Influence of Nucleation Agents Concentration on Crystallization Structure and Properties of Glass-ceramics

Deep color glass-ceramics is prepared by using gold tailings as the main raw material, and Cr2O3 is added as nucleation agent. Influence of different Cr2O3 additions on crystallization structure and properties of CaO-MgO-Al2O3-SiO2 glass-ceramics has been discussed so as to select optimum additions. DTA is employed to determine optimum crystallization and nucleation temperatures; XRD and SEM are used to characterize microstructure of each sample; and performance indexes, such as water absorption, bulk density, flexural strength and so on, are also determined. Experimental results show that when 3wt% Cr2O3 is introduced, fine glass-ceramics with diopside as the main crystal and Ca-Fe diopside as the second-crystal is obtained, and its corresponding performance indexes are as follows： water absorption 0.12%, bulk density 2.56 g/cm^3, and flexural strength 70.01 Mpa.

Copper complexes of anthrahydrazone bearing pyridyl side chain:Synthesis,crystal structure,anticancer activity,and DNA binding

To expand the study on the structures and biological activities of the anthracyclines anticancer drugs and reduce their toxic side effects,the new anthraquinone derivatives,9‑pyridylanthrahydrazone(9‑PAH)and 9,10‑bispyridylanthrahydrazone(9,10‑PAH)were designed and synthesized.Utilizing 9‑PAH and 9,10‑PAH as promising anticancer ligands,their respective copper complexes,namely[Cu(L1)Cl_(2)]Cl(1)and{[Cu_(4)(μ_(2)‑Cl)_(3)Cl_(4)(9,10‑PAH)_(2)(DMSO)_(2)]Cl_(2)}_(n)(2),were subsequently synthesized,where the new ligand L1 is formed by coupling two 9‑PAH ligands in the coordination reaction.The chemical and crystal structures of 1 and 2 were elucidated by IR,MS,elemental analysis,and single‑crystal X‑ray diffraction.Complex 1 forms a mononuclear structure.L1 coordinates with Cu through its three N atoms,together with two Cl atoms,to form a five‑coordinated square pyramidal geometry.Complex 2 constitutes a polymeric structure,wherein each structural unit centrosymmetrically encompasses two five‑coordinated binuclear copper complexes(Cu1,Cu2)of 9,10‑PAH,with similar square pyramidal geometry.A chlorine atom(Cl_(2)),located at the symmetry center,bridges Cu1 and Cu1A to connect the two binuclear copper structures.Meanwhile,the two five‑coordinated Cu2 atoms symmetrically bridge the adjacent structural units via one coordinated Cl atom,respectively,thus forming a 1D chain‑like polymeric structure.In vitro anticancer activity assessments revealed that 1 and 2 showed significant cytotoxicity even higher than cisplatin.Specifically,the IC_(50)values of 2 against HeLa‑229 and SK‑OV‑3 cancer cell lines were determined to be(5.92±0.32)μmol·L^(-1)and(6.48±0.39)μmol·L^(-1),respectively.2 could also block the proliferation of HeLa‑229 cells in S phase and significantly induce cell apoptosis.In addition,fluorescence quenching competition experiments suggested that 2 might interact with DNA by an intercalative binding mode,offering insights into its underlying anticancer mechanism.CCDC:2388918,1;2388919,2.

Crystal structure,phase transitions,and thermodynamic properties of magnesium metavanadate(MgV_(2)O_(6))

As a promising anode material for magnesium ion rechargeable batteries,magnesium metavanadate(MgV_(2)O_(6))has attracted considerable research interest in recent years.A MgV_(2)O_(6)sample was synthesized via a facile solid-state reaction by multistep-firing stoichiometric mixtures of MgO and V2O5 powder under an air atmosphere.The solid-state phase transition fromα-MgV_(2)O_(6)toβ-MgV_(2)O_(6)occurred at 841 K and the enthalpy change was 4.37±0.04 kJ/mol.The endothermic effect at 1014 K and the enthalpy change was 26.54±0.26 kJ/mol,which is related to the incongruent melting ofβ-MgV_(2)O_(6).In situ XRD was performed to investigate phase transition of the as-prepared MgV_(2)O_(6)at high temperatures.The cell parameters obtained by Rietveld refinement indicated that it crystallizes in a monoclinic system with the C2/m space group,and the lattice parameters of a=9.280 A°,b=3.501 A°,c=6.731 A°,β=111.76°.The solid-state phase transition fromα-MgV_(2)O_(6)toβ-MgV_(2)O_(6)was further studied by thermal kinetics,indicating that this process is controlled first by a fibril-like mechanism and then by a spherulitic-type mechanism with an increasing heating rate.Additionally,the enthalpy change of MgV_(2)O_(6)at high temperatures was measured utilizing the drop calorimetry,heat capacity was calculated and given as:Cp=208.3+0.03583T-4809000T^(−2)(298-923 K)(J mol^(−1)K^(−1)),the high-temperature heat capacity can be used to calculate Gibbs free energy of MgV_(2)O_(6)at high temperatures.

Co-crystallization of Resorcin[4]arene Tetracarboxylic Acid with Triethylamine:Synthesis and Crystal Structure

Treatment of resorcin[4]arene tetracarboxylic acid 1 with triethylamine in the presence of Co（CH3COO）2·4H2O and 4,4 -bipyridine gave a co-crystallization 14-·4Et3NH＋（C32H20O164-·4Et3NH＋,Mr=1069.27） from ethanol and water.The compound was structurally determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n,with a=8.1763（18）,b=12.913（3）,c=28.724（7） ,β=97.574（4）o,V=3006.3（12） 3,Z=2,Dc=1.181 g/cm3,F（000）=1152,Rint=0.0275,T=293（2） K,μ=0.086 mm-1,the final R=0.0634 and wR = 0.1752 for 5082 observed reflections with I 〉 2σ（I）. The co-crystallization is very stable at room temperature. Possibly, a network of N-H…O（=C） plays an important role in the structure. Meanwhile, the compound emits a weak cyan luminescence with peak maximum band at 458 nm.

Crystal structure transformation and lattice impurities migration of quartz during chlorine roasting

To investigate the effect of chlorine roasting on the migration and removal of trace elements in quartz lattice,firstly,an efficient pretreatment process,grinding–HCl washing–flotation–HF and HCl leaching,was used to remove the gangue minerals in quartz ore to obtain purified quartz for the preparation of high-purity quartz and the investigation of lattice impurities migration.The results showed that the high-purity quartz with total impurities less than 50μg/g could be obtained from purified quartz after being treated with chlorine at 1200°C.The variation of crystal structure and the lattice impurities migration of quartz during chlorine roasting were studied through in-situ XRD,TGA,SEM-EDS,ICP-MS,FT-IR and XPS analysis.It revealed that the decomposable impurities H_(2)O,-OH,and residual collectors in the crystal of purified quartz could be effectively removed through chlorine roasting above 900°C,which also had an obvious effect on the removal of low-valence trace elements Li,Na and K in the crystal of quartz but didn't affect the multivalent trace elements Al and Ti.This study revealed the removal and migration mechanism of the trace elements in quartz crystal during chlorine roasting.

Microstructure and forming mechanism of metals subjected to ultrasonic vibration plastic forming: A mini review

Compared with traditional plastic forming,ultrasonic vibration plastic forming has the advantages of reducing the forming force and improving the surface quality of the workpiece.This technology has a very broad application prospect in industrial manufactur-ing.Researchers have conducted extensive research on the ultrasonic vibration plastic forming of metals and laid a deep foundation for the development of this field.In this review,metals were classified according to their crystal structures.The effects of ultrasonic vibration on the microstructure of face-centered cubic,body-centered cubic,and hexagonal close-packed metals during plastic forming and the mech-anism underlying ultrasonic vibration forming were reviewed.The main challenges and future research direction of the ultrasonic vibra-tion plastic forming of metals were also discussed.

Synthesis,crystal structure,and DNA‑binding of binuclear lanthanide complexes based on a multidentate Schiff base ligand

Two new dinuclear lanthanidecomplexes,namely[Ln_(2)(dbm)_(2)(HL)_(2)(CH_(3)OH)_(2)]·4CH_(3)OH[Ln=Tb(1)and Dy(2),Hdbm=dibenzoylmethane]have been synthesized using prepared multidentate Schiff base ligand H_(3)L(hydroxy‑acetic acid(4‑diethylamino‑2‑hydroxy‑benzylidene)‑hydrazide)with good biological activity.Structure characterizations show that the complex comprises two Ln3+ions,two dbm-ions,two HL^(2-)ligands,two CH_(3)OH molecules,and four free methanol molecules.Each Ln^(3+)ion is eight‑coordinated.The two central Lnions are bridged by twoμ_(2)‑O atoms leading to a parallelogram[Ln2O2]core.The interaction between the compounds(H_(3)L,1,and 2)and the calf thymus DNA(CT‑DNA)has been further confirmed by UV‑Vis spectrometry,fluorescence titration,and cyclic voltammetry.The results showed that both 1 and 2 could undergo insertion with CT‑DNA.CCDC:2343005,1;2343006,2.

Synthesis,crystal structures,and antibacterial activities of two zinc(Ⅱ) complexes bearing 5⁃phenyl⁃1H⁃pyrazole group

A novel compound(H_(2)L)SCN(5⁃methyl⁃3⁃phenyl⁃2H⁃pyrazol⁃1⁃ium thiocyanate)has been obtained by the reaction of thiosemicarbazide with benzoylacetone in ethanol.Two zinccomplexes[Zn(HL)_(2)(NCS)(CH_(3)COO)](1)and[Zn_(2)(L)_(2)(HL)_(2)(NCS)_(2)]_(2)·2CH_(3)OH(2)have been synthesized by the coordination reactions of Zn(OAc)_(2)·2H_(2)O or ZnCl_(2)with(H_(2)L)SCN under reflux conditions.Elemental analyses and single⁃crystal X⁃ray diffraction have con⁃firmed the structures of the synthesized compounds.The(H_(2)L)SCN ligand and complex 1 pertain to the triclinic sys⁃tem with space group P1,while complex 2 belongs to the monoclinic system with space group P2_(1)/n.Additionally,the antibacterial activities of the compounds were evaluated in vitro using the agar diffusion method against the bac⁃terial strains(Candida albicans,Staphylococcus aureus,and Escherichia coli).The results showed that the ligand exhibited relatively good antibacterial activities against the bacteria,and the complexes possessed stronger antibac⁃terial activities against the same bacteria than the free ligand.CCDC:2190252,(H2L)SCN;2190253,1;2190256,2.

Cryo-EM combined with image deconvolution to determine ZIF-8 crystal structure

Metal–organic frameworks(MOFs) are crystalline porous materials with tunable properties, exhibiting great potential in gas adsorption, separation and catalysis.[1,2]It is challenging to visualize MOFs with transmission electron microscopy(TEM) due to their inherent instability under electron beam irradiation. Here, we employ cryo-electron microscopy(cryoEM) to capture images of MOF ZIF-8, revealing inverted-space structural information at a resolution of up to about 1.7A and enhancing its critical electron dose to around 20 e^(-)/A^(2). In addition, it is confirmed by electron-beam irradiation experiments that the high voltage could effectively mitigate the radiolysis, and the structure of ZIF-8 is more stable along the [100] direction under electron beam irradiation. Meanwhile, since the high-resolution electron microscope images are modulated by contrast transfer function(CTF) and it is difficult to determine the positions corresponding to the atomic columns directly from the images. We employ image deconvolution to eliminate the impact of CTF and obtain the structural images of ZIF-8. As a result, the heavy atom Zn and the organic imidazole ring within the organic framework can be distinguished from structural images.

Structure and superconducting properties of Ru_(1-x)Mo_(x)(x=0.1-0.9)alloys

We report the detailed crystal structures and physical properties of Ru_(1-x)Mo_(x)alloys in the solid solution range of x=0.1-0.9.Structure characterizations indicate that the crystal structure changes from the hcp-Mg-type,toβ-CrFe-type,and then bcc-W-type.The measurements of physical properties show that the Ru_(1-x)Mo_(x)samples with x≥0.2are superconductors and the superconducting transition temperature T_c as a function of Mo content exhibits a dome-like behavior.

Syntheses,structures,and properties of three coordination polymers based on 5⁃ethylpyridine⁃2,3⁃dicarboxylic acid and N⁃containing ligands

Three coordination polymers[Mn(epda)(2,2'⁃bipy)(H_(2)O)](1),[Mn(epda)(phen)](2),and[Co_(2)(epda)2(bpe)2(H_(2)O)_(4)]·5H_(2)O(3)(H2epda=5⁃ethyl⁃pyridine⁃2,3⁃dicarboxylic acid,2,2'⁃bipy=2,2'⁃bipyridine,phen=phenanthroline,bpe=1,2⁃bis(4⁃pyridyl)ethylene)were synthesized by solvothermal reactions and characterized by single⁃crystal X⁃ray diffraction,thermogravimetric analyses,IR spectroscopy and elemental analysis.1 displays a 1D chain struc⁃ture,and these chains are joined by O-H…O hydrogen bonding andπ⁃πstacking interactions to generate a 2D layer structure.2 displays a 2D layer structure,and adjacent layers are generated 3D architecture throughπ⁃πstacking interactions.3 displays a 1D chain structure,and adjacent chains are generated double layer structure through O-H…O hydrogen bonding.The fluorescent properties of 1 and 3 indicate that they can potentially be used as a luminescent sensor.1 was highly selective and sensitive towards o⁃nitrophenol through different detection mechanisms,however,3 was highly selective and sensitive towards 2,4,6⁃trinitrophenol.In addition,the magnetic behavior of 2 has also been investigated.CCDC:2172533,1,2355773,2,2355774,3.

Syntheses,crystal structures,and quantum chemistry calculation of two Ni(Ⅱ)coordination polymers

Two new coordination polymers,[Ni(Hpdc)(bib)(H_(2)O)]_(n)(1)and{[Ni(bib)_(3)](ClO_(4))_(2)}_(n)(2),were prepared by mixing Ni^(2+),3,5⁃pyrazoledicarboxylic acid(H3pdc)/p⁃nitrobenzoic acid and 1,4⁃bis(imidazol⁃1⁃ylmethyl)butane(bib)by a hydrothermal method,respectively.X⁃ray crystallography reveals a 2D network constructed by six⁃coordinated Ni(Ⅱ)centers,bib,and Hpdc2-ligands in complex 1,while a 2D network is built by Ni(Ⅱ)and bib ligands in 2.Furthermore,the quantum⁃chemical calculations have been performed on‘molecular fragments’extracted from the crystal structure of 1 using the PBE0/LANL2DZ method in Gaussian 16 and the VASP program.CCDC:2343794,1;2343798,2.

Effect of fermented polypeptide of Sacha Inchi(Plukenetia volubilis L.)on the structure of liquid crystal emulsion

In order to study the action mechanism of Sacha Inchi polypeptide in liquid crystal emulsion,oil-in-water liquid crystal emulsions with Sacha Inchi fermented polypeptide as the active component were prepared.The microstructures,particle sizes,stabilities,thermodynamic properties,and rheological properties of liquid crystal emulsions with different concentrations of the fermentation products were observed by Polarizing microscope,Particle size meter,Thermogravimetric differential thermal synchronous measurement system,and Rheometer,respectively.The results showed that the average particle size of fermented peptide liquid crystal emulsion was(25.7±2.8)μm,and the liquid crystal structure was complete and stable.The content of bound water and liquid crystal in the emulsion with 1%Sacha Inchi polypeptide were higher than those in the blank emulsion and the emulsions with 3%and 5%Sacha Inchi polypeptide.Rheological results indicated that the viscosity of liquid crystal emulsion with the change curve of shear rate registered the shear thinning phenomenon,which belongs to non-Newtonian fluid.The hysteresis area,energy storage modulus,and loss modulus of the 1%additive amount of liquid crystal emulsion were larger than those of the blank emulsion and the emulsions with 3%and 5%Sacha Inchi polypeptide,indicating greater thixotropy and stronger shear resistance.The hydrophilic amino acid residues of the peptide in the 1%additive amount of the emulsion were combined with the water phase,while the hydrophobic amino acid residues of the peptide entered the oil phase,which formed a viscoelastic film at the oil-water interface,so that the liquid crystal emulsion had a more stable gel network structure.

Synthesis,crystal structure and photo-physical properties of tris(4-methyl-2,5-diphenylpyridine)iridium for OLED

Organic light-emitting diodes(OLEDs)have important applications in the field of next-generation displays and lighting,and phosphorescent iridium complexes are an important class of electroluminescent phosphorescent materials.In this paper,Ir(bmppy)_(3),tris(4-methyl-2,5-diphenylpyridine)iridium,was synthesized and elvaluted for photo-physical characteristics.Single crystals suitale for X-ray diffraction(XRD)were grown from a mixture solvent of dichloromethane and absolute ethanol.The composition and structur of Ir(bmppy)_(3)were determined by element analysis,NMR spectra and XRD.The complex crystallizes in the monoclinic symmetry with the space group P21/c with a slightly distorted octahedral configuration.As measured by UV-Visible and photoluminescence spectra,Ir(bmppy)_(3) displays a maximum emission at at 527 nm at ambient temperature,a typical green-emitting profile.The complex has potential for application in the OLED industry.

THE STRUCTURE OF AGGREGATION STATE AND ISOTHERMAL CRYSTALLIZATION KINETICS OF NYLON-1010

The structure of aggregation state and isothermal crystallization behavior of Nylon-1010 have been studied by WAXD, DSE, Variance-Range Function and density measurement. The results show that crystallization of Nylon-1010 has the most suitable annealing temperature, the crystals of the Nxlon-1010 are two-dimension heterogeneous nucleation. Both low treatment temperature and high crystallization te, temperature are disadvantageous for Nylon-1010 crystal growth.

Two novel Cu(Ⅰ)complexes based on diimide and bisphosphine ligands:synthesis,crystal structure and spectroscopic properties

Two Cu(Ⅰ)complexes[Cu(Bphen)(dppBz)]ClO_(4)·2CH_(3)OH(1)and[Cu_(2)(Bphen)_(2)(dpppda)]BF_(4)(2){Bphen=4,7-diphenyl-1,10-phenanthroline,dppBz=1,2-Bis(diphenylphosphino)benzene,dpppda=N1,N1,N4,N4-tetrakis[(diphenylphosphino)methyl]-1,4-benzenediamin}were synthesized using a one-pot method.X-ray crystallography was used to elucidate their crystal structures and photophysical properties.A series of characterization tests including elemental analysis,NMR,FT-IR,UV-Vis absorption spectroscopy,fluorescence spectroscopy,thermal gravimetric analysis and terahertz time-domain spectroscopy(THz-TDS)were used to further investigate their properties.The results show that complex 1 structure is mononuclear containing two solvent molecules per unit cell,while complex 2 structure is binuclear containing two metal centers per unit cell.According to photophysical properties and density functional theory(DFT)calculations,their luminescence properties can be attributed to metal-to-ligand charge transfer(MLCT).Both complexes have a unique stability,which is confirmed by thermal gravimetric analysis.

The Crystal Structure Study of CaSrFe0.75Co0.75Mn0.5O6−δ by Neutron Diffraction

The crystal structure of CaSrFe0.75Co0.75Mn0.5O6−δ is investigated through neutron diffraction techniques in this study. The material is synthesized using a solid-state synthesis method at a temperature of 1200˚C. Neutron diffraction data is subjected to Rietveld refinement, and a comparative analysis with X-ray diffraction (XRD) data is performed to unravel the structural details of the material. The findings reveal that the synthesized material exhibits a cubic crystal structure with a Pm-3m phase. The neutron diffraction results offer valuable insights into the arrangement of atoms within the lattice, contributing to a comprehensive understanding of the material’s structural properties. This research enhances our knowledge of CaSrFe0.75Co0.75Mn0.5O6−δ, with potential implications for its applications in various technological and scientific domains.

Analyses of Reaction Mechanisms among Different Sulfonation Reagents and m-Diphenylamine and Crystal Structures of the Formed Compounds

In the traditional process, m-phenylenediamine reacts with fuming sulfuric acid at high temperature to get intermediates, and then after dehydration occurs intramolecular rearrangement to get 2,4-diaminobenzenesulfonic acid. Traditional methods need to consume a lot of fuming sulfuric acid or concentrated sulfuric acid, resulting in high industrial large-scale production cost, more waste, and posing a serious environmental pollution risk. In this thesis, three different sulfonation reagents were used for the sulfonation reaction of m-phenylenediamine, and the reaction mechanisms and crystal structures of the three pathways were investigated. The three routes are: 1) one-step synthesis of monosulfonated compound 1 from raw material and sulfur trioxide (SO3);2) rapid reaction of raw material and chlorosulfonic acid to synthesize bisulfonated compound 2;3) direct eutectic crystallization of raw material and ordinary sulfuric acid to obtain compound 3. The crystal structure of the compounds synthesized by three paths was analyzed by X-ray single crystal diffraction, and compound 1 was characterized by NMR, Fourier infrared spectra, UV-visible spectrum and Mass spectrometry. The one-step synthesis of SO3 as a sulfonation reagent has the advantages of mild reaction conditions, simple operation and low cost.

Antiphase boundary-like structure in α′′ martensite of TC21 titanium alloy

The morphology and formation mechanism of the substructure of martensite in TC21 alloy was investigated by XRD and TEM. The results showed that the martensitic transformation from β to α＂ occurs upon quenching after solution treatment between 960-1000 ℃. The antiphase boundary （APB）-like structure was observed clearly in the α＂ martensite plates. The APB-like contrasts exist along the （001） and （020） planes of α＂ martensite. This APB-like structure of α＂ martensite was identified as a kind of stacking fault with an APB-like morphology induced by martensitic transformation and not by order/disorder transition. During martensitic transformation, martensitic domains nucleate and grow, eventually encounter each other, resulting in the formation of the APBdike contrast.

Phase structure and electrochemical properties of La_(1.7+x)Mg_(1.3-x)(NiCoMn)_(9.3)(x=0-0.4) hydrogen storage alloys

The phase structure and electrochemical properties of La1.7＋xMg1.3-x（NiCoMn）9.3（x=0-0.4） alloys were investigated. The XRD analysis reveals that the alloys consist of LaNi5 phase and other phases, such as LaMg2Ni9 phase （PuNi3 structure） and La4MgNi19 phases （Ce5Co19＋Pr5Co19 structure, namely A5B19 type）. With the increase of the x value, the LaMg2Ni9 phase fades away and La4MgNi19 phases appear, while the abundance of LaNi5 phase firstly increases and then decreases. At the same time, the cell volume of LaNi5 phase and LaMg2Ni9 phase decreases. The electrochemical measurement shows that alloy electrodes could be activated in 4-5 cycles, and with the increase of the x value, the maximum discharge capacity gradually increases from 330.9 mA-h/g （x=0） to 366.8 mA-h/g （x=0.4）, but the high-rate dischargeability （HRD） and cyclic stability （S） decrease somewhat （x=0.4, HRD600=82.32%, S100=73.8%）. It is found that the HRD is mainly controlled by the electrocatalytic activity on the alloy electrode surface, and the decline of cyclic stability is due to the appearance of A5B19 type phase with larger hydrogen storage capacity, which leads to larger volume expansion and more intercrystalline stress and then easier pulverization during charging/discharging.