Growth and characterization of pure and picric acid doped ADP single crystals

doi:10.1016/j.cjph.2019.12.023

Chinese Journal of Physics

Volume 64, April 2020, Pages 138-162

https://doi.org/10.1016/j.cjph.2019.12.023 Get rights and content

Highlights

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Picric acid doped ADP crystals were grown.
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Powder XRD shows their single phasic nature.
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A PL study shows the existence of STE.
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The CBH and NSPT conduction mechanisms are studied.
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The third order NLO susceptibility is enhanced bypicric acid doping in ADP.

Abstract

Ammonium dihydrogen phosphate (ADP) is a pioneer kind of nonlinear optical crystal. It can be used in various electro-optical, nonlinear optical applications. The pure and different weight percentage of Picric acid doped ADP single crystals are grown using the slow solvent evaporation technique at room temperature. The powder XRD study shows single phasic nature of all the grown crystals. The photoluminescence study suggests that the dopant causes defect in structure of ADP by virtue of vibration relaxation and self trapping exciton. The dielectric constant and the dielectric loss of all the grown crystals exhibited universal behaviour over frequency range considered. The Correlation Barrier Hopping and the Non Overlapping Small Polaron Tunnelling kind of conductivity mechanism are observed. The grain and grain boundary is indentified using the complex Impedance and the complex modulus spectroscopy. The third order nonlinear optical susceptibility is increased on doping the Picric acid in ADP crystals. The results are discussed here.

Introduction

The ammonium dihydrogen phosphate (ADP) is an excellent piezo-electric crystal utilized for variety of nonlinear optical applications [1]. It has retains good transparency in a wide region of optical spectrum, resistance to damage by laser radiation and relatively high nonlinear optical efficiency. It is used as the second, third [2] and fourth [3] harmonic generator for Nd: YAG and Nd: YLF lasers. It is used for electro-optical applications such as Q-switches for Nd: YAG and Nd: YLF, Ti: Sapphire and Alexandrite lasers as well as for optical modulator [4], [5]. It is used in short-wavelength laser technology, nonlinear and integrated optics as a bulk electro-optical devices, as a frequency converters of coherent radiation of high-power pico-second lasers, as an optical parametric oscillators for the infrared spectral region, and as an integral optical waveguides [6]. The Picric acid is able to transfer a charge by virtue of proton transfer [7]. Since the conduction mechanism in ADP is due to migration of proton from one localized site to another, it is interesting to study the influence of the Picric acid on the structural, electrical and nonlinear optical properties of ADP crystal.

The novelty of present communication is that in a single paper authors have included complete electrical properties of pure and Picric acid doped ADP crystals. Moreover, the temperature sensitive conductivity mechanisms such as the Correlation Barrier Hopping and the Non-Overlapping Small Polaron Tunnelling are reported first time. The existence of pseudo pair of electron and hole such as self trapped excitons and polarons in such kind of crystal system is reported in present paper.

Further, the ability of Picric acid to enhance the nonlinear optical performance of host crystals is extensively reflected in third order nonlinear optical study of the crystals undertaken in present communication.

The pure and different weight percentage of Picric acid doped ADP crystals are grown using the slow solvent evaporation technique at room temperature. The 300 ml double distilled water is taken in glass beaker and then appropriate amount of pure ADP powder is dissolved in it. The beaker is then stirred using the magnetic stirrer for 4 h then the solution is filtered using the Whatmann filter paper 1. The pure ADP solution then sub divided into three glass beakers each of them contains 100 ml solution. One glass beaker is kept as such for the growth of pure ADP and then 0.4 g and 0.6 g picric acid is added into other glass beakers. The picric acid contained pure ADP solution then further stirred using the magnetic stirrer for another 4 h to prepare homogeneous solution. After span of 8 h the solutions are filtered using the Whatmann filter paper no. 1. All the glass beakers then shield with porous lid and then put them in dust free atmosphere for the growth of crystals. After 30 days good quality, yellow coloured crystals are harvested from the Picric acid contained beakers while the transparent crystals are obtained from the pure ADP beaker. The pure and 0.6 wt.% Picric acid doped ADP crystals are displayed in Fig. 1. For sake of simplicity, throughout the paper here we coded the grown crystals as pure ADP, 0.4PIC and 0.6PIC for pure ADP, 0.4wt.% and 0.6wt.% Picric acid doped ADP crystal.

The Powder XRD is carried on PHILIPS X'PERT MPD system and the data is analysed by using powder-X software. The photoluminescence emission and absorption spectra are recorded at room temperature using Shimadzu RF-5301 PC spectro fluoro photometer and the Xenon is used as excitation source. The complex Impedance spectroscopy is done for pelletized sample using HIOKI 3532 LCR HITERSTER metre in the frequency range of 100 Hz–10 MHz and in the temperature range of 323–373 K. The Z-scan study of polished and transparent single crystals is done using CW He-Ne laser of wavelength 632 nm.

Section snippets

Results and discussion

1
Powder XRD Study:

The Fig. 2 shows the powder XRD spectra of pure and 0.4wt.%, 0.6wt.% Picric acid doped ADP crystals. The figure is composed of various characteristic diffraction peaks of pure ADP and exhibited single phasic nature of all the grown crystals. The pure and picric acid doped ADP crystals are belong to tetragonal structure symmetry with slight variation in diffraction peak intensity and the unit cell parameters. The unit cell parameters of all the grown crystals are tabulated in

Complex impedance spectroscopy

Complex impedance is represented as Z* = Z' - j Z'', where Z' and Z'' are real and imaginary parts of impedance, respectively, which can be expressed as [26]: $Z^{'} = \frac{R_{g}}{1 + {(ω R_{g} C_{g})}^{2}} + \frac{R_{gb}}{1 + {(ω R_{gb} C_{gb})}^{2}}$ $Z^{″} = \frac{ω R_{g} C_{g}}{1 + {(ω R_{g} C_{g})}^{2}} + \frac{ω R_{gb} C_{gb}}{1 + {(ω R_{gb} C_{gb})}^{2}}$

Where ω = Angular Frequency, R_g = Grain Resistance, R_gb = Grain Boundary Resistance, C_g = Grain Capacitance and C_gb = Grain Boundary Capacitance.

The Figs. 16 (a–c) shows the variation between Z'' versus Z' (Nyquist plot) for grown crystals between the temperature range of

Complex modulus spectroscopy

The complex modulus spectroscopy is an important technique to study the electrical transport phenomena like carrier/ion hopping rate and conductivity relaxation time of materials [27]. The electrical phenomena related to smallest capacitance of material can be studied by it.

The Electric modulus in terms of complex function written as follows, $M * = M^{'} + {jM}^{″}$

The real and imaginary parts of the complex modulus are expressed as follows, $M^{'} = \frac{ɛ^{'}}{{ɛ^{'}}^{2} + {ɛ^{″}}^{2}}$ $M^{″} = \frac{ɛ^{″}}{{ɛ^{'}}^{2} + {ɛ^{″}}^{2}}$

Where, ε' and ε'' are real and imaginary

Z-scan

To determine the magnitude and sign of third order nonlinear optical parameters for our grown crystals such as nonlinear optical absorption coefficient, nonlinear optical refractive index and nonlinear optical third order susceptibility using the Z-scan experiment. The difference between the peak and valley transmission (ΔT_p-v) is written in terms of the on axis phase shift at the focus as [29], $Δ T_{p - v} = 0.0406 {(1 - S)}^{0.25} | Δ ϕ |$

Where, $| Δ ϕ | =$ On axis phase shift

The aperture linear transmittance (S) is

Conclusion

The pure and Picric acid doped ADP crystals are successfully grown using the slow solvent evaporation technique. The Powder XRD study revelled the tetragonal structure and the single phasic nature of all the grown crystals. The Photoluminescence study suggested increase of Stoke shift, existence of the self trapped excitons and the vibration relaxation phenomena in ADP crystal due to doping of the Picric acid. The dielectric constant and the dielectric loss have shows their usual behaviour for

Declaration of Competing Interests

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgement

The author (JHJ) is highly thankful to Mr. S.G.Khadelwal, Deputy Director, Forensic Science Laboratory, Ahmedabad for allow him to carry out such research activity. The authors are thankful to UGC, New Delhi, for funding under DRS-SAP and DST, New Delhi, for FIST.

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