Vickers Microhardness Studies Research Articles

Synthesis, growth and characterization of nonlinear optical organic crystal: 4-Methoxy Anilinium 5-Sulfo Salicylate

Quality crystals of 4-Methoxy Anilinium 5-Sulfo Salicylate (4MA5SS) were grown with the dimension of 9 mm × 6 mm × 3 mm from ethanol solution by slow evaporation solution growth technique. The cell parameters and crystal structure studied by single-crystal X-ray diffraction. FTIR spectroscopic studies were carried out to confirm the functional groups and vibrational modes present in the grown crystals. The linear optical properties of the grown crystal were studied from the UV–Vis spectrum. The surface laser damage threshold for the grown crystal was measured using Nd:YAG laser. Further, Vickers micro-hardness study was carried out to analyze the mechanical strength of the grown crystals for various loads. The dielectric measurements of this crystal in the frequency region from 50 Hz to 5 MHz showed that the material can be used for optical application.

Synthesis, growth and characterization of organic crystal triphenylmethane p-nitroaniline: a nonlinear optical crystal

Abstract A triphenylmethane-4-nitroaniline salt has been synthesized and the crystals have been grown by using slow evaporation solution growth technique. The grown single crystal was investigated by recording the powder XRD, FT-IR spectrum, UV-Vis spectrum, Vickers microhardness test, dielectric measurements and powder SHG. The growth of crystal was confirmed by analyzing the XRD pattern and it was stated that the grown material crystallized in triclinic system. Vibrational peaks of the functional groups existing in the compound were identified. Vickers microhardness studies were carried to measure the mechanical strength. In order to identify the phase transition temperature, the dielectric studies were carried out at different temperatures. Dielectric constant, dielectric loss and impedance of the crystal were monitored with respect to the frequency of electric field.

Synthesis, optical, experimental and theoretical investigation of third order nonlinear optical properties of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate single crystal

Single crystals of 8-hydroxyquinolinium 2-carboxy-6-nitrophthalate monohydrate (8HQNP) were obtained from slow evaporation solution growth method using methanol-water (1:1) as a solvent. Powder X-ray diffraction was utilized to compute the unit cell parameters and dislocation density of 8HQNP crystal. The crystalline perfection of the as-grown crystal was investigated by high-resolution X-ray diffraction at room temperature. The molecular structure was analyzed by identifying the functional groups from FT-IR and FT-Raman spectra. The cut-off wavelength and the corresponding optical band gap obtained from an optical spectrum were 376 nm and 3.29 eV respectively. The dispersion nature of refractive index was investigated by the single-oscillator Wemple and Di-Domenico model. Red emission was observed in the photoluminescence spectrum when excited with 376 nm. The low birefringence and high laser damage threshold (8.538 GW/cm2) values dictate the suitability of the crystal for optical devices. Z-scan studies revealed the third order nonlinear absorption coefficient (β) and refractive index (n2) of the 8HQNP crystal. The theoretical value of third order nonlinear susceptibility obtained from density function theory is good accordance with the experimental value. The frontier molecular orbital energy gap decreases with increasing external electric field in different directions which attributed to the enhancement of the second hyperpolarizability. The grown title crystal is thermally stable up to 102 °C which was identified using thermal analysis. Mechanical strength of 8HQNP was estimated by using Vicker's microhardness studies.

Studies on structure, growth and characterization of third order nonlinear optical 2-amino-5-chloropyridinium-4-amino benzoate single crystal

AbstractOptically transparent single crystals of 2-amino-5-chloropyridinium-4-amino benzoate (2A5CP4AB) were grown at room temperature using solution growth technique. The structure was solved with a support of single crystal XRD, which revealed that the title compound belongs to the monoclinic crystal system having centrosymmetric space group P21/n. The UV-Vis spectrum and photoluminescence properties of the title compound showed the optical transmittance and emission behavior of the compound. The optical band gap was evaluated using the Tauc plot and it was found to be about 3.53 eV. The third order nonlinear optical behavior of the crystal was determined using Z-scan technique. Mechanical properties of the title compound were studied using Vickers microhardness study.

Synthesis, structural, thermal, mechanical, second harmonic generation efficiency and laser damage threshold studies of 4-dimethylaminopyridinium-3,5-dicarboxybenzoate trihydrate single crystal

4-dimethylaminopyridinium-3,5-dicarboxybenzoate trihydrate was synthesized and single crystals grown by slow solvent evaporation solution growth technique at ambient temperature. The single crystal XRD analysis was carried out to establish the molecular structure of the title crystal. Further, the data indicate that the title salt crystallizes in orthorhombic crystal system with the non-centrosymmetric space group, Pna21. The established molecular structure was further confirmed by 1H and 13C NMR spectroscopic studies. The grown crystal has been subjected to FT-IR spectral study to identify the various functional groups. The UV–Vis–NIR transmission spectrum was recorded on powdered sample of crystal to determine the lower wavelength cut-off and optical band gap. The photoluminescence spectrum was recorded to investigate the luminescence properties of the salt crystal. The thermal and mechanical stabilities of the crystal were established by TG/DTA analyses and Vickers microhardness study, respectively. The dielectric studies of the grown crystal were executed at different temperatures as a function of frequency to investigate its electrical properties. The SHG efficiency of the title crystal was investigated and its value is 0.89 times that of KDP crystal. The laser damage threshold value is found to be 1.06 GW/cm2.

Laser induced optical and microscopic studies of salicylic acid influenced KH2PO4 crystal for photonic device applications

The present communication is aimed to explore the characteristic properties of salicylic acid (SA) doped potassium dihydrogen orthophosphate (KDOP) crystal. The single SA doped KDOP crystal with optimum dimension of 10 × 08 × 04 mm3 has been grown from solution by slow evaporation at ambient temperature. The single crystal X-ray diffraction analysis has been employed to determine the structure and cell parameters of grown crystal. The Z-scan studies have been carried out at 632.8 nm to ascertain the influential third-order non-linear optical (TONLO) nature of SA doped KDOP crystal. The Z-scan transmittance data have been used to determine the magnitude of TONLO susceptibility (χ3), absorption coefficient (β) and refractive index (n2) of SA doped KDOP crystal. For grown crystal, the surface damage due to exposure of high intensity of Nd:YAG laser operating at 1064 nm has been determined and found of order MW cm−2. The growth tendency, etch pattern and surface quality of grown SA doped KDOP crystal has been investigated by means of etching studies. The thermal response of grown crystal has been examined by differential thermal analysis employed in the range of 23–800°C. The hardness number of SA doped KDOP crystal has been investigated by means of Vickers microhardness study by applying different load ranging from 25 to 100 gm. The work hardening index and elastic stiffness coefficient have been evaluated using the hardness data. The nature of photoconductivity exhibited by grown crystal has been determined in voltage range of 10–100 V.Highlights• Z-scan analysis revealed negative non-linear refraction and reverse saturable absorption effect in SA-KDOP crystal.• The laser damage threshold of SA-KDOP crystal at 1064 nm is found to be 274·74 MWcm−2.• SA-KDOP crystal exhibited positive photoconducting nature within 10–100 V.• The dopant SA facilitated large enhancement in hardness parameters of KDOP crystal.• Etching and thermal analysis has been performed.

Synthesis, structural, thermal and mechanical properties of 1,10-phenanthrolinium-3-carboxy-4-hydroxy benzene sulphonate crystal: An efficient SHG material with a high laser damage threshold for NLO applications

Nonlinear optical material, 1,10-phenanthrolinium-3-carboxy-4-hydroxy benzene sulphonate (PCHBS) has been synthesized and single crystals grown by slow solvent evaporation solution growth technique in methanol as the solvent. The 1H and 13C NMR spectra were recorded to establish the molecular structure. The single crystal XRD analysis reveals that the title salt crystallizes in monoclinic crystal system with non-centrosymmetric space group, P21. The presence of various functional groups was confirmed by FT-IR spectroscopic studies. The UV–vis-NIR was recorded in the range 200–1200nm to find the optical transmittance window, lower cut off wavelength and optical band gap. The thermal and mechanical properties were estimated by TG/DTA analysis and Vickers microhardness study, respectively. The SHG efficiency of title crystal was measured by employing modified Kurtz and Perry powder technique. Further, the laser damage threshold value has been determined using a Q-switched Nd:YAG laser operating at 1064nm.

Vickers Microhardness Studies of Pure and Amino Acids Doped Potassium Dihydrogen Phosphate Crystals

Vickers microhardness study was carried out to understand the mechanical behaviour of pure and different amino acids (L-arginine, L-lysine, L-alanine) doped potassium dihydrogen phosphate (KDP) single crystals grown by slow solvent evaporation technique. Indentations were made on smooth {100} plane of pure and different amino acid doped crystals for loads varying from 0.298 N to 0.98 N. Vickers microhardness decreased as doping level of amino acid was increased. Indentation size effect (ISE), Kick's law, Hays and Kendall's law and Proportion specimen resistance (PSR) model were verified for pure and different amino acids doped crystals. The values of the load independent hardness and Newtonian pressure were higher in pure KDP crystals than the amino acids doped KDP crystals. It was found that as doping concentration of amino acids increased the load independent hardness and Newtonian pressure decreased. The results indicated that the doping of amino acids made KDP crystals softer.

Growth and physical characterization of organic nonlinear optical single crystal: N,N′-diphenylguanidinium formate

A second-harmonic generation (SHG) crystal N,N′-diphenylguanidinium formate (DPGF) with good quality was successfully grown by the slow evaporation method. Single crystal X-ray diffraction study confirms that the DPGF crystallizes in orthorhombic crystal system with space group P21cn. The powder XRD pattern shows the various planes of DPGF crystal. The 1H and 13C NMR spectral studies further confirm the molecular structure of the grown crystal. The various functional groups present in the grown crystal have been identified by Fourier transform infrared spectroscopy. The UV–vis–NIR spectrum was recorded to find the optical transmittance window, lower cut off wavelength and band gap of the DPGF crystal. Photoluminescence spectrum shows broad emission peak observed at 367nm. Thermal stability of the title crystal was evaluated by thermogravimetric (TG) and differential thermal analysis. Vicker's microhardness study was carried out to reveal the mechanical properties of the grown crystal. The second harmonic conversion efficiency of DPGF crystal was 1.8 times than that of KDP crystal. Gaussian 03W program has been used to calculate the molecular orbital and first order hyperpolarizability of the molecule. The calculated first order hyperpolarizability value of DPGF is found to be 16 times greater than that of urea.

Growth and characterization of α-nickel sulphate hexahydrate single crystal

Single crystal of α-nickel sulphate hexahydrate, α-NiSO4. 6H2O (α-NSH) is grown from aqueous solution by slow evaporation method. Solubility and metastable zone width of α-NSH are determined from the aqueous solution. The three dimensional structure is elucidated by single crystal X-ray diffraction studies. The α-NSH crystallizes in the non – centrosymmetric tetragonal space group P41212. The relative contributions of various intermolecular interactions involved in the crystal structure are quantified using Hirshfeld surface analysis and the decomposed two dimensional fingerprint plots. Fourier transform infrared spectral analysis and Vickers microhardness studies are carried out to characterize the grown crystal. Further the grown crystals are characterized using TGA, DSC, UV–Vis–NIR and dielectric analysis. The third order nonlinear optical properties are studied by Z–scan technique with HeNe laser radiation of wavelength 632.8 nm and the corresponding nonlinear refractive index, absorption coefficient and optical susceptibility are calculated. Crystalline perfection is assessed by etching studies and laser damage threshold is observed for the grown crystal.

Growth, spectral, optical, thermal, and mechanical behaviour of an organic single crystal: Quinolinium 2-carboxy 6-nitrophthalate monohydrate

Organic single crystals of quinolinium 2-carboxy 6-nitrophthalate monohydrate (QN) were grown by slow evaporation solution growth technique using ethanol and water as a mixed solvent. X-ray powder diffraction analysis revealed that the crystal belongs to the monoclinic crystal system with space group of P21/c. The functional groups present in the crystallized material confirmed its molecular structure. The optical transparency range and the lower cutoff wavelength were identified from the UV–vis spectrum. The optical constants were determined by UV–visible transmission spectrum at normal incidence, measured over the 200–700nm spectral range. The dispersion of the refractive index was discussed in terms of the single-oscillator Wemple and DiDomenico model. The calculated HOMO and LUMO energies show that the charge transfer occur within the molecule. Electronic excitation properties were discussed within the framework of two level model on the basis of an orbital analysis. The nonlinear optical absorption coefficient (β) and nonlinear refraction (n2) of QN was measured by Z-scan technique and reported here. Thermal stability of QN was determined using TGA/DSC curves. Vicker's microhardness studies were carried out on the (11̅0) plane to understand the mechanical properties of the grown crystal. The microhardness measurements showed a Vickers hardness value as 18.4kg/mm2 which is comparable to well-known organic crystal, urea.

Growth, hardness and laser damage threshold studies on vertical Bridgman grown piperine (PPN) single crystal

An organic piperine (PPN) single crystal was grown using vertical Bridgman technique. The diffraction planes have been indexed from powder X-ray diffraction analysis. Vickers microhardness studies were carried out on grown PPN crystal with various load ranging from 10 to 100 g. Reverse indentation size effect (RISE) is observed from the microhardness measurements. The meyer index value (n) was found to be greater than 1.6 which indicates the grown crystal belongs to soft-material category. The stiffness constant (C11) was computed using the Wooster’s empirical relation. Laser damage threshold studies have been carried out using Q-switched Nd: YAG laser. All the results are discussed in detail.

Growth, structural, UV–visible, SHG, mechanical and dielectric studies of bis-thiourea zinc chloride doped KDP crystal for NLO device applications

Optically transparent 11 × 10 × 4 mm3 bis-thiourea zinc chloride (BTZC) doped potassium dihydrogen phosphate (KDP) crystal has been grown by slow evaporation solution technique. The cell parameters of the grown crystal have been determined by single crystal X-ray diffraction analysis. The incorporation of BTZC in KDP crystal has been qualitatively analysed by FT-IR spectral analysis. The optical transparency and vital optical constants of BTZC doped KDP single crystals have been evaluated in the range of 200–900 nm. The mechanical behaviour of pure and doped KDP crystals has been investigated under the Vickers microhardness studies. The dielectric parameters of grown crystal have been investigated within the frequency range of 10–100 KHz. In Kurtz–Perry powder test, the second harmonic generation (SHG) efficiency of BTZC doped KDP crystal is found to be 1.65 times that of KDP material.

Synthesis, growth, optical and mechanical studies of ferroelectric urea-oxalic acid single crystals

A single crystal of urea oxalic acid was grown by slow evaporation method. The lattice parameters are a=5.13Å, b=12.48Å, c=7.07Å, β=98.13° with V=448.5Å3 which belongs to monoclinic system with space group P21/c obtained from single crystal X-ray diffraction analysis. UV–visible spectrum was recorded from the wavelength region of 200–800nm and its cutoff wavelength was found to be 270nm. Optical energy band gap of 4.57eV was determined using Tau's plot relation. Fourier transform infrared vibrational spectrum confirmed the presence of N–H asymmetric stretching which occurs at 3444cm−1 and 1853cm−1 arising due to the amide C=O symmetric stretching. The emission was observed at 364nm from the photoluminescence spectrum. The mechanical stability of the grown crystal was estimated by Vickers microhardness studies and it is evident that the grown crystal belongs to soft material category. Hardness related parameters such as elastic stiffness constant, fracture mechanics, brittleness index and yield strength were also evaluated. The dielectric constant and dielectric loss of the grown crystal were carried out as a function of frequency for different temperatures.

Growth and characterisation of l-lysine hydrochlorobromide (LYHCBr), a novel semiorganic non-linear optical (NLO) single crystal

A novel semiorganic non-linear optical crystal, l-lysine hydrochlorobromide (LYHCBr) dimensions of 1 × 0.2 × 0.2 cm was grown by deionised water by the conventional method. l-lysine hydrochlorobromide crystallises in non-centrosymmetric orthorhombic crystal system with space group P212121.FTIR spectrum analysis was examined to assign the functional groups of the grown crystal. The optical study shows that the crystal has lower UV cutoff wavelength at 208 nm. Thermal analysis confirms that the crystal is stable up to 244.8°C. The dielectric constant and dielectric loss of the grown crystal were determined at various temperatures in the frequency range of 100 Hz to 1 MHz. The mechanical property of the grown crystals was analysed through Vickers microhardness study. The positive photoconducting nature of the sample was verified by photoconductivity study. The Kurtz–Perry second harmonic generation (SHG) study revealed that the efficiency of LYHCBr is 1.91 times higher than that of KDP.

Structure, growth and characterization of picolinium perchlorate single crystals

Picolinium perchlorate organic single crystals were grown using slow evaporation solution growth technique at room temperature using water as a solvent. The structure of the title compound was supported by proton NMR analysis and the single crystal X-ray diffraction data. Crystallographic studies revealed that the compound crystallized in monoclinic system with space group C2/c. The HRXRD rocking curve measurements revealed the crystalline perfection of grown crystal. First order hyperpolarizability, HOMO and LUMO energies are calculated using Density Functional Theory (DFT) with a hybrid functional B3LYP and the 6-311++G(d,p) basis set. Global reactivity indices are calculated. Thermal studies were carried out on the title compound. The UV–vis–NIR spectrum was recorded to study the optical transparency of the grown crystals. The mechanical stability of the crystal was analyzed by Vicker's microhardness studies.

Effects of 1,2-dichloroethane on the optical, thermal, mechanical and NLO behaviors of ADP crystals

The effects of 1,2-Dichloroethane (DCE) over a concentration range from 1 to 5mol% on the optical absorption, hardness, thermal, microhardness behaviors and SHG efficiency of ammonium dihydrogen phosphate (ADP) single crystals grown by slow evaporation solution growth technique have been investigated. The powder X-ray diffraction and FT-IR analyses indicate that the crystals undergo considerable stress as a result of doping and these also confirm the slight distortion of the structure of the crystal in the presence of a high concentration of dopant (5mol%). UV–vis studies reveal that the absorption of the DCE doped crystals is less than that of pure ADP. Thermal studies (TG/DTG) disclose that the decomposition temperature of doped ADP is more than that of pure ADP. Vicker's microhardness study reveals that the addition of DCE increases the hardness of the ADP. SHG efficiency of DCE doped ADP is higher than that of pure ADP. Presence of dopant was confirmed by energy-dispersive spectrometry.

Vickers microhardness studies on Cobalt Mercury Thiocyanate single crystals grown in silica gel

Vickers microhardness study was carried for the gel-grown Cobalt Mercury Thiocyanate single crystal, subjected to the loads 10, 25, 50 and 100g. Vickers hardness number Hv was calculated and it is found to increase with the applied load. Mayer's index number ‘n’ and elastic stiffness constant were calculated. The results are discussed in detail.

Structural, topographical, linear and non linear optical, electrical and mechanical properties of pure and barium @ amino hydrogen chloride monohydrate single crystal by Slow Evaporation Solution Method

Single crystals of pure and Ba @ amino hydrogen chloride (l-histidine hydrogen chloride) monohydrate (C6H9N3O2·HCl·H2O) were grown by Slow Evaporation Solution Technique (SEST). The grown crystals were investigated by single crystal XRD, FT-IR, Energy Dispersive X-Ray (EDX), Scanning Electron Microscopy (SEM), Linear Optical (UV–vis–NIR), Non Linear Optical (NLO), Dielectrics and Vickers microhardness studies to find the crystal and molecular structure, composition, surface morphology, linear and non linear optical, electrical and mechanical behavior. Structural difference between l-histidine hydrochloride (LHC) and Ba @ l-histidine hydrochloride (Ba@LHC) crystals was studied by single XRD analysis. Functional groups were identified by FTIR spectroscopy. The linear optical spectrum is correlated with the non linear (second harmonic generation, SHG) properties.

Synthesis, Growth and Characterization of Ni2+ incorporated Potassium Acid Phthalate crystal: A Potential material for NLO applications

Undoped and Nickel nitrate (Ni2+) doped Potassium acid phthalate (KAP C8H5KO4) single crystals were grown by cost effective Slow Evaporation Solution Growth. The grown crystals were subjected to various characterization techniques. The structural and lattice parameters were analyzed by single crystal X-ray diffraction. The spectral properties were assessed by FTIR spectral analysis. Optical characters were analyzed by UV-Vis spectral studies. Mechanical properties of the doped and undoped crystals were evaluated by Vicker's Microhardness study. Thermal stability of the sample was assessed by TG/DTA analysis. EDX analysis confirms the incorporation of metal ion into the crystal lattice of the title compound. SHG studies confirm that Ni2+ doped KAP crystal is a potential candidate for NLO applications.