Multi-technique Investigation Research Articles

Interaction of anionic dye ethyl orange and cationic CnTAC surfactants: A multi technique investigation

This research presents the application of electrical conductivity measurements to ascertain the critical micelle concentration (CMC) values for N-alkyltrimethylammonium chloride surfactants (CnTAC; with alkyl chain lengths of n = 12, 14, 16, and 18). Complementary spectrophotometric analysis was conducted to probe the interactions between CnTAC series and Ethyl Orange (ETO), an anionic dye. Applying the Benesi-Hildebrand and Scott equations, we evaluated the binding constant (Kb) of the cationic micelles’ interaction with ETO, which in turn facilitated calculations of Gibb’s free energy (ΔG°) changes. These calculations provided insight into the binding affinity of ETO to the micelles. Our findings suggest that the interaction between ETO and CnTAC is contingent on the surfactant concentration, with higher concentrations leading to a disassociation of the ETO-CnTAC complex and a reduction in ETO adsorption. Notably, the alkyl chain length within CnTAC molecules critically affects various properties, including ΔG°, CMC, and other thermodynamic parameters that determine the surfactant’s energetic behavior. The study underscores the importance of the alkyl chain length in dictating the interaction dynamics and properties of CnTAC surfactants. A trend was observed where longer alkyl chains lead to increased Kb values and reductions in both CMC and ΔG°, enhancing dye solubilization and interaction spontaneity. The affinity sequence of ETO to the micelles, influenced by alkyl chain length, was found to be C12TAC < C14TAC < C16TAC < C18TAC.

Comparative versatility and diverse biological applications of eco-friendly zinc oxide and cobalt oxide nanoparticles using Punica granatum L. peel extract

A fundamental element of nanotechnology today is the advancement of sustainable, environmentally friendly and economically viable approaches to green synthesis of nanomaterials. In this study, fresh aqueous extract of pomegranate peels was used as reducing and stabilizing agents in a rapid and eco-friendly approach for the synthesis of zinc oxide nanoparticles (ZnO-NPs) and cobalt oxide nanoparticles (Co3O4-NPs). X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Transmission electron microscope (TEM), Energy Dispersive Analysis of X-rays (EDX), and Fourier-transform Infrared Spectroscopy (FT-IR) were used to analyze the biosynthesized ZnO-NPs and Co3O4-NPs. XRD analysis confirmed the crystalline structures of ZnO-NPs and Co3O4-NPs as approximately 33.4 and 11.9 nm, respectively. SEM images showed distinct morphologies, while EDX and elemental mapping confirmed compositional integrity. FT-IR validated the characteristic functional groups present in both nanoparticles. TEM analysis provide the average particle size of ZnO-NPs and Co3O4-NPs were observed at 41.25 and 17.19 nm, respectively. The zeta potential of green synthesized ZnO-NPs and Co3O4-NPs were found to have a distinct peak at −12.5 and −16.3 mV, respectively. Both NPs have shown potent antimicrobial activity against four common pathogens, with increased antimicrobial activity against increasing concentrations of NPs. In vivo studies show a protective role for both ZnO-NPs and Co3O4-NPs against doxorubicin (DOX)-induced toxicity. In addition, Co3O4-NPs were effective against hepatotoxicity, nephrotoxicity, and endocrine disruption in male albino rats. Multi-technique investigation in this study offers a comprehensive understanding and indicates promising biological applications of ZnO-NPs and Co3O4-NPs.

Multi-technique investigation of silicon nitride/aluminum membranes as optical blocking filters for high-energy space missions

Multi-technique investigation of silicon nitride/aluminum membranes as optical blocking filters for high-energy space missions

Exploring the interaction between a fluorescent Ag(I)-biscarbene complex and non-canonical DNA structures: a multi-technique investigation.

Silver compounds are mainly studied as antimicrobial agents, but they also have anticancer properties, with the latter, in some cases, being better than their gold counterparts. Herein, we analyse the first example of a new Ag(I)-biscarbene that can bind non-canonical structures of DNA, more precisely G-quadruplexes (G4), with different binding signatures depending on the type of G4. Moreover, we show that this Ag-based carbene binds the i-motif DNA structure. Alternatively, its Au(I) counterpart, which was investigated for comparison, stabilises mitochondrial G4. Theoretical in silico studies elucidated the details of different binding modes depending on the geometry of G4. The two complexes showed increased cytotoxic activity compared to cisplatin, overcoming its resistance in ovarian cancer. The binding of these new drug candidates with other relevant biosubstrates was studied to afford a more complete picture of their possible targets. In particular, the Ag(I) complex preferentially binds DNA structures over RNA structures, with higher binding constants for the non-canonical nucleic acids with respect to natural calf thymus DNA. Regarding possible protein targets, its interaction with the albumin model protein BSA was also tested.

Multi-technique investigation on the surface interaction of diatomaceous earth with organic phase change material: Experimental and molecular dynamics aspects

To promote diatomaceous earth (DE)-based phase change composite as green energy building materials, this paper bridges the studies of experimental and molecular dynamics (MD) focusing on the absorption effect of phase change materials (PCMs). Octadecanoic acid (OA) was selected as PCMs and DE as supporting material for the fabrication of composite PCMs at different loading ratios; effect on thermal properties and porosity of the composite PCMs were further investigated by MD simulation. In consonance with ATR-FTIR and XRD analyses, the highest loading ratio (DEOA-4) was proven to absorb a high amount of PCMs, with excellent thermal stability and chemical compatibility. DEOA-4 exhibited higher latent heat storage capacity of 52.67 J/g, with a loading ratio and loading efficiency of 32.13 and 32.98 %. Besides, MD simulation showed that increasing the OA loading would decrease the fractional free volume of DEOA models, resulting in a limited mobility of PCMs molecules, as confirmed by self-diffusion coefficient at room and melting temperatures. Experimental and computational studies revealed that pore-filling process plays an imperative role during PCMs absorption. An adequate amount of loading ratio can potentially enhance the pore-filling process, maximize the efficiency of the performances, and promote the development of green energy in concrete structures.

Interplay between coordination sphere engineering and properties of nickel diketonate-diamine complexes as vapor phase precursors for the growth of NiO thin films.

NiO-based films and nanostructured materials have received increasing attention for a variety of technological applications. Among the possible strategies for their fabrication, atomic layer deposition (ALD) and chemical vapor deposition (CVD), featuring manifold advantages of technological interest, represent appealing molecule-to-material routes for which a rational precursor design is a critical step. In this context, the present study is focused on the coordination sphere engineering of three heteroleptic Ni(II) β-diketonate-diamine adducts of general formula [NiL2TMEDA] [L = 1,1,1-trifluoro-2,4-pentanedionate (tfa), 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedionate (fod) or 2,2,6,6-tetramethyl-3,5-heptanedionate (thd), and TMEDA = N,N,N',N'-tetramethylethylenediamine]. Controlled variations in the diketonate structure are pursued to investigate the influence of steric hindrance and fluorination degree on the chemico-physical characteristics of the compounds. A multi-technique investigation supported by density functional calculations highlights that all complexes are air-insensitive and monomeric and that their thermal properties and fragmentation patterns are directly dependent on functional groups in the diketonate ligands. Preliminary thermal CVD experiments demonstrate the precursors' suitability for the obtainment of NiO films endowed with flat and homogeneous surfaces, paving the way to future implementation for CVD end-uses.

Experimental and density functional theory studies of laminar double-oxidized graphene oxide nanofiltration membranes

The type and loading level of oxygen-containing functional groups on graphene oxide (GO) nanosheets significantly affect the size and alignment of nanochannels formed between the GO nanosheets and the separation performance of laminar GO membranes. Here, we demonstrate how double-oxidation of GO leads to the higher surface charge of GO nanosheets, the formation of highly stable water-based GO solution, more-ordered deposition of GOs on the polyethersulfone membrane through the pressure-assisted self-assembly method, and the formation of highly durable GO membranes possessing smoother surface morphology and higher antifouling properties. A multi-technique investigation was applied to follow the physicochemical difference between GO and double-oxidized GO, and the physical stability and separation performance of the corresponding membranes using experimental and computational studies. The double-oxidized GO-based membranes provided a significantly high water flux of 230 L/(m2.h) in 2.5 bar transmembrane pressure, excellent rejection of 99.9% for methylene blue (MB) dye, and outstanding separation performance stability over time. In contrast, GO membranes showed rejection of 81.5% for MB, and their separation performance diminished significantly over time. The antifouling properties of double-oxidized GO membranes were substantially higher (∼ four times) due to their higher negative surface charge and smoother surface morphology. The density functional theory (DFT) was used to gain insight into the interactions between the functional groups and the reasoning for the higher mechanical stability of double-oxidized GO membranes. Results revealed that the formation energy of GO decreases by increasing the number density of functional groups. It was also found that a higher number of carboxyl groups at the edges of the double-oxidized GO leads to higher hydrogen bonding, higher binding energy, and a more stable GO-membrane structure.

Early-age reactivity of calcined kaolinitic clays in LC3 cements: a multitechnique investigation including pair distribution function analysis

Limestone Calcined Clay Cements, LC3, allows CO2 emissions savings up to 40%. The resulting binders have competitive mechanical performances after a week. However, the reactivity of LC3 at early ages is slow and should be improved. Here, we use a multitechnique approach to help in the understanding of early age reactivities which were measured by calorimetry, Frattini assay, and mechanical strengths. The disorder in the kaolinites was quantified by powder diffraction. Some footprints of the local disorder in the resulting metakaolin have been investigated by synchrotron pair distribution function (sPDF). It is concluded that Al-O interatomic correlation position and intensity in the sPDF of the calcined kaolinitic clays could be an additional good descriptor to follow early age reactivity. The results were complemented by 27Al MAS-NMR studies. The rate of the pozzolanic reaction at early ages is governed by the particle size, surface area, and local disorder of metakaolin.

Elucidation of LMCT Excited States for Lanthanoid Complexes: A Theoretical and Solid-State Experimental Framework.

Photophysical and magnetic properties arising from both ground and excited states of lanthanoid ions are relevant for numerous applications. These properties can be substantially affected, both adversely and beneficially, by ligand-to-metal charge-transfer (LMCT) states. However, probing LMCT states remains a significant challenge in f-block chemistry, particularly in the solid state. Intriguingly, the europium compounds [EuIII(18-c-6)(X4Cat)(NO3)]·MeCN (18-c-6 = 18-crown-6; X = Cl (tetrachlorocatecholate, 1-Eu) or Br (tetrabromocatecholate, 2-Eu) are distinctly darkly-colored, in marked contrast to the analogues with other lanthanoid ions in the 1-Ln and 2-Ln series (Ln = La, Ce, Nd, Gd, Tb, and Dy). Herein, we report a multi-technique investigation of these compounds that has allowed elucidation of the LMCT character of the relevant absorption bands using magnetometry, absorption and emission spectroscopies, and solid-state electrochemistry. To support experimental observations, we present a semi-quantitative multireference ab initio model that (i) captures the anomalously low-lying LMCT excited state observed in the visible spectrum of 1-Eu (and its absence in the other 1-Ln analogues); (ii) elucidates the contribution of the LMCT excitation to the crystal field split 7FJ ground-state wave functions; and (iii) identifies the crucial role played by radial dynamical correlation of the EuIII 4f electrons in the description of the LMCT excited state, modeled by the inclusion of 4f → 5f excitations in the optimized wave function. By providing a set of experimental and theoretical tools, this work establishes a framework for the elucidation of LMCT excited states in lanthanoid compounds in the solid state.

Composition triggered Aggregation/Solubilization behaviour of mixed counter charged gemini Surfactants: A Multi-technique investigations

• Fluorescence parameters can be used to detect the interaction between counter charged geminis. • Composition variation modulates the apparent dielectric constant of the mixed micelle. • Mixing can tune micelles of different architectures which further depend on spacer nature. • Zeta (ζ) values show charge reversal during composition variation. • A correlation has been proposed for the dependence of MSR on the micellar environment- morphology- composition. Aqueous association behaviour of counter charged gemini surfactants has been studied by fluorometry, dynamic light scattering (DLS), Zeta(ζ)-potential and SANS measurements at 303 K. For the purpose, P, P'-1,4-butanedieyl, P, P'-didodecylester, disodium salt, anionic surfactant(12–4-12A) and cationic gemini surfactants: Butanediyl-1,4-bis (N, N-dimethyl-N-tetradecyl-ammonium) dibromide (14–4–14); Ethane-1,2-diyl bis (N, N-dimethyl-N-tetradecyl-ammonium acetoxy) dichloride (14-Eg-14) and (D-isosorbate-1,4-diyl bis (N, N-dimethyl-N-tetradecylammonium acetoxy) dichloride (14-Isb-14) were mixed for varying mole fraction range ( x = 0–1). Fluorescence data using pyrene as a probe are used to obtain CMC values which were theoretically treated using regular solution theories. It has been observed that mixing causes non spherical micelles and even vesicle formation was observed in one of the combinations (12–4-12A + 14–4–14) at x = 0.4. Various compositions are used to solubilize polycyclic aromatic hydrocarbon (pyrene, anthracene and phenanthrene) in order to have an idea of solubility enhancement efficacy. Micellar morphology/environment has been used to draw a correlation between apparent dielectric constant (D exp ) - composition - solubilization potential. Findings can be used for loading various hydrophobic materials in an appropriate amphiphilic mixture for various applications such as dye solubilization, drug solubilization, drug delivery or drug targeting.

Compositional and spectroscopic investigation of three ungrouped carbonaceous chondrites

AbstractUngrouped carbonaceous chondrites are not easily classified into one of the well‐established groups due to compositional/petrological differences and geochemical anomalies. Type 2 ungrouped carbonaceous chondrites represent a very small fraction of all carbonaceous chondrites. They can potentially represent different aspects of asteroids and their regolith material. By conducting a multitechnique investigation, we show that Queen Alexandra Range (QUE) 99038 and Elephant Moraine (EET) 83226 do not resemble type 2 carbonaceous chondrites. QUE 99038 exhibits coarse‐grained matrix, Fe‐rich rims on olivines, and an apparent lack of tochilinite, suggesting that QUE 99038 has been metamorphosed. Its polyaromatic organic matter structures closely resemble oxidized CV3 chondrites. EET 83226 exhibits a clastic texture with high porosity and shows similarities to CO3 chondrites. It consists of numerous large chondrules with fine‐grained rims that are often fragmented and discontinuous and set within matrix, suggesting a formation mechanism for the rims in a regolith environment. The kind of processes that can result in such chemical compositions as in QUE 99038 and EET 83226 is currently not fully known and clearly presents a conundrum. Tarda is a highly friable carbonaceous chondrite with close resemblance to Tagish Lake (ungrouped C2 chondrite). It comprises different types of chondrules (some with Fe‐rich rims), framboid magnetite, sulfides, carbonates, and phyllosilicate‐ and carbon‐rich matrix, and is consistent with being an ungrouped C2 chondrite.

Effect of rice husk ash on carbon sequestration, mechanical property and microstructure evolution of cement-based materials with early-age carbonation treatment

Recycling of agricultural wastes to develop low-carbon supplementary cementitious materials requires the understanding of their effects on carbon sequestration, mechanical property and microstructure characteristics of cement-based materials. This work aims to disclose the mechanism of above-mentioned behavior in porous-structured rice husk ash (RHA) blended pastes using multi-technique investigations including mercury intrusion porosimetry (MIP), 29Si magic angle spinning nuclear magnetic resonance (29Si MAS NMR), Scanning electron microscope/Energy Dispersive Spectrometer (SEM/EDS) techniques coupled with carbonation-hydration model. It was discovered that pastes with increased dosages of RHA (5%–15%) presented an increase of CO2 uptake compared to that of control paste. It also showed an enhanced compressive strength after 12 h carbonation while simultaneously maintained a comparable strength development at 28 d. A declined permeability from water absorption experiment was also obtained especially in carbonated paste with 10% RHA. The enhanced polymerization degree of C–S–H and the decreased porosity due to the formation of calcite were the main contributors to the improved performances in RHA blended pastes.

A Multi-Technique Investigation of the Complex Formation Equilibria between Bis-Deferiprone Derivatives and Oxidovanadium (IV).

The increasing biomedical interest in high-stability oxidovanadium(IV) complexes with hydroxypyridinone ligands leads us to investigate the complex formation equilibria of VIVO2+ ion with a tetradentate ligand, named KC21, which contains two 3-hydroxy-1,2-dimethylpyridin-4(1H)-one (deferiprone) moieties, and with the simple bidentate ligand that constitutes the basic unit of KC21, for comparison, named L5. These equilibrium studies were conducted with joined potentiometric–spectrophotometric titrations, and the results were substantiated with EPR measurements at variable pH values. This multi-technique study gave evidence of the formation of an extremely stable 1:1 complex between KC21 and oxidovanadium(IV) at a physiological pH, which could find promising pharmacological applications.

Multi-technique investigation regarding the impact of cellulose nanofibers on ultra-high-performance concrete at the macroscopic and microscopic levels

Cellulose nanofibers (CNFs) are renewable building materials with excellent potential for development. In this paper, we present a multi-technique study of the properties of samples with CNF addition at the macroscopic and microscopic levels. The hydration kinetics, autogenous shrinkage, microstructure, mechanical properties, and durability of the samples were investigated. The results are as follows: (1) CNFs suppress early hydration and accelerate later hydration. (2) The autogenous shrinkage decreased considerably with an increase in added CNFs. (3) Thermogravimetric analysis revealed that as the CNFs content increased, the combined water and calcium hydroxide content increased. X-ray diffraction and attenuated total reflection–Fourier transform infrared experiments revealed the calcium hydroxide content in the hydration products was low. (4) SEM tests revealed fiber pull-out, hydration product attachment on the CNFs surface, and fiber pocket formation in specimens with 0.3% CNF. (5) A two-aspect effect of CNFs on compressive strength was observed, namely an increase followed by a decrease. The final strength change depends on the amount of CNFs added and the high strength of the CNFs. (6) The addition of 0.1% CNFs refined the pore structure and improved the electrical resistivity. When CNFs were added in excess, the porosity increased and the resistivity decreased.

Multi-Technique Diagnostic Investigation in View of the Restoration of “The Glory of St. Barbara” Painting by Mattia Preti

The present paper illustrates the results of a diagnostic investigation performed on the oil on canvas painting “The Glory of St. Barbara” (1680–1688) by Mattia Preti. The painting is located inside the St. Barbara Church in Taverna (Catanzaro, Italy), the city that gave birth to the artist. In situ, non-invasive studies, by applying X-ray fluorescence (XRF) spectroscopy, along with laboratory micro-destructive analytical investigations, by employing electron probe microanalyses (EPMA) coupled with energy-dispersive spectrometry (EDS) and micro-Raman (µ-Raman) spectroscopy, were combined to retrieve the color palette and identify the painting technique and style of the famous master. As a result of this multi-scale characterization, an extraordinary pictorial technique was revealed, enriching knowledge about one of the oldest pictorial traditions outlined by Mattia Preti, and solving doubts still existing about many of his investigated artworks. Moreover, the achieved results represent useful and essential tools to address management issues of the artwork, by providing valuable information for planning and monitoring future restoration interventions of the canvas.

Hydration and microstructure of glass powder cement pastes – A multi-technique investigation

The industrial adoption of new supplementary cementitious materials requires the understanding of their effects on the hydration and on the long-term properties of concrete, in order to adapt design and construction methods. Although the evolution of properties differs from that of Portland cement systems, the constructability of glass powder (GP) blended-cement systems was found to be maintained (i.e., similar 2-day strength) and gains were observed in the long-term performances (i.e., similar strength but higher resistivity, suggesting higher durability). This paper aims to understand and describe the mechanisms responsible for these behaviours using a multi-technique investigation approach (calorimetry, XRD-Rietveld-PONKCS, thermodynamic modelling, quantitative chemical analyses, and more). The results disclose the chemo-physical effects of GP on early age hydration kinetics, the impact of cement dilution on phase assemblage, and the long-term pozzolanic reaction of GP leading to C-S-H with a lower calcium content, a higher alkali uptake and a refined porosity.

Multitechnique investigation of concrete with coal gangue

Although the research of coal gangue as construction aggregate has been conducted for many years, the fundamental knowledge about the links between the microscopic properties of coal gangue and the macroscopic properties of concrete has not been discovered yet. In this paper, gravel was entirely replaced by coal gangue to improve the utilization rate. The compressive strength, fluidity, and compactness of concrete were studied to explore the macro performance of coal gangue concrete (CGC). Meanwhile, mercury intrusion porosimeter (MIP), scanning electron microscope (SEM), and nanoindentation were used to comprehensively analyze the pore structure, morphology, and micromechanical properties of coal gangue as aggregate. The experimental results showed that coal gangue has a hierarchical structure, wide pore distribution, and poor mechanical properties in microcosmic. Compared with ordinary concrete (OC), both the fluidity and compressive strength of CGC were lower. However, due to the large porosity and water absorption of coal gangue, the bonding surface between coal gangue and cement was denser, which makes the overall compactness of CGC better than OC. The width of the interface transition zone (ITZ) of CGC did not change significantly with the water-cement ratio (w/c), while that of OC did. When w/c was greater than 0.4, the compressive strength of CGC was only about 10% lower than that of OC. The pore structure and micromechanical properties of coal gangue determined the compactness and strength of CGC.

Multi-Technique Investigation of Grave Robes from 17th and 18th Century Crypts Using Combined Spectroscopic, Spectrometric Techniques, and New-Generation Sequencing.

The textile fragments of the funeral clothes found in the 17th and 18th century crypts were subjected to spectroscopic, spectrometric, and microbial investigation. The next-generation sequencing enabled DNA identification of microorganisms at the genus and in five cases to the species level. The soft hydrofluoric acid extraction method was optimized to isolate different classes of dyes from samples that had direct contact with human remains. High-performance liquid chromatography coupled with diode matrix and tandem mass spectrometry detectors with electrospray ionization (HPLC-DAD-ESI-MS/MS) enabled the detection and identification of 34 colourants that are present in historical textiles. Some of them are thus far unknown and uncommon dyes. Indigo, madder, cochineal, turmeric, tannin-producing plant, and young fustic were identified as sources of dyes in textiles. Scanning electron microscopy with energy-dispersive X-ray detector (SEM-EDS) and Fourier transform infrared spectroscopy (FT-IR) were used to identify and characterize fibres and mordants in funeral gowns. Of the 23 textile samples tested, 19 were silk while the remaining four were recognized as wool. The presence of iron, aluminium, sodium, and calcium suggests that they were used as mordants. Traces of copper, silica, and magnesium might originate from the contaminants. The large amount of silver indicated the presence of metal wire in one of the dyed silk textiles. SEM images showed that textile fibres were highly degraded.

Multi technique investigation on interaction between 5-(2-thiazolylazo)-2,4,6-triaminopyrimidine and HSA and BSA

In research laboratories and in various industries, azo compounds are among the most effective and commonly used organic dyes. The association between human (HSA) and bovine (BSA) serum albumins with 5-(2-thiazolylazo)-2,4,6-triaminopyrimidine (TTP) was investigated in this research using spectroscopy methods and molecular modeling study. The fluorescence quenching results showed that the quenching mechanisms were static and dynamic processes for HSA and BSA, respectively. From the thermodynamic observations, it is clear that the binding process is a spontaneous molecular interaction, in which van der Waals and hydrogen bonding interactions for HSA and hydrophobic interaction for BSA play the major roles. According to Förster energy transfer, non-radiative energy transferred from HSA and BSA to TTP, is provided by close distance (r 0) between TTP and Trp residues of HSA and BSA. The synchronous fluorescence spectroscopy, FT-IR findings and UV-Vis absorption data confirm that TTP can induce conformational and micro environmental changes in both the proteins. Furthermore, docking results predicted the probable binding site of TTP in subdomain IIA of HSA and BSA molecules where Trp residues are located. Types of amino acid residues surrounding the TTP molecule supported that van der Waals forces, hydrophobic forces and electrostatic forces play important roles in stabilization of drug-protein complexes formed. Communicated by Ramaswamy H. Sarma

Multi-technique investigation of Ni-doped ZnO thin films on sapphire by metalorganic chemical vapor deposition

Optical and material properties of nickel-doped zinc oxide (ZnO-Ni) grown by metalorganic chemical vapor deposition with varying Ni source flow rates are investigated. ZnO-Ni showed a good crystal quality with (002) orientation but deteriorated at high Ni source flow rates. Photoluminescence responses show a reduction in the bandgap of ZnO-Ni with an increase in the Ni source flow and also with an increase in the temperature. Ni-doping can enhance luminescences at low concentrations (&amp;lt;25 SCCM and ∼2%) and suppress at high concentrations. Ni-related defects occur more toward the surface than bulk of the thin films. Longitudinal optical phonon replicas named 1LO and 2LO redshifts at low Ni source flow rates ≤100 SCCM with an increase in the temperature from 14 to 300 K, but exhibits an “S-shaped” red-blue-red shift with a dip at 50 K at higher Ni source flow rates (150 SCCM). Ni-doping also induces asymmetric crystal vibrations and rougher surfaces with the Ni incorporation. This study enhances the understanding of Ni-doped ZnO that is needed to apply transition-metal doped ZnO for various optoelectronic applications.