Subsurface Damage in Scratch Testing of Potassium Dihydrogen Phosphate Crystal

Potassium dihydrogen phosphate （KDP） is an important electro-optic crystal, often used for frequency conversion and Pockels cells in large aperture laser systems. To investigate the influence of anisotropy to the depth of subsurface damage and the profiles of cracks in subsurface of KDP crystal, an experimental study was made to obtain the form of subsurface damage produced by scratches on KDP crystal in [100], [120] and [110] crystal directions on （001） crystal plane. The results indicated that there were great differences between depth and crack shape in different directions. For many slip planes in KDP, the plastic deformation and cracks generated under pressure in the subsurface were complex. Fluctuations of subsurface damage depth at transition point were attributed to the deformation of the surface which consumed more energy when the surface deformation changed from the mixed region of brittle and plastic to the complete brittle region along the scratch. Also, the process of subsurface damage from shallow to deep, from dislocation to big crack in KDP crystal with the increase of radial force and etch pit on different crystal plane were obtained. Because crystallographic orientation and processing orientation was different, etching pits on （100） crystal plane were quadrilateral while on （110） plane and （120） plane were trapezoidal and triangular, respectively.

Recent Advances in Nonlinear Optical Phosphate Materials

In recent years, motivated by the discovery of deep-UV（wavelengths below 200 nm） nonlinear optical（NLO） phosphates, Ba3P3O（10）X（Cl, Br）, phosphates have entered into a passionate research era. In this review, recently discovered phosphate materials containing different anionic groups, i.e., isolated [PO4], [P2O7] dimer, [P3O（10）] trimer, and [PO3]∞ chain, are summarized, including their syntheses, structures, NLO performances and properties. Especially phosphates with short absorption edges in the deep-UV region and good SHG efficiency are introduced in detail. We hope that this work will present a clear view of the crystal chemistry of phosphates and promote the discovery of new high-performing second-order NLO materials to meet the urgent needs in laser science.

Electrical Conduction in Deuterated Ammonium Dihydrogen Phosphate Crystals with Different Degrees of Deuteration

Conductivity measurements of deuterated ammonium dihydrogen phosphate （DADP） crystals with different deuterated degrees are described. The conductivities increase with the deuterium content, and the value of the a-direction is larger than that of the e-direction. Compared with DKDP crystals, DADP crystals have larger conductivities, which is partly due to the existence of A defects. The ac conductivity over the temperature range 25-170℃has shown a knee in the curve ofln（σT） versus T-1. The conductivity activation energy calculated by the slope of the high temperature region decreases with the deuterium content. The previously reported phase transition is not seen.

Investigation of the trajectory uniformity in water dissolution ultraprecision continuous polishing of large-sized KDP crystal

Large-sized potassium dihydrogen phosphate(KDP)crystals are an irreplaceable nonlinear optical component in an inertial confinement fusion project.Restricted by the size,previous studies have been aimed mainly at the removal principle and surface roughness of small-sized KDP crystals,with less research on flatness.Due to its low surface damage and high machining efficiency,water dissolution ultraprecision continuous polishing(WDUCP)has become a good technique for processing large-sized KDP crystals.In this technique,the trajectory uniformity of water droplets can directly affect the surface quality,such as flatness and roughness.Specifically,uneven trajectory distribution of water droplets on the surface of KDP crystals derived from the mode of motion obviously affects the surface quality.In this study,the material removal mechanism of WDUCP was introduced.A simulation of the trajectory of water droplets on KDP crystals under different eccentricity modes of motion was then performed.Meanwhile,the coefficient of variation(CV)was utilized to evaluate the trajectory uniformity.Furthermore,to verify the reliability of the simulation,some experimental tests were also conducted by employing a large continuous polisher.The results showed that the CV varied from 0.67 to 2.02 under the certain eccentricity mode of motion and varied from 0.48 to 0.65 under the uncertain eccentricity mode of motion.The CV of uncertain eccentricity is always smaller than that of certain eccentricity.Hence,the uniformity of trajectory was better under uncertain eccentricity.Under the mode of motion of uncertain eccentricity,the initial surface texture of the100 mm×100 mm×10 mm KDP crystal did achieve uniform planarization.The surface root mean square roughness was reduced to 2.182 nm,and the flatness was reduced to 22.013μm.Therefore,the feasibility and validity of WDUCP for large-sized KDP crystal were verified.

Synthesis,Single-crystal Structure,and Computational Studies of a Yavapaiite Structure Compound:Pb(Sb0.5Fe0.5)(PO4)2

The single crystals and powder of a Yavapaiite Structure phosphate,namely,PbSb0.5Fe0.5（PO4）2,were synthesized by solid state method and characterized by X-ray single-crystal diffraction and powder diffraction.The title compound crystallizes in the monoclinic system,space group C2/c（No.15） with a = 16.716（4）,b = 5.186（7）,c = 8.130（2）A,β = 114.93（6）°,Z = 4,R（I 〉 2s（I）） = 0.0430,R indices（all data） = 0.0460,and T = 293（2） K.The title compound belongs to the Yavapaiite Structure A^（Ⅱ）M^（Ⅳ）（PO4）2 compounds,and the Sb1 atom and Fe1 atoms occupy the same site（M） and their occupancy factors are refined to be 0.5 and 0.5 having a sum occupancy factor of 1.0.Its structure consists of [M（PO）4]n^2n- layers running parallel to the（b,c） plane built up of cornerconnected MO6 octahedra and PO4 tetrahedra.Additionally,the calculations of energy band structure,and density of states have been performed with the density functional theory method.The studies of computational calculation and UV experimental results show that the new compound is an indirect band-gap insulator.

Micro water dissolution machining principle and its application in ultra-precision processing of KDP optical crystal

In this paper, a micro water dissolution machining （MWDM） principle is proposed for machining potassium dihydrogen phosphate （KDP） crystal using water-in-oil micro-emulsion as an abrasive-free polishing fluid. In addition, two instances of the application of this principle to ultra-precision machining of KDP crystals are presented. Computer-controlled optical surfacing （CCOS） and diamond wire cutting （DWC） process were carried out according to the MWDM principle. In the case of the CCOS technology, it is found that the micro-waviness was removed completely by following the MWDM principle. The surface undulation decreased from 40 nm to less than 10 nm, and the surface root-mean-square （rms） roughness obviously reduced from 8.147 to 2.660 nm. In the case of the DWC process, the surface rms roughness reduced from 8.012 to 2.391 gm, and the cutting efficiency was improved. These results indicate that the MWDM principle can efficiently improve the machining quality of KDP optical crystal and has a great potential to machine water-soluble materials.

Elastic-plastic-brittle transitions of potassium dihydrogen phosphate crystals:characterization by nanoindentation

Potassium dihydrogen phosphate(KDP)crystals are widely used in laser ignition facilities as optical switching and frequency conversion components.These crystals are soft,brittle,and sensitive to external conditions(e.g.,humidity,temperature,and applied stress).Hence,conventional characterization methods,such as transmission electron microscopy,cannot be used to study the mechanisms of material deformation.Nevertheless,understanding the mechanism of plastic-brittle transition in KDP crystals is important to prevent the fracture damage during the machining process.This study explores the plastic deformation and brittle fracture mechanisms of KDP crystals through nanoindentation experiments and theoretical calculations.The results show that dislocation nucleation and propagation are the main mechanisms of plastic deformation in KDP crystals,and dislocation pileup leads to brittle fracture during nanoindentation.Nanoindentation experiments using various indenters indicate that the external stress fields influence the plastic deformation of KDP crystals,and plastic deformation and brittle fracture are related to the material's anisotropy.However,the E l Ning Hou 13b908074@hit.edu.cn Liang-Chi Zhang liangchi.zhang@unsw.edu.au 1 School of Mechatronics Engineering,Harbin Institute of Technology,Harbin 150001,People's Republic of China 2 School of Mechatronics Engineering,Shenyang Aerospace University,Shenyang 110136.People's Republic of China'Laboratory for Precision and Nano Processing Technologies,School of Mechanical and Manufacturing Engineering,The University of New South Wales,Sydney,NSW 2052,Australia effect of loading rate on the KDP crystal deformation is practically negligible.The results of this research provide important information on reducing machining-induced damage and further improving the optical performance of KDP crystal components.

Understanding the formation mechanism of subsurface damage in potassium dihydrogen phosphate crystals during ultraprecision fly cutting

Potassium dihydrogen phosphate(KDP)crystals play an important role in high-energy laser systems,but the laser damage threshold(LDT)of KDP components is lower than expected.The LDT is significantly influenced by subsurface damage produced in KDP crystals.However,it is very challenging to detect the subsurface damage caused by processing because a KDP is soft,brittle,and sensitive to the external environment(e.g.,humidity,temperature and applied stress).Conventional characterization methods such as transmission electron microscopy are ineffective for this purpose.This paper proposes a nondestructive detection method called grazing incidence X-ray diffraction(GIXD)to investigate the formation of subsurface damage during ultra-precision fly cutting of KDP crystals.Some crystal planes,namely(200),(112),(312),(211),(220),(202),(301),(213),(310)and(303),were detected in the processed subsurface with the aid of GIXD,which provided very different results for KDP crystal bulk.These results mean that single KDP crystals change into a lattice misalignment structure(LMS)due to mechanical stress in the subsurface.These crystal planes match the slip systems of the KDP crystals,implying that dislocations nucleate and propagate along slip systems to result in the formation of the LMS under shear and compression stresses.The discovery of the LMS in the subsurface provides a new insight into the nature of the laser-induced damage of KDP crystals.

Experimental study on high-efficiency polishing for potassium dihydrogen phosphate (KDP) crystal by using two-phase air-water fluid

A high-efficiency polishing approach using two-phase air–water fluid(TAWF)is proposed to avoid surface contamination and solve the inefficiency of previous water-dissolution polishing techniques for potassium dihydrogen phosphate(KDP)crystal.In the proposed method,controllable deliquescence is implemented without any chemical impurity.The product of deliquescence is then removed by a polishing pad to achieve surface planarization.The mechanism underlying TAWF polishing is analyzed,a special device is built to polish the KDP crystal,and the effect of relative humidity(RH)on polishing performance is studied.The relationship between key parameters of polishing and surface planarization is also investigated.Results show that the polishing performance is improved with increasing RH.However,precisely controlling the RH is extremely difficult during TAWF polishing.Controllable deliquescence can easily be disrupted once the RH fluctuates,which therefore needs to be restricted to a low level to avoid its influence on deliquescence rate.The material removal of TAWF polishing is mainly attributed to the synergistic effect of deliquescence and the polishing pad.Excessive polishing pressure and revolution rate remarkably reduce the life of the polishing pad and the surface quality of the KDP crystal.TAWF polishing using IC-1000 and TEC-168S increase the machining efficiency by 150%,and a smooth surface with a root mean square surface roughness of 5.5 nm is obtained.

Mechanism and inhibition of trisodium phosphate particle caking： Effect of particle shape and solubility

We investigated the influence of particle shape and solubility on the caking behavior of trisodium phosphate by considering the adhesion free energy and crystal bridge theory. Caking of trisodium phosphate during the drying process under static conditions is a two-step process： adhesion followed by crystal bridge formation between particles. The adhesion free energy plays an important role in adhesion. Trisodium phosphate particles cannot adhere to each other and cake when the adhesion free energy is greater than a critical value, which varies with particle shape. Compared with granular particles, cylindrical particles have larger contact area between particles, which results in more crystal bridges forming and a higher caking ratio. Thus, the critical value is about 100 mJ/m^2 for cylindrical particles, but 60 mJ/m^2 for granular particles at 25 ℃. Concerning the solubility, when particles are similar shapes and soluble in the rinsing liquid, the caking ratio has a linear relationship with adhesion free energy. However, if the particles are insoluble in the rinsing liquid, caking can be completely prevented regardless of adhesion free energy because no crystal bridges form during the growth process. Hence, caking of trisodium phosphate particles could be inhibited by screening rinsing liquids, and optimizing the particle shape and size distribution.

Material removal mechanisms and characteristics of potassium dihydrogen phosphate crystals under nanoscratching

Potassium dihydrogen phosphate(KDP)crystals are important materials in high-energy laser systems.However,because these crystals are brittle and soft,machining-induced defects often emerge in KDP components.This study aimed to investigate the material removal mechanisms and characteristics of KDP during nanoscratching using Berkovich,spherical,and conical indenters.We found that KDP surface layers could be removed in a ductile mode at the micro/nanoscale and that dislocation motion was one of the main removal mechanisms.Removal characteristics are related to the stress fields generated by indenter geometries.The spherical indenter achieved a ductile removal mode more easily.The lateral force of nanoscratching increased with an increase in the normal force.The coefficient of friction(COF)followed the same trend as the lateral force when spherical and conical indenters were used.However,the COF was independent of the normal force when using a Berkovich indenter.We found that these COF variations could be accurately described by friction models.