM and x-ray diffraction; their thermal degradation behaviour was investigated using thermo-gravimetric analyser (TGA) for temperatures up to 1200°C. Whereas PET specimens showed a tendency towards flattening out and increased surface area during collisions in ball mills, petroleum coke particles tended to break down into smaller particles. 10:90 and 90:10 blends of PET and coke showed significant microstructural evolution with increasing speeds and time including fracture, strain hardening and re-welding. X-ray diffraction results showed clear evidence for increasing amorphous component in petroleum coke without much influence on PET crystallinity. Thermo-gravimetric results showed a significant increase in the overall degradation and much higher weight losses associated with mechanical alloying. This study has shown that mechanical alloying could be used to modify the degradation behaviour of coke/plastic blends and corresponding yield during pyrolysis with implications for plastic waste management.

This investigation mainly focused on the microstructural analysis of Al based hybrid metal matrix composites. Aluminium as base metal and reinforced with 2% B4 C, ZrO2 (2%,4%,6%), SiC (4%,8%,12%). Specimens were manufactured by using conventional stir casting technique. Hybrid metal matrix composites were examined by using Scanning electron microscope. This research explained XRD, EDS and Fractography analysis. This investigation shows the reinforced material has given better results in all aspects than pure Al6061 alloy and homogeneous dispersion of particles inside the matrix. Porosity, delamination, cracks, particle distributions were observed through microstructural analysis. Additionally determined the crystal size of pure Aluminium 6061 alloy and hybrid composites.

In this study, changes in the microstructure of coal tar pitch during successive processes, including pyrolysis, polycondensation, and crystallization, were examined in connection with the resulting variations in structure factors, as measured by XRD analysis, and functional groups, as confirmed by FTIR spectroscopy. To this end, four zones were defined based on variations in crystallinity, which were indicated by d002 and Lc. Each zone was further characterized by interpreting crystallinity development in relation to changes in functional groups and specimen height. At around 400 °C, polycondensation occurred as the C-Har and C-Hal peaks decreased in intensity. These peak reductions coincided with the formation of mesophase spheres, resulting in enhanced crystallinity. Subsequently, at around 500 °C, the peak intensity of C-H and COOH decreased, which was attributed to the release of large amounts of gasses. This led to sharp volume changes and a temporary reduction in crystallinity. All these results suggest that changes in the functional groups of coal tar pitch at lower temperatures (600 °C or less) during the carbonization process are closely associated with variations in its crystallinity. The major findings of the present study provide valuable insights for designing highly effective processes in the manufacturing of synthetic graphite blocks using CTP as a binder material, including by selecting appropriate temperature ranges to minimize volume expansion and crystallinity degradation and determining the lowest possible carbonization temperature to ensure adequate binder strength.

The suspension cross-linking technique has been utilized to create the magnetic chitosan nanoparticles, which were then applied to the magnetic carrier method at 80°C. First the FeCl2 and FeCl3 solution co-precipitated and synthesized Fe3O4 for utilization in the formation of magnetic chitosan nanoparticles, it has been characterized by utilizing DLS (Dynamic light scattering), XRD (X-ray diffraction spectrometer), FTIR (Fourier transform infrared spectroscopy), which identified structure, size, FE-SEM (Field Emission Scanning Electron Microscope) and HR-TEM (High-resolution transmission electron microscopy) which identified structure and particle size whereas magnetic behavior of chitosan nanoparticles was determined by VSM (Vibrating sample magnetometer). According to the results collected, the magnetic chitosan nanoparticles have been spherical in form and size ranging from around 250 to 400 nm.

Asphaltenes constitute a heavy fraction of fossil fuels and their characterization is still a very difficult and challenging issue due to their complex and variable composition. Asphaltene components are highly condensed aromatic molecules having some heteroatom and aliphatic functionalities. Their molecular weights distribution span a wide range, from hundreds to millions of units, in dependence on the diagnostic used, leading to speculation about possible occurrence of self-aggregation. In the present work, mass spectrometry, with properly developed mathematical methods, size ex-clusion chromatography and X-ray diffraction analysis have been applied to asphaltenes for giving some further insight on their MW distribution and characteristics. The results here reported give further quantitative support to the experimental data interpretation already reported in previous works.

The carbon-carbon cross-coupling of phenyl s-tetrazine (Tz) units at their ortho-phenyl positions allows to form constrained bis(tetrazines) with original tweezer structures. In these compounds, the face-to-face positioning of the central tetrazine cores is endorsed by pi-staking of the electron-poor nitrogen-containing heteroaromatic moieties. The resulting tetra-aromatic structure can be used as a weak coordinating ligand with cationic silver. This coordination generates a set of bis(tetrazine)‐silver(I) coordination complexes tolerating a large variety of counter anions of various geometries, namely, PF6–, BF4–, SbF6–, ClO4–, NTf2–, OTf2–. These compounds were characterized in the solid-state by single crystal XRD and reflectance spectra, and in solution by 1H NMR, mass spectrometry, electroanalysis and UV-visible absorption spectroscopy. The X-ray diffraction (XRD) structure of complexes {[Ag(3)][PF6]}∞ (4) and {[Ag(3)][SbF6]∞ (6), where 3 is 3,3'-[(1,1'-biphenyl)-2,2'-diyl]-6,6'-bis[phenyl]-1,2,4,5-tetrazine, revealed the formation of 1D polymeric chains, characterized by an evolution to a large opening of the original tweezer and a coordination of silver(I) via two chelating nitrogen atom and some C=C pi-interactions. Electrochemical and UV spectroscopic properties of the original tweezer and of the corresponding silver complex are reported and compared. 1H NMR titrations with AgNTf2 allowed to determine the stoichiometry, and apparent stability of two solution species, namely [Ag(3)]+ and [Ag(3)2]2+, that formed in CDCl3/CD3OD 2:1 v/v mixtures.

This study deals with vibrational and crystallographic aspects of the thermally induced transformation of serpentine-like garnierite into quartz, forsterite, and enstatite occurring at about 620 °C. Powder specimens of garnierite have been annealed in static air between room temperature and 1000 °C. The resulting products from the transformations detected based on thermogravimetric and differential thermal analysis, have been extensively characterized via microRaman spectroscopy, and X-ray diffraction. Our study shows that serpentine-like garnierite consists of a mixture of different mineral species. Furthermore, these garnierites and their composition can provide details based on the mineralogy and the crystalline phases resulting from the thermal treatment.

Graphene-oxide (G) was prepared by the Hummers’ method. A G-COOH layer was synthesised using chloroacetic acid and G. To fabricate carboxylated graphene-RuO2 (G-COORu) nano¬¬-composites, RuO2 nano particles were grown on graphene layers using a one-step thermal method, -COOH(G-COOH), and RuCl3. All materials were characterised using X-ray diffraction, transmission electron microscopy, scanning electron microscopy, 13C-nuclear magnetic resonance as well as X-ray photoelectron, Fourier-transform infrared spectroscopy, and Raman. The electrochemical characteristics of the G-COORu supercapacitors were analysed using electrochemical impedance spectroscopy, cyclic voltammetry, constant current charge–discharge tests, and Nyquist impedance plots. The supercapacitors exhibit a specific capacitance of ~125 F g-1 at 100 mA cm-2 within the potential range of 0–1.0 V. The method used here provides a simple approach for the deposition of RuO2 nano particles on graphene layers and can be widened to the fabrication of other classes of hybrids based on G layers for specific technical applications.

Although various atmospheric corrosion simulation models have been developed that give good results, industrial environments are still challenging. This paper aims to investigate the effect industrial atmospheres in Bor on the mechanical properties of structural steel S235JR and to create a constitutive model and also laboratory experimental conditions that will give the best results as an accelerated corrosion test. Atmospheric corrosion tests lasted six months, using sites close to the Electrolytic Refining Plant and Sulphuric Acid Plant, as well as air quality monitoring stations at a remote location in the city of Bor. The laboratory experiments included a salt chamber test lasting 120 h and 240 h and immersing the specimen in the electrolyte from the Electrolytic Refining Plant for 30 days. The results were compared with the standard specimens stored in the laboratory. The X-ray diffraction (XRD) method was used to identify the composition of corrosion products. The scanning electron microscopy (SEM) analysis was applied to analyze the fracture surfaces of the specimens. The use of the Complete Gurson Model (CGM) described the tensile characteristics of the corroded specimens. The study has shown that an enhanced acceleration model and conditions could be developed using numerical analysis of the test results.

The reactivity of 3,5-di-(pyridin-4-yl)-1,2,4-thiadiazole (L1) with 1,4-diiodotetrafluorobenzene (1,4-DITFB) was explored and the halogen-bonded 1:1 co-crystal (1) was successfully isolated and structurally characterized.

Alkali-Silica Reaction (ASR), which develops over time into a harmful internal reaction in concrete, produces a harmful gel due to the reaction between the reactive silica in the aggregate and the alkalis of the pore solution. Due to the multi-scale nature of this long-term phenomenon, understanding its mechanism in concrete structures remains difficult to assess. Accelerated Mortar Bar Testing (AMBT) ASTM C1260 is among the commonly used methods to understand ASR formation in a short time. In this study, the chemical characterisation of concretes produced from volcanic rock type basalt aggregate was compared with the chemical characterisation of ASR concretes after AMBT was applied. In addition, 20% FA was substituted into the concrete to investigate the effect of fly ash (FA) on ASR. Specimens with limestone aggregate (PL), basalt aggregate (BBC) and 20% basalt aggregate with fly ash substitution instead of cement (BBC20FA) were prepared for the investigation. Scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA) techniques were used to characterise the morphology and analytical composition of the concretes. It was determined that basalt aggregate does not cause ASR and its use with fly ash increases the strength and durability of concrete.

The reaction of pyridinium chlorochromate with furan to give enedione derivatives cannot be performed by using commercial PCC. Homemade and commercial PCC had different color and showed some differences in the XRD spectrum. XPS showed the presence of relevant amount of Cr(III) in the homemade reagent. DFT calculations showed that Cr(III) impurities in the reagent can catalyze the reaction with furan derivatives, if oxygen atom in the Cr(III) derivative attacks the furan ring, while it is reoxidized by PCC, through a migration of a chlorine atom.

Purpose Professional oral hygiene procedures are recommended by dentists, twice a year. BioHPP is a polyetheretherketone polymer used in prosthetic dentistry as a frame material. The aim was to investigate whether routine dental cleaning procedures such as ultrasonic scaling and brushing affect the surface proprieties of prosthetic BioHPP restorations. To evaluate the surface properties of different restorations based on BioHPP (veneered with composite resin and polished) after brushing and ultrasonic scaling exposure. Materials and Methods The 66 BioHPP specimens were divided into three groups (n=22). The first group was the control group, and no further treatment was applied. The specimens in the second group were veneered with composite resin and in the third group the specimens were veneered with composite resin and polished. Each group of samples was divided into 3 subgroups: 0- no treatment, 1-exposed to tooth brushing, 2-exposed to ultrasonic scaling. The surface morphology was investigated by atomic force microscopy (AFM). The structure of samples was analysed using the XRD technique, and the surface wettability was done. Results Control group specimens were significantly rougher compared to other groups (p ≤ 0.05). There was no statistically significant difference in the contact angle of water analyses between the samples. Conclusion: Composite veneered BioHPP showed the highest surface resistance to brushing and ultrasonic scaling.

2,7-bis(pyridin-4-ylethynyl)-9H-carbazole (1) was synthesized by reacting 4-ethynylpyridine hydrochloride with 2,7-dibromo-9H-carbazole. The full characterization of compound 1 is presented, and the crystal structure of its monohydrate co-crystal was determined by single-crystal XRD analysis.

ZnO has many technological applications which largely depend on its properties that can be tuned by controlled synthesis. Ideally, the most convenient ZnO synthesis is carried out at room temperature in aqueous solvent. However, the correct temperature values are often loosely defined. In the current paper we performed synthesis of ZnO in aqueous solvent, by varying reaction and drying temperature by 10°C steps and monitored the synthesis products primarily by XRD. We found out that a simple direct synthesis of ZnO, without additional surfactant, pumping of freezing, required both a reaction (TP) and a drying (TD) temperature of 40°C. Higher temperatures also afford ZnO, but lowering any of the TP or TD below the threshold value results either in the achievement of Zn(OH)2 or in a mixture of Zn(OH)2/ZnO. A more detailed Rietveld analysis of the ZnO samples reveals a density variation with the synthesis temperature and an increase of the nanoparticles average size also verified by SEM images. The optical properties of ZnO obtained by UV-Vis reflectance spectroscopy indicate a red shift of the band gap by ~0.1 eV.

We present a cost- and time-efficient method for the controlled preparation of single phase La(IO3)3 nanoparticles via a simple soft-chemical route which takes a matter of hours, thereby providing an alternative to the common hydrothermal method which takes days. Nanoparticles of pure α-La(IO3)3 and pure δ-La(IO3)3 were synthesised via the new method depending on the source of iodate ions, thereby demonstrating the versatility of the synthesis route. The crystal structure, nanoparticle size-dispersal and chemical composition were characterised via angle- and energy-dispersive powder X-ray diffraction, scanning electron microscopy and Fourier-transform infrared spectroscopy.

The ceramic sherds from approximately 20 samples of lead-glazed tableware, recovered from diverse archaeological sites, including three repurposed storage pits transformed into dumpsters within the medieval city of Santarém (13th-14th century), underwent a meticulous examination. This investigation utilized techniques such as micro-Raman, ground state diffuse reflectance absorption, and X-ray fluorescence spectroscopies, in addition to X-ray diffraction and stereomicroscopy. A parallel study was conducted on contemporaneous European ceramics (glazed sherds) sourced from archaeological sites dating back to the 13th-15th centuries in Saintonge (France), Ardenne, Zomergem, and Bruges (Belgium), as well as Surrey-Hampshire, Kingston, and Cheam (England). The colour of the ceramic bodies is predominantly white or whitish, with a few exhibiting a vivid red hue. Ceramic sherds with a light paste composition were likely crafted using kaolin clays as raw materials. Analyses of fabric, mineralogical, and elemental composition of the sherds suggest that the majority of Santarém's glazed ceramics were locally or regionally produced, potentially derived from a Pliocene kaolin-rich sand formation. However, this conclusion is not supported by the absence of discovered lead glaze kilns or workshops in Santarém for the late Middle Ages. A distinctive feature from the European workshop ceramics lies in the quartz temper content and fabric.

The ceramic pastes of ca. 31 samples recovered from the Almaraz archaeological site, located in the south bench of Tagus River, were studied in detail using XRF, micro-Raman and GSDR spectroscopies, as well as the XRD technique. The ceramic sherds could be grouped into six categories, Red Slip tableware, Decorated tableware, Yellow Slip tableware, Grey tableware, Common tableware and Handmade pottery. Our studies of the mineralogic composition of the sherds` body indicate that all ceramics were produced locally, using silicious clays in most cases and calcareous clays in a few ones. Micro-Raman and ground state diffuse reflectance absorption spectroscopy provided useful information regarding the materials used to produce the coloured ceramics: hematite and brookite for the red slip and decorated ceramics, jacobsite or carbon black for the black decoration or grey ceramics. For the yellow slip tableware a simple engobe rich in yellow clay was used. XRF spectroscopic studies provided the elemental composition of all samples, and biplots of the Potassium (K) versus Calcium (Ca) contents, normalized to the silicon content of each ceramic paste, clearly show that Pliocene and Miocene local clays sources were used to produce most ceramics. Only one sherd can be considered a Lisbon production.

The growing interest in Na-ion batteries as a “beyond lithium” technologies for energy storage drives the research for high-performance and environment-friendly materials. Na2Ti3O7 (NTO) as an eco-friendly, low-cost anode material shows a very low working potential of 0.3 V vs Na+/Na but suffers from poor cycling stability, which properties can be significantly influenced by materials synthesis and treatment. Thus, in this work, the influence of the calcination time on the electrochemical performance and the reaction mechanism during cycling were investigated. NTO heat-treated for 48 h at 800 °C (NTO-48h) demonstrated enhanced cycling performance in comparison to NTO heat-treated for only 8 h (NTO-8h). The pristine material was thoroughully characterized by X-ray diffraction, laser granulometry, X-ray photoelectron spectroscopy, and specific surface area measurements. The reaction mechanisms induced by sodiation/desodiation and cycling were investigated by opernado XRD. Electrochemical impedance spectroscopy was used to evidence the evolution of the solid electrolyte interface layer (SEI) and modification of charge transfer resistances as well as the influence of cycling on capacity decay. The evolution of the crystallographic structure of NTO-48h revealed a more ordered structure and lower surface contamination compared to NTO-8h. Moreover, the residual Na4Ti3O7 phase detected after the sodium extraction step in NTO-8h seems correlated to the lower electrochemical performance of NTO-8h compared to NTO-48h.

The present study illustrates the strong effect of geometrical parameters on the magneto-structural properties of Co2MnSi glass-coated microwires prepared using the Taylor-Ulitovsky method. Thus, two samples with different geometrical aspect ratios (ρ= d / D) have been fabricated, where d is the metallic nuclei diameter and D is the total diameter of the Co2MnSi microwire. The XRD analysis shows a significant change by modifying the aspect ratio, for ρ = 0.46 the main peak with miller indices (220) is recognized as an A2-type disordered cubic structure. Meanwhile, in the sample with a low aspect ratio, ρ = 0.31, the perfect L21 ordered cubic structure is attained. In addition, a decrease in average grain size from 36.62 nm to 28.07 nm by increasing the aspect ratio from 0.46 to 0.31 is observed. The magnetic characterization has been done in a wide range of temperatures and magnetic fields. Both of Co2MnSi samples show ferromagnetic behavior in a whole measuring temperatures range. A significant increase in coercivity and normalized reduced remanence by decreasing the aspect ratio is observed. The change in the magnetic properties is attributed to the modification in the microstructure, which is induced during the fabrication process. Such a dependence on the microstructure and magnetic properties on the ρ-ratio can be associated either with the internal stresses distribution and magnitude or with different quenching rates of microwires with different aspect ratios. The current findings demonstrate the tunability of microstructure and magnetic properties of Co2MnSi-glass-coated microwires simply, by a small modification in the geometric properties during the manufacturing process and without excreting any additional post-processing. The variation in geometric parameters of Co2MnSi glass-coated microwires allows us to tune magnetic properties and structure, which is essentially advantageous for sensing devices development.

In this work, some micro-samples belonging to the open-air rock art site of Cueva de la Vieja (Alpera, Albacete, Spain) were analysed. These samples were collected after and before a desalination treatment carried out with the aim of removing a whitish layer of concretion that affected the painted panel. The diagnostic study was performed to study the conservation state of the panel and then to confirm the effectiveness of treatment. Micro energy dispersive X-ray fluorescence spectrometry, Raman spectroscopy and X-ray diffraction were employed for the characterization of the degradation product as well as that of mineral substrate and pigments. The micro-samples analysis demonstrated that the painted layer was settled on a dolomitic limestone with silicon aggregates and aluminosilicates as well as iron oxides. The whitish crust was composed by sulfate compounds like gypsum (CaSO4·2H2O) with minor amount of epsomite (MgSO4.7H2O). An extensive phenomenon of biological activity was demonstrated since, in almost all the samples analysed, the presence of calcium oxalates monohydrate (CaC2O4H2O) and dehydrate (CaC2O42H2O) were found. Probably the presence of both calcium oxalates had favoured the conservation of pictographs. In addition, some carotenoids pigments, scytonemin (C36H20N2O4) and astaxanthin (C40H52O4) were characterized both by Raman spectroscopy and by X-ray diffraction. Hematite was found as a pigment voluntarily used for the painting of the panels used in mix with hydroxyapatite and amorphous carbon. The results of the analyses of the samples taken after the cleaning treatment confirmed a substantial decrease in sulphate patina on the panel surface.

In this work, we report manganese phthalocyanine (MnPc) films obtained by ultrasonic spray-pyrolysis technique at 40°C deposited on glass substrate subjected to thermal annealing at 100 °C and 120°C. The MnPc films were characterized by UV/Vis spectroscopy, Raman spectroscopy, X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The absorption spectra of the MnPc films were studied in a wavelength range from 200 to 850 nm, where the characteristic bands of a metallic phthalocyanine known as B and Q bands were observed in this range of the spectrum. The optical energy band (Eg) was calculated by the Tauc equation. It was found that for these MnPc films, the Eg has the values of 4.41, 4.46 and 3.58 eV corresponding to as deposited, annealing 100°C and 120°C, respectively. The Raman spectra of the films showed their characteristic vibrational modes of the MnPc films. In X-ray diffractograms of these films, the characteristic diffraction peaks of a metallic phthalocyanine are observed, presenting a monoclinic phase. SEM images of these films were studied in cross section obtaining thicknesses of 2, 1.2 and 0.3 μm to as deposited, annealing 100°C and 120°C, successively. Also, in the SEM images of these films, both the average particle sizes ranging from 4 to 0.041 µm and the average diameter from 4.8 to 0.091 μm were obtained. The results agree with those reported in the literature for MnPc films deposited with other techniques.

The mechanisms of formation of induced intrinsic and impurity radiative states, which consist of intrinsic and impurity electron-hole trapping centers in irradiated Ca2P2O7-Mn and Ca2P2O7 phosphates, were investigated using thermoactivation and vacuum-ultraviolet spectroscopy methods. These centers are excited at photon energies of 4.0 eV and 4.5 eV, which are within the matrix's transparency region. New radiative induced states at 3.06 eV and 2.92 eV are demonstrated to be generated upon the excitation of anions by photons with energies of 5.0 and 5.64 eV. This process is due to charge transfer from the ion to the impurities, specifically Mn^2+ O^2- Mn^2+ and the neighboring ion O^2- (P2O7)^4-. Furthermore, upon the excitation of matrix anions with photon energies exceeding the band gap (8.0 - 8.25 eV), electron trapping by impurities such as Mn^2+ and (P2O7)^4- ions results.

Abstract: In the past years, lithium-ion solid-state batteries demonstrated significant advancements regarding such properties as safety, long-term endurance, and energy density. The properties of these depend on solid-state electrolytes and especially ionic transport interfacial transport with cathode or anode materials. Solid-state electrolytes based on lithium halides offer new opportunities due to their unique features such as broad electrochemical stability window, high lithium-ion conductivity, and elasticity at close to melting point temperatures that help to improve lithium-ion transport at interfaces. A comparative study of lithium indium halide (Li3InCl6) electrolytes syn-thesized by a mechano-thermal method using different optimization parameters revealed a signif-icant effect of ball-milling time, temperature, and pressure on lithium-ion transport. Based on the Electrochemical Impedance Spectroscopy (EIS) data in the temperature range of 25-100 °C, the optimized Li3InCl6 electrolyte phase demonstrates high ionic conductivity reaching 0.98 mS cm−1 at room temperature. However, at 70 °C, phase transformation was observed leading to significant changes in the activation energy for lithium-ion transport. In-situ X-ray diffraction and in-situ/operando X-ray photoelectron spectroscopy techniques confirmed the tempera-ture-dependent behavior of Li3InCl6 synthesized. These observations provide critical information for practical applications of solid-state electrolytes and nanocomposites based on Li3InCl6 within the broad temperature range for lithium-ion solid-state batteries with improved morphology, chemical interactions, and structural integrity.

In this study, we report a detailed experimental and theoretical investigation of three glycols, namely ethane-1,2-diol, 2-methoxyethan-1-ol and 1,2-dimethoxy ethane. For the first time, the X-Ray spectra of the latter two liquids was measured at room temperature, and they were compared with the newly measured spectrum of ethane-1,2-diol. The experimental diffraction patterns were interpreted very satisfactorily with molecular dynamics calculations, and suggest that in liquid ethane-1,2-diol most molecules are found in gauche conformation, with intramolecular hydrogen bond between the two hydroxyl groups. Intramolecular H-bonds are established in the mono-alkylated diol, but the interaction is weaker. The EDXD study also evidences strong intermolecular hydrogen-bond interactions, with short O···O correlations in both systems, while longer methyl-methyl interactions are found in 1,2-dimethoxy ethane. X-Ray studies are complemented by micro Raman investigations at room temperature and at 80°C, that confirm the conformational analysis predicted by X-Ray experiments and simulations.

Ga doped ZnO thin films were formed by the Ultrasonic Chemical Spray Pyrolysis method onto substrates using zinc acetate and gallium (III) nitrate hydrate as precursors. The structural, optical, surface and electrical properties were studied as a function of increasing Ga doping concentration from 0 to 6 at %. Structural studies were shown polycrystalline with a hexagonal crystal structure. The transparency in the visible range was around 85% for thin film deposited using 6 at % Ga doping. With the aim of determining surface images and surface roughness of the films atomic force microscope images were taken. Ga doping of ZnO thin films could markedly decrease surface roughness. Electrical resistivity was determined by four point method. The resistivity 2.0% Ga doped ZnO film was the lowest resistivity of 1.7 cm. In the photoluminescence measurements of the films, existence of UV and defect emission band was observed. As a result, Ga doped ZnO films have advanced properties and promising materials for solar cells.

NDBs were fabricated from gum arabic (GA) and polyvinyl alcohol (PVA) in different ratios using novel techniques (casting, dehydration, and peeling). The GA/PVA blends were cast with a novel vibration-free horizontal flow (VFHF) technique, producing membranes free of air bubble defects with a homogenous texture, smooth surface, and constant thickness. The casting process was achieved on a self-electrostatic template (SET) made of poly-(methyl methacrylate), which made peeling the final product membranes easy due to its non-stick behavior. After settling of the cast membranous blind, sheets were dried using nanometric dehydration under a mild vacuum stream using a novel stratified nanodehydrator (SND) loaded with P2O5. After drying the TBM, the dry, smooth membranes were peeled easily without scratching defects. The physicochemical properties of the NDBs were investigated using FTIR, XRD, TGA, DTA, and AFM to ensure that the novel techniques did not distort the product quality. The NDBs retained their virgin characteristics, namely, their chemical functional groups (FTIR results), crystallinity index (XRD data), thermal stability (TGA and DTA), and ultrastructural features (surface roughness and permeability), as well as their microbial biodegradation ability. Comparing the two TBM’ s precursors, PVA had a higher crystallinity index (CI), more mass loss at higher temperatures, greater thermal stability due to higher heat resistance, and a higher clearance of surface roughness due to its large particle size (PS), as well as its higher permeability parameters, namely pore diameter (PD) and void volume (VV), than those for GA. Accordingly, increasing the PVA allocation in the bioplastic blends can enhance their properties except for mass loss, whereby increasing the GA allocation in the TBM blend reduces its mass loss at an elevated temperature. In addition, there is no statistical difference between the NDBs and ordinary air-dried NDBs in PS, PD, and VV, indicating that the novel procedures used did not distort their parent properties examined, as well as their ability for biodegradation. In comparison to control samples, the separated bacteria and fungus destroyed the NDBs. Pseudomonas spp. and Bacillus spp. were the two main strains of isolated bacteria, and Rhizobus spp. was the main fungus. The nanodehydration method gave the best solution for the prompt drying of water-based biopolymers free of manufacturing defects, with simple and easily acquired machinery required for the casting and peeling tasks, in addition to its wonderful biodegradation behavior when buried in wetted soil.

This study aimed to develop chitosan-based apigenin spray dried solid dispersion using 1:1,1:1.5,1:2 w/w ratios. The results of process yield and drug assay were found to be (87.5%, 94.2%, and 95.86%), (95.2 ±1.34%), (99.5 ±0.85%), and (97.6 ±2.42%), respectively, for AC1, AC2, and AC3. Flow properties indicate the free flow of powders. FTIR revealed compatibility among chitosan and apigenin, and DSC and XRD showed prepared solid dispersion was on a molecular level and available in amorphous. In contrast, SEM images reflect irregular block and near-spherical shape elongated particles in the selected AC2. The antimicrobial examination reflects that AC2 was more effective against Gram-positive, negative, and fungal strains. AC2 SDSDs has more anti-oxidant property compared to pure flavonoid (AGN). Anti-proliferative activity against A549 lung cancer cell lines showed better anti-cancer activity by AC2 SDSDs. The selected AC2 SDSD filled in a 3D shell pill and further characterized for 3D shell pill for dissolution profiles and stability studies. The product has sustained release and similar release profiles after three months of storage. The findings suggest that the AC2 SDSDs may be a promising candidate for further development as a 3D printed drug delivery system for treating multiple disease conditions using model flavonoid- apigenin.

This paper analyzed the main diseases of the friction high-strength bolt (FHSB) joints in order to study the characteristics of the corrosion products of the joints in steel bridge and the influence factors. Seven representative FHSB connection pairs and eight steel plate samples were selected from the Dongying Shengli Yellow River Bridge, which has been in operation for 33 years. Then Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS) and X-Ray Diffraction (XRD) were used to analyze the microscopic morphology and chemical composition of the corroded surface of the samples. Finally, this paper discussed the relationship between the corroded sample surface and the environmental corrosion. The research results showed that construction quality problems, such as non-standard hole expansion, segmental slab joint dislocation and contact surface pollution, accelerated corrosion of the contact surface. With the increase of corrosion degree of joints, the contact surface of aluminum spraying layer gradually changed from a rugged and dense state to a smooth and porous powder state. With the corrosion of the steel plate substrate, the contact surface gradually changed from a fluffy stratified state to a surface bonding state. It was inferred that the friction coefficient of the FHSB connection node on the corroded aluminum sprayed contact surface first decreased and then increased. The corroded node samples detected not only a large number of S and Cl elements, but also the oxides of Mn, Si and other elements as well as FeS. It was speculated that node corrosion was also related to atmospheric (acid rain) and industrial dust and other corrosive environments. Almost all samples detected the component SiO2 of the Yellow River soil, as well as Mg, Ca, K, Na and other elements at the same time, which is basically consistent with the component elements of the Yellow River soil. Therefore, it was inferred that it was related to the inclusion of the Yellow River soil.

Today, more than 70 million tons of lignin are produced by the pulp and paper industry every year. However, the utilization of lignin as a source for chemical synthesis is still limited due to the complex and heterogeneous lignin structure. The purpose of this study was a selective photodegradation of industrially available kraft lignin in order to obtain appropriate fragments and building block chemicals for further utilization, e.g. polymerization. Thus, kraft lignin obtained from soft wood black liquor by acidification was dissolved in sodium hydroxide and irradiated at a wavelength of 254 nm with and without the presence of titanium dioxide in various concentrations. Analyses of the irradiated products via SEC showed decreasing molar masses and decreasing polydispersity indices over time. At the end of the irradiation period the lignin was depolymerised to form fragments as small as the lignin monomers. TOC analyses showed minimal mineralisation due to the depolymerisation process.

Influence of particle size on the mechanical strength of alkali activated material from waste refractory monolithic was investigated in this study. Precursor was chemically and mineralogically analysed, separated on 4 fractions and alkali activated with Na-water glass. Alkali activated materials were thoroughly investigated under SEM and XRD to evaluate the not predicted differences in mechanical strength. Time dependence of curing temperature on mechanical strength was investigated in the sample prepared from a fraction that caused the highest compressive strength.

The current investigation presents porous ceramic materials prepared of cenospheres prepared by spark plasma sintering. The impact of sintering temperature, mould diameter (20 and 30 mm diameter) and cenosphere size on the properties of the sintered material was investigated. Shrinkage of the samples during sintering started at 900 °C. Sample shrinkage during sintering increases with increasing temperature and decreases with increasing mould size; increasing sample sintering temperature increases the apparent density of all sample series CS 63-150 µm in 20 mm mould from 0.97 to 2.3 g·cm-3 at 1050 - 1300 °C, in 30 mm mould 0.81 - 1.87 g·cm-3 at 1050 - 1200 °C, in 50 mm mould 0.54 - 0.75 g·cm-3 at 1050 - 1150 °C, while CS 150-250 µm in 20 mm mould 0.93 - 1.96 g·cm-3 at 1050 - 1200 °C. Total porosity decreases from 61.5% to 3.9% with increasing sintering temperature from 1050 to 1250 °C, while open porosity reduces at lower temperatures, with closed porosity being highest in samples sintered at 1150 °C. When the sintering temperature increases from 1050 to 1300 °C, the compressive strength of the CS 63-150 samples produced in a 20 mm mould increases from 11 MPa to 312 MPa. These results correlate with the Rice model, which describes an exponential dependence of compressive strength on material porosity and fully dense material compressive strength.

2-(5,6-diphenyl-1,2,4-triazin-3-yl)pyridinium dichloroiodate (I) (1) was synthesized by reacting 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine with ICl in dichloromethane solution. The structural characterization of 1 by SC-XRD analysis was accompanied by elemental analysis, FT-IR, and FT-Raman spectroscopy measurements.

Stabilized un-doped Zinc Telluride (ZnTe) thin films were grown on glass substrates under vacuum using closed space sublimation (CSS) technique. A dilute copper nitrate solution (0.1/100 ml) was prepared for copper doping known as ion exchange process in the matrix of ZnTe thin film. The reproducible polycrystalline cubic structure of undoped and Cu doped ZnTe thin films with preferred orientation (111) was confirmed by X-rays diffraction (XRD) technique. Lattice parameter analyses verified the expansion of unit cell volume after incorporation of Cu species into ZnTe thin films samples. The micrographs of scanning electron microscopy (SEM) were used to measure the variation in crystal sizes of samples. The energy dispersive X-rays was used to validate the elemental composition of undoped and Cu-doped ZnTe thin films. The bandgap energy 2.24 eV of ZnTe thin film decreased after doping Cu to 2.20 eV may be due to the introduction of acceptors states near to valance band. Optical studies showed that refractive index was measured from 2.18 to 3.24 whereas thicknesses varied between 220 nm to 320 nm for un-doped and Cu doped ZnTe thin film respectively using Swanepoel model. The oxidation states of Zn⁺², Te⁺² and Cu⁺¹ through high resolution X-ray photoelectron spectroscopy (XPS) analyses was observed. The resistivity of thin films changed from ~10⁷ Ω-cm for undoped ZnTe to ~1 Ω-cm for Cu-doped ZnTe thin film, whereas p-type carrier concentration increased from to respectively. These results predicted that Cu-doped ZnTe thin film can be used as an ideal, efficient and stable intermediate layer between metallic and absorber back contact for the heterojunction thin film solar cell technology.

In this work, we have proposed two new methods for the synthesis of [TcO2L4]+ (where L = im-idazole (Im), methylimidazole (MeIm)) complexes using thiourea (Tu) and Sn(II) as reducing agents. The main and by-products of the reactions were determined, and possible reaction mechanisms were proposed. We have shown that the reduction of Tc(VII) with thiourea is ac-companied by the formation of the Tc(III) intermediate and further oxidation to Tc(V). The reac-tion conditions changing can lead to the formation of Tc(VII) and Tc(IV) salts. Seven new crystal structures are described in this work: Tc(V) complexes, salts with Tc(VII) and Tc(IV) anions. For halide salts of Tu the cell parameters were determined. In all obtained compounds, except for [TcO2(MeIm)4]TcO4, there are π-stacking interactions between aromatic rings. An increase in the anion size lead to weaken intermolecular interactions. Halogen bonds and anion-π interactions have also been found in hexahalide-containing compounds. The Hirshfeld surface analysis showed that the main contribution to the crystal packing is made by van der Waals interactions of the H···H type (42.5–55.1%), H···C/C ···H (17.7–21.3%) and hydrogen bonds, which contribute 15.7–25.3% in total.

The aging mechanism of 10% and 30% nickel substituted manganese hexacyanoferrate cathode material in aqueous zinc-ion batteries has been explored through the advanced synchrotron-based two-dimensional x-ray fluorescence technique. Thanks to the two-dimension modality, not only the metal concentration dynamics throughout the entire electrodes was followed during the aging process, but their spatial distribution was also revealed, suggesting the route of the material transformation. The dissolution of Mn and Ni, and the penetration of Zn inside the framework, alongside the Mn aggregations outside the hexacyanoferrate framework were detected. Additionally, the possibility of conducting x-ray absorption spectroscopy measurements on the regions of interest made it possible to explore the chemical state of each metal, and furthermore, synchrotron-based powder x-ray diffraction demonstrated the gradual structural modification in 30% Ni-containing sample series, in terms of the different phase formation.

The tribological performance of metalwork steel tools is of vital importance in both cold and hot working processes. One solution for improving metal tool life is the application of coatings. This paper investigates the effect of CrAlSiN thin-film PVD-deposition on the tribological behaviour of tool steel K340. The sliding wear performance of the coated K340 steel is analysed in relation to both the uncoated K340 steel and a range of tool steels dedicated to hot- and cold-working, such as X155CrVMo12-1, X37CrMoV5-1, X40CrMoV5-1, 40CrMnMo7 and 90MnCrV8. The investigated tool steels were heat-treated, while K340 was subjected to thermochemical treatment and then coated with a CrAlSiN hard film (K340/CrAlSiN). The hardness, chemical composition, phase structure and microstructure of steels K340 and K340/CrAlSiN are examined. Tribological tests were conducted using the ball-on-disc tester in compliance with the ASTM G99 standard. The tests were performed under dry unidirectional sliding conditions, using an Al2O3 ball as a counterbody. The wear factor and coefficient of friction are estimated and analysed with respect to hardness and alloying composition of the materials under study. SEM observations are made to identify the sliding wear mechanisms of the analysed tool steels and PVD-coated K340 steel. In contrast to the harsh abrasive-adhesive wear mechanism observed for uncoated tool steels, the abrasive wear dominates in case of the AlCrSiN. The deposited thin film effectively prevents the K304 substrate from harsh wear severe degradation. Moreover, thanks to the deposited coating, the K304/CrAlSiN sample has a COF of 0.529 and a wear factor of K=5.68×10−7 m3 N−1 m−1, while the COF of the reference tool steels ranges from 0.702 to 0.885 and their wear factor ranges from 1.68×10−5 m3 N−1 m−1 to 3.67×10−5 m3 N−1 m−1. The CrAlSiN deposition reduces the wear of the K340 steel and improves its sliding properties, which makes it a promising method for prolonging the service life of metalwork tools.

MoS₂/TiO₂ nanostructures made of MoS₂ nanoparticles covering TiO₂ nanosheets have been synthesized, either via ex-situ or in-situ approaches. Morphology and structure of MoS₂/TiO₂ hybrid nanostructures have been investigated and imaged by means of X-ray diffraction (XRD) analysis and high-resolution transmission electron microscopy (HRTEM), while the vibrational and the optical properties have been investigated by Raman, Fourier-transform infrared spectroscopy (FTIR) and UV−visible (UV-Vis) techniques. The different stacking degrees together with the size distribution of the MoS₂ nanosheets, decorating the TiO₂ nanosheets, have been carefully obtained from HRTEM images. The nature of the surface sites on the main exposed faces of both materials has been detected by means of in-situ FTIR spectra of adsorbed CO probe molecule. The results coming from the ex-situ and in-situ approaches will be compared, by highlighting the role of the synthesis processes in affecting morphology and structure of MoS₂ nanosheets, including their curvature, surface defects, and stacking order. Some more, it will be shown that the in-situ approach is affecting the reactivity of the TiO₂ nanosheets too, hence in turn affects the MoS₂/TiO₂ nanosheets interaction.

(1) Background: Since fullerene C60 is insoluble in water and is toxic, it is not applicable in biomedicine and cosmetics. For this reason, the first derivative FD-C60 (fullerenol) was synthesized, which solved the problem of solubility in water and partially reduced toxicity. In order to maximally reduce toxicity and increase biomedical efficiency, the second derivative SD-C60 (3HFWC- Hyper-Harmonized-Hydroxylated Fullerene Water Complex), was created. (2) Methods: In order to obtain the most reliable data, several different methods are applicable in the characterization of FD-C60 and SD-C60 with water layers (NIR, FTIR, 13C-NMR,  1H-NMR, TGA/DTA, XRD, AFM/MFM etc.). (3) Results: FD-C60 as an individual structure is about 1.3 nm in size, while SD-C60 as an individual structure is 1030 nm in size. The aforementioned methods showed that SD-C60 contains water layers, which explains the difference between those two structures in the physicochemical properties, and their effects on biomolecules. (4) Conclusions: Based on the above methods and techniques, FD-C60 and SD-C60 are two different substances in terms of size, structure, and physicochemical properties; FD-C60 at 100C has endothermic characteristics and SD-C60 at 133C has exothermic characteristics, FD-C60 possesses water molecules only from humidity, while SD-C60 has water molecules from both humidity and extra water molecules in layers, the zeta potential of FD-C60 is -25.85 mV, while it is -43.29 mV for SD-C60.

The (benzylthio)acetic acid (HBTA) and some aminopyrimidines, namely 2-aminopyrimidine (2-AP), 5-aminopyrimidine (5-AP), 2-amino-4,6-dimethylpyrimidine (2-A-4,6-DMP) and 2,4,6-triaminopyrimidine (2,4,6-TAP), were successfully embodied as structural units into the construction of a total of four novel supramolecular organic frameworks. The received crystalline solids were inspected by single crystal X-ray diffraction (SC XRD) in order to obtain insight into the structural and supramolecular facets. The SOFs deriving from 2-AP, 5-AP as well as 2-A-4,6-DMP crystallize in the form of true co-crystals (1-3), while the one originating from 2,4,6-TAP crystallizes as salt solvate (4). The SC XRD results indicated the different contents of structural residues present in the asymmetric units of the crystals 1-4 despite the using the same molar ratio of molecular co-formers in each case. The molecular structures of co-crystals 1-3 consist of either one neutral residue of each starting components (1 and 3) or a half nonionized residue of aminopyrimidine ingredient and one neutral residue of acidic specie (2). The asymmetric unit of salt solvate 4 is composed of two ionized residues of each co-former (two 2,4,6-TAP+ cations and two BTA- anions) and one MeOH solvent molecule. The most extensive H-bonding network is observed in the crystal structure of salt solvate 4. The relevant molecular ingredients in co-crystals 1-3 are mainly hold together by the neutral Ocarboxylic–H···Npyrimidine and Namine–H···Ocarboxylic H-bonds. In the case of aggregate 4, the corresponding ionic residues are predominantly sustained by the charged-assisted Npyrimidinium–H···Ocarboxylate and Namine–H···Ocarboxylate hydrogen interactions. The MeOH solvent incorporated into the crystal lattice of adduct 4 is also involved in H-bonding by simultaneously serving as the single donor in OMeOH–H···S and the single acceptor in Namine–H···OMeOH H-bonds afforded the structural diversity within the 2,4,6-TAP+ cations and BTA- anions. Other weaker sets of additional non-covalent contacts existing in the crystal structures of analyzed conglomerates are involved in the self-assembly, stabilization and expansion of total supramolecular organic frameworks. The fact of the formation of non-covalent bonded supramolecular organic frameworks in question is also reflected in corresponding results obtained through elemental analysis (EA), Fourier transform infrared spectroscopy (FT−IR) and thermal analysis (TG/DSC).

Free volume is an extremely important intrinsic defect in polymers. Structurally, the free volume is the randomly distributed holes in the polymer molecular chain segments. From the perspective of molecular movement, it is also the space needed for the movement of molecular segments. In proton exchange membrane fuel cells, the free volume is also the space needed for the directional conduction of protons. Irradiation grafting sulfonated polyvinylidene fluoride (PVDF) is one of the methods to produce proton exchange membrane with good proton channel rate. Using the LYS-1 program, based on the linear absorption coefficient and backscatter coefficient models, the percentage of annihilated positrons in PVDF in the two-layer model and the three-layer model was studied, and comparing the two fitting results it is determined that the model closest to the positron annihilation percentage required by the PALS experiment is the two-layer model, which allows the percentage of positrons that are annihilated in PVDF films with a thickness of 100 μm to reach 46% using the high energy positron source ⁴⁴Ti without using the positron moderator. Using positron annihilation lifetime spectrum (PALS) analysis methods, based on Eldrup's classical model of free volume, the influence of absorbed doses of α particles on the free volume and crystallinity of PVDF was investigated, respectively. Based on the two test results the model of cross-linking and degradation of polyvinylidene fluoride irradiated by α particles was determined. Afterwards, X-ray diffraction (XRD) methods was used to study the change of PVDF crystal area before and after irradiation. The XRD results are consistent with the results measured by PALS.