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.

Characteristics of Laser-Induced Surface and Bulk Damage of Large-Aperture Deuterated Potassium Dihydrogen Phosphate at 351 nm

Deuterated potassium dihydrogen phosphate damage performance at 351 nm is studied on a large-aperture laser system. Bulk and rear-surface damage are initiated under the 3ω fluences of 6.T J/cm2 and 33/cm2, and show different growth characteristics under multiple laser irradiations with the fluence of 6 J/cm2. The size and number of bulk damage keep unchanged once initiated. However, surface damage size also does not grow, while surface damage number increases linearly with laser shots. Different damage thresholds and growth behaviors suggest different formations of bulk and surface damage precursors. The cause of surface damage is supposed to be near-surface absorbing particles buried under the sol-gel coating.

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.

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.

Investigation into the room temperature creep-deformation of potassium dihydrogen phosphate crystals using nanoindentation

It has been a tremendous challenge to manu facture damage-free and smooth surfaces of potassium dihydrogen phosphate (KDP) crystals to meet the require ments of high-energy laser systems. The intrinsic issue is whether a KDP crystal can be plastically deformed so that the material can be removed in a ductile mode during the machining of KDP. This study investigates the room tem perature creep-deformation of KDP crystals with the aid of nanoindentation. A stress analysis was carried out to identify the creep mechanism. The results showed that KDP crystals could be plastically deformed at the nanoscale. Dislocation motion is responsible for creep-deformation. Both creep rate and creep depth decrease with decrease in peak force and loading rate. Dislocation nucleation and propagation bring about pop-ins in the load displacement curves during nanoindentation.

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.

大截面KDP晶体在激光核聚变研究中的应用

介绍了大截面ＫＤＰ晶体在激光核聚变中的应用，并简述了该晶体的研究动态。

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.

KDP晶体生长习性与快速生长研究

发现由五氧化二磷合成的KDP晶体生长原料中含有大量还原性亚磷酸盐杂质．实验表明，亚磷酸盐对晶体锥面生长有显著的抑制作用．低浓度时造成柱面扩展，在高浓度时则使整个晶体的生长速度变慢．这种原料以适当方法提纯后，用“点籽晶”技术进行快速生长实验，平均生长速度达到13．7mm／天．

KDP晶体磨削表面缺陷及损伤分析

在对磷酸二氢钾(KDP)晶体进行磨削加工的基础上,利用光学显微镜、ZYGO三维表面形貌仪和扫描电子显微镜对KDP晶体磨削加工表面层缺陷及损伤进行了研究,发现磨削加工后的KDP晶体表面有较大的划痕和脆性破碎现象,材料以脆性去除为主。

KDP晶体三倍频晶面微观力学行为及加工性能

为了揭示磷酸二氢钾(KDP)晶体三倍频晶面微观弹塑性力学行为及加工性能,开展了纳米压痕研究。建立了KDP晶体三倍频晶面各向异性力学模型,基于光滑粒子流体动力学(SPH)方法对纳米压痕进行了数值仿真并完成了纳米压痕测试实验。实验结果表明:实验与仿真计算的载荷-压入深度关系曲线的相关系数为0.996 328,吻合度较高,验证了力学模型的正确性,得出KDP晶体三倍频晶面的屈服强度为240MPa。数值仿真结果显示:由于材料的各向异性,工件内部应力呈不规则圆弧状分布;载荷大小与等效应力影响深度呈近似线性递增关系;材料表面等效塑性应变分布形状与压头投影面几何形状相类似,存在复映效果。当载荷小于2mN时,各压头的残余应力深度差异性较小(小于0.2μm);随着载荷逐渐增大,这种差异不断扩大。得到的结果为实现KDP晶体三倍频晶面的高效低损伤加工提供了理论支撑。

单点金刚石飞切KDP晶体表面缺陷深度的研究

基于印压断裂力学理论分析了磷酸二氢钾晶体表面缺陷面积与中位裂纹深度的关系.在刀具参量和主轴转数一定的情况下,采用不同切削深度和进给速率对磷酸二氢钾晶体进行单点金刚石飞切加工实验,并计算晶体表面单位面积缺陷的占比系数.实验结果表明,晶体表面缺陷深度与面积占比系数成正相关,与理论分析结果相符,进而提出了利用计算晶体表面缺陷占比系数估测缺陷深度的方法.最后基于该方法得到高效率切削步骤,并加工获得了表面粗糙度算术平均值优于5nm的超光滑晶体表面.

KDP晶体中铝取代钾点缺陷第一性原理计算

为了明确Al3+在KDP晶体生长过程中对光学性质和力学性质的具体影响,采用第一性原理计算程序包VASP软件计算并分析了Al取代K对KDP晶体的晶体结构、电子能态密度和光学性质,并同理想KDP晶体进行对比研究。结果表明,KDP晶体中Al取代K的缺陷形成能为0.974 e V,并且Al替位K点缺陷引起的晶格畸变非常微弱,缺陷比较容易形成。Al取代K后晶体能带中价带顶附近的态密度发生了变化,并且带隙中存在缺陷能级,取代后KDP晶体的带隙宽度减小为4.37 e V,缺陷增加了KDP晶体对可见到紫外波段的光子吸收,影响KDP晶体光学质量及其激光损伤性能。计算力学性质发现,Al替位掺杂KDP晶体比理想KDP晶体的杨氏模量增加了,这会减弱晶体抗激光损伤能力。

KDP无磨粒抛光微机械作用力学模型建立与仿真

无磨粒化学机械抛光是一种柔和的表面处理方法,可以有效去除磷酸二氢钾(KDP)晶体表面的小尺度飞切刀纹。在抛光过程中不使用磨粒,KDP晶体与抛光垫粗糙峰直接接触,两者之间相对运动,在表面接触应力的作用下,抛光垫对KDP晶体表面产生微机械作用,在实现材料去除和改善表面质量方面具有重要的作用。为了深入了解无磨粒化学机械抛光中微机械去除作用,文章通过研究表面接触应力分布和变化规律,对抛光过程中的微机械作用进行定量分析,建立了KDP晶体与抛光垫粗糙峰接触力学的数学模型并开展系统研究。根据Hertz理论对抛光过程中KDP晶体表面接触应力进行了计算与分析,研究了抛光压力、摩擦系数、抛光垫杨氏模量和抛光垫粗糙峰半径等抛光参数对微机械作用的影响规律,获得了不同抛光条件下最大许用抛光压力。结合实验结果,对KDP晶体与抛光垫之间的微机械作用进行了实验验证,进一步揭示了KDP晶体无磨粒化学机械抛光去除机理。

激光聚焦线扫描法测量KDP晶体坯片的体缺陷

为了快速准确测量磷酸二氢钾(KDP)晶体坯片的体缺陷,提出了高速激光聚焦线扫描散射成像方法,并建立了相应的测量系统。研究了该系统的测量原理和图像采集、图像处理和体缺陷信息提取方法。基于激光散射技术,结合高速运动装置对晶体坯片内部进行三维扫描,用线阵CCD探测器接收气泡、包裹物等体缺陷产生的散射光。然后利用折射率匹配液消除粗糙表面带来的不利影响。最后结合数字图像处理技术,对采集的图像进行实时处理。通过去除背景后与设定阈值比较得到具有体缺陷特征的图像,再对其进行二值化处理,提取得到体缺陷的位置和尺寸信息。利用该检测装置对KDP晶体坯片体缺陷进行了测量,结果显示其检测分辨率优于40μm,能够为晶体坯片的精确切割和最大程度的利用提供依据,从而节省了大量成本。

激光预处理技术及其应用

回顾了国内在激光预处理技术研究方面取得的进展。综述了基于激光预处理技术提升基频介质膜、磷酸二氢钾/高掺氘磷酸二氢钾(KDP/DKDP)晶体等光学元件抗激光损伤性能的机理、效果和关键技术。针对高功率激光驱动器中关键光学元件激光负载能力的提高,建立了大口径光学元件激光预处理平台,实现了基频介质膜元件的激光预处理工程化作业。比较了纳秒和亚纳秒脉冲宽度激光对DKDP晶体损伤性能的影响。基于亚纳秒激光预处理后,纳秒激光辐照至14.4J/cm2(5ns)尚未出现"本征"损伤的实验结果,提出了用于DKDP晶体的亚纳秒激光预处理方案,并指出亚纳秒激光预处理技术将成为高功率激光三倍频晶体抗激光损伤性能达标的关键技术。

杂质对于磷酸二氢钾结晶的影响研究

初步净化后湿法磷酸生产的磷酸二氢钾常含有多种杂质。采用间歇结晶法研究了Fe3+、Al3+、Mg2+、Ca2+、F-、SO42-杂质对磷酸二氢钾结晶介稳区宽度、结晶晶形、诱导时间、结晶生长速度等的影响。实验结果表明:各种杂质离子均导致结晶介稳区增大,其中高价金属离子Fe3+、Al3+的影响最为显著,随着Fe3+、Al3+浓度的增加,晶体的长径比显著增大,晶体由棱柱状变为针状,诱导时间延长,晶体生长速度变小,Al3+的影响比Fe3+略大。F-浓度增大,晶体的长径比反而变小。SO42-浓度增大,平均粒径先减小后由于生成聚晶而增大,晶形仍为棱柱状,单晶长径比先缓慢增大而后略有减小。掺杂Ca2+、Mg2+对晶形影响很小。研究结果对于磷酸二氢钾的结晶生长条件选择有重要的参考价值。

磷酸二氢钾晶体飞切过程中温度场的分布及其对切屑形貌的影响

研究了磷酸二氢钾(KDP)晶体飞切加工过程中温度场的分布,探索了切削温度对KDP晶体切削过程的影响。首先,采用热力耦合有限元分析对KDP晶体切削过程进行了仿真,获得了不同切削深度下材料内部温度场的分布。分别使用飞切机床和纳米压痕仪在不同速度下切削KDP晶体,发现不同切削速度下形成的切屑的微观形貌存在显著差异,分析指出这可能是由于在不同切削速度下切削区域温度差异导致的。最后,对低速加工过程中获得的切屑进行加热试验,并观测了不同温升条件下切屑微观形貌的变化。飞切加工仿真实验显示:当切深为200nm时,切削区域的温度达到110℃;而实际实验结果表明:当温度超过100℃时,切屑的微观形貌会发生明显变化。综合仿真及实验结果可知:在KDP晶体飞切加工过程中切削区域的温度将超过100℃,因此在对KDP晶体切削机理进行研究时,必须考虑温度对材料力学性能及其去除过程的影响。

磷酸二氢钾结晶的影响因素研究

采用间歇实验法研究了pH、降温速率等条件和铁(Ⅲ)、氟杂质对磷酸二氢钾结晶过程的影响。结果表明:在pH为3.0时,结晶析出温度和结晶析出量均最大,随着pH增加,颗粒聚集明显,表观粒径增大;随着降温速率的增大,结晶速度逐渐增大,晶体平均粒径减小,介稳区宽度逐渐增大,结晶的成核级数为4;杂质铁(Ⅲ)对结晶影响显著,随着铁(Ⅲ)质量分数的增加,晶体的长径比明显增大,晶形由棱柱状变为针状,介稳区明显变宽,结晶诱导期明显延长;杂质氟对结晶影响较小,随着氟质量分数的增加,介稳区宽度变宽,单晶长径比减小,晶形由长柱状变为方柱状,最后变为短粗状;在有氟存在时,比溶液中只掺杂铁(Ⅲ)时所得晶体的长径比减小,但结晶改善的效果并不理想。实验结果对磷酸二氢钾的生产过程有指导意义。