App-based Quantification of Crystal Phases and Amorphous Content in ZIFs Biocomposites

The performance of Zeolitic Imidazolate Frameworks (ZIFs) as protective hosts for proteins in drug delivery or biocatalysis strongly depends on the type of crystalline phases used for the encapsulation of the biomacromolecule (biomacromolecule@ZIF). Therefore, quantifying the different crystal phases, and the amount of amorphous content of ZIFs is becoming increasingly important for a better understanding of the structure-property relationship. Typically, crystalline ZIF phases are qualitatively identified from diffraction patterns. However, accurate phase examinations are time-consuming and require specialized expertise. Here, we propose a calibration procedure (internal standard ZrO2) for the rapid and quantitative analysis of crystalline and amorphous ZIF phases from diffraction patterns. We integrated the procedure into a user-friendly web application, named ZIF Phase Analysis, which facilitates ZIF-based data analysis. As a result, it is now possible to quantify i) the relative amount of various common crystal phases (sodalite, diamondoid, ZIF-CO3-1, ZIF-EC-1, U12 and ZIF-L) in biomacromolecule@ZIF biocomposites based on Zn2+ and 2-methylimidazole (HmlM) and ii) the crystalline-to-amorphous ratio. This new analysis tool will advance the research on ZIF biocomposites for drug delivery and biocatalysis.

Recent developments in reactivity testing of supplementary cementitious materials

Identification and rapid characterization of novel supplementary cementitious materials (SCMs) is a critical need, driven by shortfalls in conventional SCMs. In this study, we present a discussion of recently developed reactivity tests – the R3 test, the modified R3 test, the lime strength test, and the bulk resistivity index test. These tests measure reactivity parameters such as heat release, bound water, calcium hydroxide consumption, strength, and bulk resistivity. All tests can screen inert from reactive materials. To additionally differentiate pozzolanic and latent hydraulic materials, two parameters, for example, calcium hydroxide consumption and heat release, are needed. The influences of SCM bulk chemistry, amorphous content, and fineness on measured reactivity are outlined. Reactivity test outputs can predict strength and durability of cement paste/mortar/concrete; however, caution must be exercised as these properties are influenced by a variety of other factors independent of reactivity. Thoughts are provided on using reactivity tests to screen materials for concrete durability.

Accuracy in Cement Hydration Investigations: Combined X-ray Microtomography and Powder Diffraction Analyses

Cement hydration is a very complex set of processes. The evolution of the crystalline phases during hydration can be accurately followed by X-ray powder diffraction data evaluated by the Rietveld method. However, accurate measurements of some microstructural features, including porosity and amorphous content developments, are more challenging. Here, we combine laboratory X-ray powder diffraction and computed microtomography (μCT) to better understand the results of the μCT analyses. Two pastes with different water–cement ratios, 0.45 and 0.65, filled within capillaries of two sizes, ϕ = 0.5 and 1.0 mm, were analysed at 50 days of hydration. It was shown that within the spatial resolution of the measured μCTs, ~2 μm, the water capillary porosity was segmented within the hydrated component fraction. The unhydrated part could be accurately quantified within 2 vol% error. This work is a first step to accurately determining selected hydration features like the hydration degree of amorphous phases of supplementary cementitious materials within cement blends.

Reinforcing Mechanism of WC Particles in Fe-Based Amorphous Matrix Coating on Magnesium Alloy Surface

To protect magnesium alloy surfaces from wear and corrosion, an Fe-based amorphous coating was prepared on WE43 through the Ni60 interlayer by high-velocity oxygen-fuel (HVOF) spraying. The porosity was ~1%, and the amorphous content exceeded 90%. The wear and corrosion resistance of the composite coating with WC particles wrapped in a Ni layer as the reinforcing phase were compared with that of the completely amorphous coating. The friction coefficient (COF) of the composite coating was 0.3, which is only half of that of the WE43 substrate, and the composite coating exhibited a more stable wear behavior than the completely amorphous coating. The corrosion tendency of the composite coating is lower than that of stainless steel, with a corrosion potential of −0.331 V, and the addition of WC particles did not deteriorate the corrosion resistance considerably. The bonding mechanism of the bonding interface between the amorphous structure and the particles of the reinforcing phase was investigated by transmission electron microscopy (TEM). Reinforcing particles were confirmed to form metallurgical bonding with the coating. It was found that the Ni layer showed excellent bonding performance in the form of a mixture that is amorphous and nanocrystalline. Therefore, the Fe-based amorphous composite coating on a magnesium alloy surface shows a potential protective effect.

Effect of new crystalline phase on the ionic conduction properties of sodium perchlorate salt doped carboxymethyl cellulose biopolymer electrolyte films

Dopant induced modifications in the microstructure of sodium carboxymethyl cellulose (NaCMC) were characterized by FTIR, XRD, DSC and EIS techniques. FTIR analysis exhibited a considerable microstructural modification in NaCMC upon NaClO4⋅H2O doping invoked through complex formation via Lewis acid-base interaction and hydrogen bond formation between ions and dipoles. This resulted in the modification in the orderliness/disorderliness of polymer chains as observed from XRD deconvolution. At higher salt concentrations, the complexity of the network causes the formation of new amorphous and crystalline phases as reflected in the XRD studies. DSC analysis showed an increase in Tg as the salt concentration increased, indicating a reduction in polymer chains flexibility. The contribution of free ions has masked over the enhancement in amorphous content to conductivity at a lower concentration of salt in the matrix, later on, the formation of a new crystalline phase due to transient crosslinks by Na+…ClO4−…Na+ has affected the ion transport process.

CHARACTERIZATION OF CHEMICALS FROM PROSOPIS JULIFLORA (PJ) – A POTENTIAL ENHANCER FOR LIGHTWEIGHT POLYMER APPLICATIONS

The latest research is about ProsopisJuliflora’s mining and characterization officers. The fibres were cut, chemically treated using sodium and hydrochloric acid (alkali) solutions. Chemically modified and non-modified fibres have been analysed for their thermal, chemical, crystalline, electrical, morphological and tensile characteristics. The findings showed that a cellulose content was increased by 59.8 % with a reduction of amorphous content and humidity by chemical treatment with alkali. However, due to its acid-plus attacks whose values were lower than untreated, the treatment for hydrochloric acid reduced cellulosis material. There were four hundred and seventeen nm of crystalline fibre of alkaline therapy, less than one 68.01 nm. Thus the ProsopisJuliflora can be suggested for lightweight polymer applications as a possible reinforcement.

High-Performance HVOF-Sprayed Fe-Based Amorphous Coating on LA141 Magnesium Alloy via Optimizing Oxygen Flow and Kerosene Flow

To solve the problem of poor corrosion and wear resistance of Mg-Li alloys, Fe-based amorphous coatings were prepared by high velocity oxygen-fuel spraying technology (HVOF) on the LA141 magnesium alloy substrate with a Ni60 intermediate layer. The microstructure and performance of Fe-based amorphous coatings with different oxygen flow and kerosene flow were characterized and analyzed. The results demonstrate that there is an optimal oxygen/kerosene ratio where the porosity of Fe-based amorphous coating is the lowest. Moreover, the amorphous content increases with the decrease in the oxygen/kerosene ratio. In particular, when the oxygen flow is 53.8 m3/h and the kerosene flow is 26.5 L/h, the Fe-based amorphous coating possesses the lowest porosity (0.87%), the highest hardness (801 HV0.1), the highest bonding strength (56.9 MPa), and an excellent corrosion and wear resistance. Additionally, it can be seen that the Fe-based amorphous coating is composed of amorphous splats and amorphous oxides, but the Ni60 intermediate layer exhibits an amorphous and crystalline multi-phase structure. The high bonding strength of the coating is attributed to the low porosity of Fe-based amorphous coating and the localized metallurgical bonding between different layers. Finally, the mechanisms on corrosion and wear of Fe-based amorphous coatings are also discussed.

Mechanically activated mine tailings for use as supplementary cementitious materials

Two mine tailings are evaluated for their potential as supplementary cementitious materials. The mine tailings were milled using two different methods – ball milling for 30 minutes and disc milling for durations ranging from 1 to 15 minutes. The modified R3 test was carried out on the mine tailings to quantify their reactivity. The reactivity of the disc milled tailings is greater than those of the ball milled tailings. Strong correlations are obtained between milling duration, median particle size, amorphous content, dissolved aluminum and silicon, and reactivity of the mine tailings. The milling energy results in an increase in the fineness and the amorphous content, which do not appreciably increase beyond a disc milling duration of 8 minutes. The reactivity increases significantly beyond a certain threshold fineness and amorphous content. Cementitious pastes were prepared at 30% supplementary cementitious materials replacement level at a water-to-cementitious materials ratio of 0.40. No negative effects of the mine tailings were observed at early ages in cement pastes based on isothermal calorimetry and thermogravimetric analysis, demonstrating the potential for these materials to be used as supplementary cementitious materials.

Modification of structural, thermal and optical properties of PC-PET/CdSe NCP using gamma radiation

In the current study we synthesized a nanocomposite (NCP) from polycarbonate/polybutylene terephthalate (PC-PET) blend and CdSe nanoparticles (NPs) through ex-situ casting methodology. CdSe NPs were synthesized using thermolysis technique with N2 gas flow. X-ray diffraction data for CdSe NPs are reported. The Rietveld refinement indicated that the synthesized CdSe acclimatizes cubic zinc blends constitution of a lattice parameter 6.057 Å and an average grain size of 2 nm. The PC-PET/CdSe NCP samples were irradiated by gamma doses between 20 and 230 kGy. The induced variations in the structure, thermal and optical properties of the gamma irradiated PC-PET/CdSe NCP have been illustrated by means of TEM, XRD, TGA, FTIR and UV-vis spectroscopes. The irradiation with doses in the range 50-230 kGy leads to the domination of crosslinking that improves the amorphous content. This increases the degradation temperature from 417 to 432oC indicative of an enhancement in the thermostability of the NCP samples. Also, the optical band gap is reduced from 4.28 to 3.76 eV which is ascribed to the enhancement in the amorphous content of the irradiated PC-PET/CdSe NCP. This specifies that the gamma irradiation causes a more compactness of the NCP and leads to appropriate spreading of CdSe NPs within the PC-PET matrix. Additionally, the CIE approach was used to describe the colored samples. It is found that the PC-PET/CdSe NCP acquires color due to gamma doses, as the color intensity reached a remarkable color difference larger than 5 (14.9) which is a reasonable challenge in saleable reproduction on printing press.