Growth of 4-(dimethylamino) benzaldehyde doped triglycine sulphate single crystals and its characterization

Single crystals of triglycine sulphate (TGS) doped with 1 mol% of 4-(dimethylamino) benzaldehyde (DB) have been grown from aqueous solution at ambient temperature by slow evaporation technique. The effect of dopant on the crystal growth and dielectric, pyroelectric and mechanical properties of TGS crystal have been investigated. X-ray powder diffraction pattern for pure and doped TGS was collected to determine the lattice parameters. FTIR spectra were employed to confirm the presence of 4-(dimethylamino) benzaldehyde in TGS crystal, qualitatively. The dielectric permittivity has been studied as a function of temperature by cooling the sample at a rate of 1 °C/min. An increase in the Curie temperature T_c=51 °C (for pure TGS, T_c=48.5 °C) and decrease in maximum permittivity has been observed for doped TGS when compared to pure TGS crystal. Pyroelectric studies on doped TGS were carried out to determine pyroelectric coefficient. The Vickers's hardness of the doped TGS crystals along (0 1 0) face is higher than that of pure TGS crystal for the same face. Domain patterns on b-cut plates were observed using scanning electron microscope. The low dielectric constant, higher pyroelectric coefficient and higher value of hardness suggest that doped TGS crystals could be a potential material for IR detectors.     

Surface morphology, chemical contrast, and ferroelectric domains in TGS bulk single crystals differentiated with UHV non-contact force microscopy

Ferroelectric bulk single crystals of tri-glycine sulphate (TGS) have been investigated in ultra-high vacuum (UHV) using dynamic force microscopy (DFM) in the non-contact (nc) mode. Both chemical contrast from different sub-unit cell cleavage steps, and ferroelectric domains were differentiated by recording the variation in interaction force affecting the excitation amplitude A_exc applied to the piezo shaker in constant amplitude DFM. No chemical difference was found for steps measuring half the unit cell height b, in contrast to b/4—steps where sulphate ions change the local short-range chemical forces. By varying the bias voltage applied to the TGS counter electrode, the sign of bound surface charge within each ferroelectric domain was determined. Domain walls separating regions with antiparallel polarisation vectors are resolved down to a 9 nm domain wall width. Furthermore, we achieved atomic resolution with nc-DFM on cleaved TGS samples indicating the monoclinic unit cell at the ferroelectric sample surface with a=1.0±0.05 nm, c=0.55±0.05 nm, and β=107±3°.     

Crystal growth and dielectric, mechanical, electrical and ferroelectric characterization of n-bromo succinimide doped triglycine sulphate crystals

Single crystals of triglycine sulphate (TGS) doped with n-bromo succinimide (NBS) were grown at ambient temperature by the slow evaporation technique. An aqueous solution containing 1-20 mol% of n-bromo succinimide as dopant was used for the growth of NBSTGS crystals. The incorporation of NBS in TGS crystals has been qualitatively confirmed by FTIR spectral data. The effect of the dopant on morphology and crystal properties was investigated. The cell parameters of the doped crystal were determined by the powder X-ray diffraction technique. The dielectric constant of NBS doped TGS crystal was calculated along the ferroelectric direction over the temperature range of 30-60 °C. The dielectric constant of NBSTGS crystals decrease with the increase in NBS concentration and considerable shift in the phase transition temperature (T_C) towards the higher temperature observed. Pyroelectric studies on doped TGS were carried out to determine the pyroelectric coefficient. The emergence of internal bias field due to doping was studied by collecting P-E hysteresis data. Temperature dependence of DC conductivity of the doped crystals was studied and gradual increase in the conductivity with the increase of dopant concentration was observed. The activation energy (ΔE) calculated was found to be lower in both the ferroelectric and the paraelectric phases for doped crystals compared to that of pure TGS. The micro-hardness studies were carried out at room temperature on thin plates cut perpendicular to the b-axis. Less doped TGS crystals show higher hardness values compared to pure TGS. Piezoelectric measurements were also carried out on 010 plates of doped TGS crystals at room temperature.     

Thermally stimulated electron emission from chromium-doped triglycine sulfate in the paraelectric phase

Thermally stimulated electron emission from a ferroelectric chromium-doped triglycine sulfate (TGS) crystal was experimentally observed to occur in a temperature range 6 K above the Curie point from samples heated at a relatively high rate. Increasing the heating rate q was shown to cause the emission current density to increase throughout the temperature range studied. The emission onset temperature in chromium-doped TGS depends only weakly on the rate q and is close to that for pure TGS, and the emission cutoff temperature grows monotonically with q at comparatively low heating rates and stabilizes at high q. At the same time, the interval of emission extension into the paraelectric phase here is about one half that for pure TGS heated at the same rate. The specific features of emission observed for this crystal can be assigned to relaxation of the charges screening the spontaneous polarization. The lower emission cutoff temperature for the chromium-doped TGS compared to that for pure TGS is accounted for by the shorter Maxwellian relaxation time in the doped crystal.     

Pyroelectric coefficient manipulation in doped TGS crystals

Pure and l-alanine doped Triglycine sulphate (TGS) crystals were grown in paraelectric phase (∼52 °C). Doped crystals show unequal growth rates along the ferroelectric axis. Pure TGS crystals show peculiar dielectric behavior in the ferroelectric phase, after crossing up and down the Curie point in two successive runs between room temperature and 80 °C. Much higher and unstable permittivity was found returning in the ferroelectric phase. At constant temperature (35 °C), permittivity follows a relaxation process, characterized by two relaxation times. l-Alanine doped TGS crystal shows more than one order of magnitude smaller permittivity and dielectric losses. Internal bias field of ∼1 kV/cm, induced by the dopant, made the crystal almost monodomain and pined polarization in one direction. Pyroelectric coefficient measurements were performed at constant heating rate of the samples, using a computer controlled He cryostat and Keithley 6517 electrometer. The temperature dependence of P⁺ polarization component, obtained by computer integration of the pyroelectric coefficient, was measured on a large temperature interval (−20/+80 °C). Pyroelectric coefficient of the doped samples was also measured by the same procedure, using a dc bias electric field, pointing in the opposite direction to the pined polarization. The polarization could be reversed, on the whole temperature range, by dc fields higher than bias or coercive field. Surprisingly, for the first time, the pyroelectric coefficient (p) was found constant on quite large temperature intervals. Doped TGS crystals show much smaller values of permittivity ?_r versus the pure one and consequently, get higher figure of merit M = p/?_r. The pyroelectric coefficient of this material can be tailored to become constant on a defined temperature range, under a dc field control. This characteristic makes this material valuable to be used as pyroelectric material for IR devices.     

Ferroelastoelectric phenomena in a uniaxial ferroelectric TGS crystal

Possibility of the ferroelastoelectric behavior manifestations in a uniaxial ferroelectric TGS crystal was investigated. Analysis of the spontaneous piezoelectric moduli tensors for each of the 180°-domains formed as a result of the phase transition in TGS revealed possible directions for simultaneous application of the electric field and mechanical stresses to induce the switching effect in TGS. Influence of the uniaxial mechanical stresses σ₁₁, σ₂₂, σ₃₃ on the parameters of saturated and unsaturated dielectric hysteresis loops in TGS is considered. It was found that a nontraditional E ₃σ₁₂ combination of fields may lead to the domain switching in TGS crystals.     

Single crystal neutron diffraction study of triglycine sulphate revisited

In order to get the exact hydrogen-bonding scheme in triglycine sulphate (TGS), which is an important hydrogen bonded ferroelectric, a single crystal neutron diffraction study was undertaken. The structure was refined to an R-factor of R[F ²] = 0.034. Earlier neutron structure of TGS was reported with a very limited data set and large standard deviations. The differences between the present and the earlier reported neutron structure of TGS are discussed.      

Dielectric properties of film materials based on polyethylene terephthalate and polycarbonate with ferroelectric inclusions

The dielectric properties of film materials based on polyethylene terephthalate and polycarbonate with inclusions of triglycine sulfate (TGS) and TGS with admixture of L, ??-alanine (ATGS) have been studied. An increase in the temperature of the phase transition in these materials as compared to in bulk TGS and ATGS has been revealed.     

透射光栅谱仪衍射成像特性的理论模拟

应用部分相干光衍射理论,研究了透射光栅仪对单位振幅的单色扩展光源和连续谱扩展光源的衍射特性,给出了成像面上挑强分布表达式,并数值模拟了该谱仪对黑体辐射连续谱扩展光源的接收成像。     

Structure of triglycine sulfate embedded in porous aluminum oxide

The X-ray diffraction investigations have been performed for nanocomposite materials based on porous aluminum oxide with inclusions of TGS and TGS, which is doped with L,α-alanine (ATGS). The presence of the TGS and ATGS textures in pores of Al₂O₃ films has been found. It has been established that, under conditions of confined geometry, the broadening of diffraction maxima of the reflection is caused by the size effect. The temperature dependences of the order parameter for porous aluminum oxide with TGS inclusions have been constructed.     

Temperature dynamics of triglycine sulfate domain structure according to atomic force microscopy and dielectric spectroscopy data

A hydrogen-containing ferroelectric triglycine sulfate (TGS) was comprehensively studied with an atomic force microscopy (AFM) and dielectric spectroscopy. The domain structure dynamics was in situ investigated with piezoresponse force microscopy (PFM) during heating and cooling the TGS crystal near phase transition. Relaxation dependencies of domain boundaries general perimeter and domain dimensions were obtained. TGS dielectric spectra measured at the frequency range from 10 to 10¹¹ Hz were analyzed on basis of significant contribution of conductivity into the dielectric response of ferroelectrics and a good agreement with the experimental data was received. It allows us to obtain more information about temperature dynamics of the domain structure.     

TGS单晶的内偏置电场

本文从实验上验证了用热力学方法处理TGS晶体内偏置电场的正确性。分析了纯TGS晶体辐照改性与LATGS晶体的E_b-T关系有所区别的原因。文中还讨论了辐照改性的退化问题。 关键词：     

Growth,structural, mechanical,spectral and dielectric characterization of NaCl-added Triglycine sulfate single crystals

Pure and sodium chloride (NaCl)-added Triglycine sulfate (TGS) crystals were grown from aqueous solutions by slow evaporation technique. The values of concentration of dopants in the mother solution were 0.2, 0.6 and 1 mol%. The solubility of the grown samples have been found out at various temperatures. The determination of unit cell parameters was carried out by single crystal XRD method and found that the grown crystals crystallize in monoclinic structure. The dielectric characterization for the pure and NaCl-doped TGS crystals was performed by measuring the dielectric parameters like dielectric constant and dielectric loss with various frequencies in the range 10²–10⁶ Hz and with the temperatures ranging from 30 to 70 °C and this study reveals an increase of dielectric constant and loss with the increase of NaCl concentration. Studies on mechanical properties like microhardness and density of the grown pure and NaCl-doped TGS crystals were carried out. UV–Visible transmittance studies were carried out for the grown samples. A sharp fall in the transmittance is observed at 228 nm for pure and NaCl-doped TGS crystals. Atomic absorption spectroscopic (AAS) study was done on the NaCl-doped TGS crystals to ascertain the presence of Na⁺ ions in the lattice.     

Single crystals of triglycine sulphate containing palladium

Single crystals of TGS doped with Pd₂₊ have been grown from aqueous solutions using the method of temperature decrease. It was found that the relative growth rate along thec-axis is not constant through the growth process being larger by more than an order of magnitude (in medium size crystals, ca. 30 g) than in pure TGS crystals. Investigation of the domain structure revealed that in the growth pyramids ¦110¦, the crystals are poled in one direction. The internal bias field in these growth pyramids was experimentally found to be of the order of 1 kV/cm. The high internal field excludes the possibility of spontaneous depoling and makes the Pd²⁺-doped TGS crystals suitable for pyroelectric applications.     

Effects of composition ratio on structure and phase transition of ferroelectric nanocomposites from silicon dioxide nanoparticles and triglycine sulfate

The present work is devoted to study on influences of silicon dioxide nanoparticles (SiO₂) on structure and phase transition of a classical ferroelectric of triglycine sulfate (TGS) by synthesizing a composite containing SiO₂ and TGS at different composition weight ratios. Particle size analysis, X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) techniques were utilized to charaterize the synthesized composite. The experiments for investigation of phase transition were conducted from 20 to 120°C under a weak electric field (1?V.cm^?1) at 1?kHz. The results revealed an expansion of ferroelectric phase of TGS by 15–55°C with increasing the SiO₂ content. Besides, an additional phase transition point which is characteristic for the bulk clusters of TGS was found at low content of SiO₂. The detected anomalies were discussed thoroughly based on the interaction between components in the composite.     

溶剂变更法生长的TGS单晶的介电和热电性能

用新的溶剂变更法生长TGS单晶,即在TGS水溶液中缓慢加入无水乙醇而使TGS结晶析出。测量了这种方法生长的单晶的电滞迴线、介电常数和热电系数。测量结果表明,与降温法生长的单晶的性能是相同的。 关键词：     

Magnetic memory effects in triglycine sulfate ferroelectric crystals

The effect of a magnetic field on the processes of relaxation of the defect structure relaxation in a triglycine sulfate (TGS) ferroelectric (nonmagnetic) crystal has been observed for the first time. The atomic-force microscopy study has shown that the application of a static weak magnetic field (2 T, 20 min) significantly changes the size distribution of defect nanoclusters characteristic of TGS. Previously known macroscopic aftereffects of the magnetic field in TGS (slow relaxation of the dielectric susceptibility, symmetrization of P–E dielectric hysteresis loops, etc.) can be explained by the redistribution of pinning centers of domain walls caused by the magnetically induced reconfiguration of the defect structure.     

The impedance-characteristic method in the study of specific temperature features of dielectric anomaly suppression in triglycine sulfate

The reflection and absorption coefficients in a waveguide loaded on ferroelectric triglycine sulfate (TGS), which has a layered domain structure near the phase transition, are calculated by the impedance-characteristic method. The calculated and experimental data do not reveal any correlations with the specific temperature features in the TGS dielectric response to microwave irradiation. The mechanism of the microwave effect is discussed.     

Copper vanadate nanowires-based MIS capacitors: synthesis,characterization, and their electrical charge storage applications

Dielectric properties of porous glass nanocomposites with TGS crystals embedded into six porous matrices with average pore size from 5 to 312 nm were investigated in the temperature range from 280 to 380 K at selected frequencies. The results are discussed based on the effect of the particle size on the phase transition temperature of TGS nanocomposites. Temperature–size phase diagram of TGS composites was derived. Non-monotonic character of the temperature-driven phase transition (T _p) with the decreasing particle size was determined. The nature of the T _p variation can be ascribed to the size-effect theoretically predicted by Zhong et al. (Phys Rev B 50:698–703, 1994).