Growth and characterization of hexamethylenetetramine crystals grown from solution

Organic nonlinear optical single crystals of hexamethylenetetramine (HMT; 10 × 10 × 5 mm³) were prepared by crystallization from methanol solution. The grown crystals were subjected to various characterization techniques such as single crystal XRD, powder XRD, UV-Vis and electrical studies. Single crystal XRD analysis confirmed the crystalline structure of the grown crystals. Their crystalline nature was also confirmed by powder XRD technique. The optical transmittance property was identified from UV-Vis spectrum. Dielectric measurements were performed as a function of frequency at different temperatures. DC conductivity and photoconductivity studies were also carried out for the crystal. The powder second harmonic generation efficiency (SHG) of the crystal was measured using Nd:YAG laser and the efficiency was found to be two times greater than that of potassium dihydrogen phosphate (KDP).     

Studies on the nonlinear optical single crystal: Ammonium d,l-tartrate (C4H9NO6)

The organic nonlinear optical material ammonium d,l-tartrate single crystal has been successfully grown by slow evaporation solution technique (SEST). The grown crystals were characterized by single crystal XRD and the lattice parameters have been confirmed. The structural perfection of the grown crystal was analyzed by high-resolution X-ray diffraction measurement. The optical transmittance spectrum shows that the material has a good optical transparency in the entire visible region with the UV cut-off wavelength at 234 nm. Thermogravimetric and differential scanning calorimetric measurements were performed to study the thermal properties of the grown crystal. Chemical etching studies were attempted to determine the dislocation density of the grown crystal. Mechanical behavior was assessed using Vickers hardness testing carried out on (0 0 1) crystallographic plane. The Kurtz–Perry powder SHG technique confirms the NLO property of the grown crystal and the efficiency of AMT crystal was found to be 1.3 times that of standard KDP crystal.     

Growth and characterization of l-proline cadmium chloride monohydrate single crystals

A novel semi-organic material of l-proline cadmium chloride monohydrate (l-PCCM) has been successfully synthesized and single crystal was grown by slow evaporation solution growth technique at room temperature. The grown single crystals have been characterized by different instrumentation techniques like XRD, FTIR, UV-Vis-NIR and TG/DTA measurements. Its nonlinear optical property has been tested by Kurtz powder method. The mechanical properties of grown crystals have been studied using Vickers microhardness tester. Its relative SHG efficiency is two times higher than that of potassium dihydrogen phosphate (KDP) single crystal.     

Growth and characterization of organic material 2-hydroxypyridine single crystal by modified vertical Bridgman technique

Large size (15 mm diameter and 80 mm length) organic material 2-hydroxypyridine single crystal has been grown using the double wall ampoule with nano translation by modified vertical Bridgman technique for the first time. Material of the grown crystal was confirmed by single and powder X-ray diffraction (XRD) measurements. Fourier transform infrared (FTIR) analysis was used to identify the functional groups present in the grown crystal. High resolution X-ray diffraction (HRXRD) has been performed to analyze the crystalline perfection of the grown single crystal. The optical property of the grown crystal was analyzed by UV–vis–NIR and photoluminescence (PL) spectral measurements. The thermal characteristics of the grown crystal were analyzed by thermogravimetric (TG) and differential thermal analyses (DTA). The dielectric measurements were carried out with four different frequencies at various temperatures ranging from 308 to 373 K and the results indicate an increase in the dielectric parameters with the increase of temperature at all frequencies. The second harmonic generation (SHG) studies were used to analyze the nonlinear optical property of the grown crystal.     

Investigation on growth,structural, optical,thermal, dielectric and mechanical properties of organic l-prolinium trichloroacetate single crystals

A new organic nonlinear optical material l-prolinium trichloroacetate (l-PTCA) single crystal has been synthesized and grown by slow solvent evaporation technique at room temperature using water as solvent. Single-crystal X-ray diffractometer was utilized to measure unit cell parameters and to confirm lattice parameter. The powder X-ray diffraction pattern of the grown l-PTCA has been indexed. The modes of vibration of different molecular groups present in the sample were identified by the FTIR spectral analysis. The optical transmittance window and the lower cutoff wavelength of the l-PTCA have been identified by UV–vis–NIR studies. Thermal stability of the l-prolinium trichloroacetate was determined by TGA/DTA measurements. Dielectric measurements were carried out at various temperatures at frequency range 10–1 MHz. The mechanical properties of the grown crystals have been analyzed by Vickers microhardness method. The chemical etching studies were carried out on the grown crystals. Its SHG efficiency has been tested by Kurtz powder method.     

Studies on the growth aspects of semi-organic cadmium zinc thiourea acetate: A promising new NLO crystal

Single crystals of a new nonlinear optical material, cadmium zinc thiourea acetate (CZTA), were successfully grown by slow evaporation of the aqueous solution at room temperature. Single crystal X-ray diffraction pattern and FTIR spectrum analysis have confirmed the formation of the new crystal. The optical transmission studies and second harmonic generation (SHG) efficiency studies justified the device quality of the grown crystals.     

Growth and characterization of cobalt thiourea sulfate,a new nonlinear optical material

A new semi-organic nonlinear optical crystal of cobalt thiourea sulfate (CTS) has been grown by solvent evaporation solution growth method at room temperature. The unit cell parameters were evaluated by single crystal X-ray diffraction technique. The vibrational frequencies of various functional groups in the crystals have been derived from FT-IR analysis. The range and percentage of optical transmission are ascertained by recording the UV–VIS–NIR spectrum. The thermal behavior of the crystals has been investigated by DTA and TGA analyses. The mechanical property of the grown crystals has been analyzed by Vicker's microhardness method. The NLO property of the grown crystal has been confirmed by the Kurtz powder second harmonic generation (SHG) test.     

Synthesis, crystal growth and characterization of organic material: N-Bromosuccinimide (NBS) for NLO applications

The organic nonlinear optical crystal of N-Bromosuccinimide (NBS) was grown by slow cooling solution growth technique using methanol as solvent. Single crystal and powder X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectral analyses were carried out to confirm the NBS crystals. The ultra violet (UV)-Visible and photoluminescence spectral studies were carried out, the green band at 2.02 eV can be attributed to radiative recombination between deep donors and shallow acceptors. The second harmonic generation (SHG) behaviour of NBS was tested by Kurtz-Perry powder technique. The hardness behaviour, laser damage threshold and dielectric characteristics of NBS crystals were studied.     

Study of pure and l-tartaric acid doped ammonium dihydrogen phosphate single crystals: A novel nonlinear optical non-centrosymmetric crystal

Single crystals of pure and l-tartaric acid (LTA) C₄H₆O₆ doped ammonium dihydrogen phosphate (ADP) (NH₄) H₂PO₄ were grown by slow evaporation solution technique (SEST) at ambient conditions. Powder X-ray diffraction (PXRD) analysis was carried out to confirm the crystal structure and no additional phase was observed due to doping except a systematic variation in peak intensities. Fourier transform infrared spectral analysis was done to examine the presence of various functional groups in the grown crystals. UV–VIS–NIR spectroscopic analysis was carried out to see the change in optical transparency of pure ADP and crystals due to LTA with different doping concentrations. Second harmonic generation (SHG) efficiency measurement was done to examine the enhancement in the nonlinear optical characteristics of the grown crystals. The effect of LTA dopant on crystal morphology, thermal and mechanical properties of ADP have also been presented in this paper. The above studies reveal the effect of incorporation of LTA into the lattice of ADP crystals.     

Growth and characterization of 4-methyl benzene sulfonamide single crystals

Single crystals of 4-methyl benzene sulfonamide (4MBS) were successfully grown from aqueous solution by low temperature solution growth technique. The grown crystal was characterized by single crystal XRD and powder XRD methods to obtain the lattice parameters and the diffraction planes of the crystal. UV–vis–NIR absorption spectrum was used to measure the range of optical transmittance and optical band gap energy. The optical transmission range was measured as 250–1200 nm. FTIR spectral studies were carried out to identify the presence of functional groups in the grown crystal. The thermal behavior of the crystal was investigated from thermo gravimetric analysis (TGA) and differential scanning calorimetry (DSC) study. The absence of SHG was noticed by Kurtz and Perry powder technique. The third order NLO behavior of the material was confirmed by measuring the nonlinear optical properties using Z-scan technique and it was found that the crystal is capable of exhibiting saturation absorption and self-defocusing performance.     

A study on the <Emphasis Type="SmallCaps">l</Emphasis>-lysine-iodic acid: semi organic non linear optical single crystals for electro-optic applications

Non linear optical single crystals of l-lysine-iodic acid (LLI) of dimensions upto 24?×?14?×?5 mm³ have been grown successfully by slow evaporation technique from aqueous solution. The crystal structure of the grown material was solved by single crystal X-ray diffraction analysis and it was found that the LLI crystal belongs to monocinic system with space group P2₁. Functional groups of the grown crystal were identified by Fourier Transform Infrared (FTIR) spectral analysis. The UV–Vis spectral analysis was carried out to measure the transparent range of the LLI crystal which is nearly 85% and the band gap energy is found to be 5.51 eV. Thermal stability and decomposition temperature of LLI crystal was found by means of TGA and DTA analyses. The mechanical behavior of the grown crystal has been employed using Vicker’s micro hardness technique. The Second Harmonic Generation (SHG) efficiency of the crystal was investigated and it was found to be 3.2 times of KDP. The particle size dependent SHG studies of LLI crystals were performed using Nd:YAG laser. The laser damage threshold value of LLI crystal is found to be 8.54 GW/cm². Dielectric study indicates the reasonable dielectric constant and low dielectric loss of LLI crystal which are essential properties to develop optoelectronic devices. The ac and dc electrical conductivity measurements were carried out at various temperatures. Photoconductivity study exhibits the negative photoconductivity nature of the LLI crystal and the results are discussed for the first time.     

Growth and characterization of 4-dimethylamino-N-methyl 4-stilbazolium tosylate (DAST) single crystals grown by nucleation reduction method

Good quality single crystal 4-dimethylamino-N-methyl 4-stilbazolium tosylate (DAST) has been grown by novel nucleation reduction method instead of regular slope nucleation technique (SNT). The grown crystal was subjected to high resolution X-ray diffraction (HRXRD) studies, the perfection of the crystal was found to be better than the crystal grown by slope nucleation technique and slow cooling method. The UV-vis-NIR spectrum was recorded for the grown crystal and relative second harmonic generation (SHG) efficiency was investigated to explore the nonlinear optical (NLO) property. The dielectric and thermal behaviour of the crystal were also studied. The nuclear magnetic resonance (NMR) studies also performed for the identification of different modes present in the compound. The photoluminescence and mechanical were carried out and the results were discussed in detail.     

Growth and characterization of a new NLO material: l-Glutamic acid hydro bromide [l-GluHBr]

l-(+)-Glutamic acid hydro bromide, an isomorphic salt of l-glutamic acid hydrochloride, was synthesized and the synthesis was confirmed using Fourier transform infrared analysis. Solubility of the material in water was determined. l-Glutamic acid hydro bromide crystals were grown by low temperature solution growth using the solvent evaporation technique. Single crystal X-ray diffraction studies were carried out and the cell parameters, atomic co-ordinates, bond lengths and bond angles were reported. High-resolution X-ray diffraction studies were carried out and good crystallinity for the grown crystal was observed from the diffraction curve. The grown crystals were subjected to dielectric studies. Ultraviolet-visible-near infrared spectral analysis shows good optical transmission in the visible and infrared region of the grown crystals. The second harmonic generation efficiency of l-glutamic acid hydro bromide crystal was determined using the Kurtz powder test and it was found that it had efficiency comparable with that of the potassium di-hydrogen phosphate crystal.     

Crystal growth, structure and characterizations of a new semiorganic nonlinear optical material—β-Alanine zinc chloride

The title compound, β-alanine zinc chloride—a new semiorganic nonlinear optical crystal was grown by slow evaporation technique. Single crystals of β-alanine zinc chloride have been subjected to X-ray diffraction analysis to determine the crystal structure. The powder X-ray diffractogram of the crystal has also been recorded. The amount of carbon, nitrogen and hydrogen in the crystals was also estimated. Fourier Transform Infrared and Raman spectral measurements have been carried out on the grown crystals in order to identify the functional groups. The presence of hydrogen and carbon in the β-alanine zinc chloride was confirmed by using proton and carbon nuclear magnetic resonance spectral analyses. The percentage of zinc in the crystal was determined by atomic absorption spectroscopy. Optical behavior such as ultraviolet-vis-near infrared transmittance spectrum and second harmonic generation has been investigated. The mechanical strength and thermal behavior of the grown crystal have been analyzed.     

Melt growth of novel organic nonlinear optical material and its characterization

Ethyl P-amino benzoate (EPAB) is also known as benzocaine was recently identified as new organic non linear optical (NLO) material which is having nearly six times higher SHG efficiency than that of KDP. Hence, growth of unidirectional EPAB crystal gains importance for phase matching studies and this is the first melt growth report of EPAB single crystal. Seeding with the microtube in the present technique eliminates the need for pre-grown seed and has more probability to grow bulk single crystal. Growth direction of the μT-Cz grown EPAB single crystals was identified as <100> using X-ray powder diffraction studies. Thermal properties and optical transparency of the grown material were analyzed by TG and DTA and UV-VIS spectroscopic studies respectively. Laser damage threshold study shows nearly five times high damage threshold than KDP.     

Influence of NH4Cl on the < 1 0 0> directed growth and properties of ADP crystal

Good quality, pure and ammonium chloride added < 1 0 0> directed ADP single crystals with different sizes were grown by Sankaranarayanan-Ramasamy method with the vision to improve the properties of the crystal. The grown crystals have cylindrical morphology and the crystals were subjected to UV-Vis., DTA, microhardness, laser damage threshold, dielectric, piezoelectric and SHG studies. The addition of ammonium chloride improves the quality and yields crystals with transparency more than 80% in minimum duration of growth. Higher laser damage threshold and mechanical stability were observed in ammonium chloride added ADP crystals. Low dielectric loss shows that the grown crystal contains minimum defects. Good piezoelectric behaviour was observed for the grown crystals. The SHG efficiency of the crystals was obtained using Nd-YAG laser, which is approximately 3 times that of pure ADP and shows the suitability of the ingot for nonlinear optical applications.     

Synthesis,crystal growth,structural, spectral,thermal, mechanical,linear and nonlinear optical studies of organic single crystal 4-Iodo 4-nitrostilbene (IONS): A potential NLO material

An organic nonlinear optical material 4-Iodo 4-nitrostilbene (IONS) has been synthesized and good optical quality single crystal was grown from ethyl methyl ketone solvent by the solution growth technique. Single and powder X-ray diffraction analyses reveals that the grown crystal belongs to monoclinic crystal system with noncentrosymmetric space group ‘P2₁’ and it has good crystalline nature. Functional groups and molecular structure of the title compound were confirmed by FTIR and ¹H NMR respectively. The UV–Vis–NIR absorption study reveals no absorption in the visible region and the cut-off wavelength was found to be at 412.84 nm, TG/DTA, mass spectral analysis, photoluminescence and microhardness studies have been carried out for the grown crystals and results are discussed in detail. The second harmonic efficiency of the IONS was determined by Kurtz–Perry powder technique which reveals that the IONS crystal (3.1 V) has greater efficiency i.e., 143 times to that of KDP (21.7 mV).     

Studies on growth and characterization of an NLO crystal: L-alanine hydrogen chloride (LAHC)

A nonlinear optical (NLO) salt viz. L-alanine hydrogen chloride (LAHC) has been synthesized and solubility of the synthesized salt in de-ionized water was determined at different temperatures. Single crystals of L-alanine hydrogen chloride (LAHC) salt were grown by solution method with slow evaporation technique. The grown crystals were characterized by single crystal X-ray diffraction (XRD) and powder XRD analyses to study the crystal structure. The crystallinity of LAHC crystal was confirmed by the powder X-ray diffraction study and diffraction peaks were indexed. FTIR study was used to confirm the presence of various functional groups in the grown crystals. UV–visible transmittance spectrum was recorded to study the optical transparency of LAHC crystal. The nonlinear optical (NLO) property of the grown crystal was confirmed by Kurtz–Perry powder test. The density of LAHC crystal was determined by floatation method. The mechanical strength of the crystal was estimated by Vickers hardness test. The grown crystals were subjected to TG/DTA analyses. The dielectric behavior of the sample was also studied.     

Investigating optical,electrical, and mechanical traits of thiourea admixtured KDP single crystals to explore NLO device applications

The 0.5 and 1 mol% thiourea “mixed” potassium dihydrogen phosphate (KDP) crystals have been developed by conventional slow solution evaporation method. The crystallographic parameters of grown crystals have been determined by employing single crystal X-ray diffraction technique. The functional groups of grown crystals were successfully identified by means of FTIR spectral analysis. The optical transmittance is 79%, 84%, and 89% for KDP, 0.5 mol thiourea mixed KDP, and 1 mol thiourea mixed KDP crystal. The energy band gap (E_g) of KDP, 0.5 mol thiourea mixed KDP, and 1 mol thiourea mixed KDP crystal is 3.71 eV, 3.61 eV, and 3.75 eV, respectively. The Kurtz–Perry test has been employed to determine the SHG efficiency and SHG efficiency of 0.5 and 1 mol thiourea mixed KDP crystal is 2.09 and 2.22 times superior to KDP crystal. Effect of thiourea mixing on hardness properties of KDP crystal have been scrutinized using the Vickers microhardness studies. The frequency dependent dielectric behavior of grown crystals has been analyzed at room temperature.

     

Feasibility study on Czochralski (Cz) growth of 3-methoxy 4-hydroxy benzaldehyde (MHBA) single crystals for nonlinear optical applications

Reported large nonlinear optical coefficients such as d₂₂ = 23.8d₃₆^KDP, d₂₁ = 13.5d₃₆^KDP, d₂₃ = 29.1d₃₆^KDP, d₂₅ = 12.8d₃₆^KDP of 3-methoxy 4-hydroxy benzaldehyde (MHBA) attract research on its bulk crystal growth for device application. The X-ray rocking and X-ray topographic studies of Cz-grown organic monoclinic crystals invariably reveal closely aligned sub-crystals which made melt growth difficult. In this context, the single crystal growth of MHBA by Czochralski pulling technique has been successfully demonstrated for the first time in the literature. Comparison study of obtained X-ray powder diffraction data with the literature confirmed the monoclinic structure. High-resolution X-ray diffraction (HRXRD) study confirms the better crystalline perfection of the grown crystal in comparison to that of solution-grown crystals and revealed the optimization of the growth process along [211¯] direction. TG, DTA and optical transmission studies carried out on the grown crystal exhibit its thermal and optical properties for SHG application.