离子束作用下KDP晶体表面粗糙度研究

为了避免传统加工过程对KDP( Potassium dihydrogen phosphate)晶体表面产生损伤、嵌入杂质等降低晶体抗激光损伤阈值的不利因素,文章探索采用离子束抛光技术实现KDP晶体的加工.本文主要分析了离子束抛光作用下KDP晶体表面粗糙度的演变过程,采用垂直入射和倾斜45°入射两种方式研究KDP晶体表面粗糙度,利用倾斜45°入射的加工方式提高了KDP晶体的表面质量,其表面均方根粗糙度值由初始的3.07 nm减小到了1.95 nm,实验结果验证了离子束抛光加工KDP晶体的可行性.     

KDP晶体金刚石线锯切割表面缺陷分析

采用树脂金刚石线锯对KDP晶体进行了锯切实验,使用扫描电子显微镜对KDP晶体锯切的表面缺陷进行了分析,分析了走丝速度和工件进给速度对KDP晶体表面缺陷特征的影响.分析发现线锯锯切的晶片表面缺陷主要有呈锯齿状形态的沟槽、表面破碎、划痕、橘皮状的外观、凹坑、以及锯切表面嵌入脱落磨粒和切屑.走丝速度增大,工件进给速度降低,锯切材料的表面缺陷逐渐由以脆性破碎凹坑为主转变为以材料微切削去除留下的沟痕为主.锯丝表面脱落的金刚石磨粒在锯切过程中在锯丝压力作用下挤压嵌入或冲击加工表面造成凹坑,对材料表面和亚表面质量的损害严重.其分析结果为获得高质量的锯切表面,进一步优化工艺参数提供了实验参考依据.     

Ca^2＋对KDP晶体的光损伤阈值的影响

Ca2 是KDP原料中一种常见的杂质离子,这种杂质不仅会影响晶体的生长过程,而且会加重晶体的光散射.通过传统降温法和点籽晶快速生长法生长不同Ca2 掺杂浓度的KDP晶体样品,对样品进行激光损伤实验,结果表明,Ca2 的存在降低了KDP晶体的光损伤阈值,其原因主要在于Ca2 掺杂导致晶体内部缺陷增多,内应力增加以及晶体中的散射颗粒密度增大使晶体光吸收加重.     

pH值对KDP晶体溶解度和溶液稳定性的影响

测定了不同pH值(2.0～5.5)生长溶液中KDP晶体(KH2PO4)的溶解度曲线,实验结果表明:随着生长溶液pH值的改变,KDP溶解度明显增大.讨论了KDP晶体溶液pH值、溶液组成和溶液饱和点温度三者之间的关系.进行了高pH值(3.8～5.6)KDP生长溶液的稳定性实验,发现高pH值生长溶液中的临界成核半径rC增大,溶液的稳定性提高.在不同pH值溶液中进行了晶体生长实验,探讨了不同pH值生长溶液中配合物对KDP晶体生长习性的影响.     

Na+对KDP晶体生长的影响

本文利用传统的降温法和"点籽晶"快速生长法在不同Na+掺杂浓度的溶液中生长KDP晶体,定量研究了Na+对KDP晶体生长的影响.实验发现:Na+的存在降低了溶液的稳定性,致使KDP晶体柱面容易扩展.Na+的存在对KDP晶体的光学性能基本没有影响.     

磷含量对金刚石镀层形貌及其加工性能的影响

通过化学镀方法,在金刚石颗粒表面制备一层不同P含量的Ni-P合金层;利用SEM分析了镀层的微观形貌;并用其制备了固结磨料研磨垫,比较了不同P含量金刚石研磨垫在加工过程中的摩擦系数、声发射信号及研磨垫的耐磨性;探索了不同研磨垫的加工特性;并与电镀镍金刚石进行了对比.结果表明:金刚石镀层P含量能够明显改变金刚石的形貌;研磨过程中的摩擦系数、材料去除速率和工件表面粗糙度随着P含量的增加呈先增大后减小的趋势;中磷金刚石磨粒对工件的摩擦力和切入深度最大,研磨垫的磨粒保持性与自修整性平衡;电镀金刚石表面粗糙度及加工性能介于低磷与中磷之间.     

纳米尺度延性域干切削KDP晶体的无粘屑研究

为了避免使用切削液及其相应清洗工艺对KDP晶体表面产生雾化、引入杂质等降低晶体抗激光损伤阈值的不利因素,采用干切削技术对KDP晶体进行超精密切削.在干切削KDP晶体工艺中所遇到的难点是切削屑片易粘附已加工表面,由此产生屑片粘附点难清洗、易雾化等问题.本文提出了基于真空抽屑装置干切削KDP晶体的新工艺,重点解决了干切削工艺下KDP晶体表面粘屑现象,实现了无需清洗、无杂质的加工表面.在选择延性域切削参数条件下,取得了表面粗糙度为2.69 nm(Ra)的无粘屑、超光滑表面.     

KDP晶体各向异性力学特性分析

利用压痕实验研究了KDP晶体在(001)晶面不同晶向上的硬度和断裂韧性力学特性,在此基础上利用划痕实验对(001)晶面不同晶向上的脆塑性转变点位置进行了研究.结果表明:在KDP晶体(001)晶面的[110]晶向上硬度值最小,断裂韧性值最大,最易产生塑性变形,最不易产生脆性断裂,在该方向上可以得到较大的临界切削深度,而在[100]晶向上硬度最大,最易产生脆性断裂,不易产生塑性变形,临界切削深度最小.此研究结果为磨削实验提供指导意义,即在(001)晶面上沿[110]晶向能加工出表面质量较好的KDP晶体.     

LBO晶体超光滑表面抛光机理

胶体SiO2抛光LBO晶体获得无损伤的超光滑表面,结合前人对抛光机理的认识,探讨了超光滑表面抛光的材料去除机理,分析了化学机械抛光中的原子级材料去除机理.在此基础上,对胶体SiO2抛光LBO晶体表面材料去除机理和超光滑表面的形成进行了详细的描述,研究抛光液的pH值与材料去除率和表面粗糙度的关系.LBO晶体超光滑表面抛光的材料去除机理是抛光液与晶体表面的活泼原子层发生化学反应形成过渡的软质层,软质层在磨料和抛光盘的作用下很容易被无损伤的去除.酸性条件下,随抛光液pH值的减小抛光材料的去除率增大;抛光液pH值为4时,获得最好的表面粗糙度.     

KDP晶体缺陷对生长应力分布的影响

本文采用有限元法分析了不同尺寸、形状的晶体缺陷对大口径KDP晶体生长应力分布的影响.结果表明,晶体中的缺陷导致了晶体内部应力集中,且应力集中程度与缺陷尺寸、晶体生长尺寸呈反向变化,而最大主应力与缺陷尺寸、晶体生长尺寸呈正向变化.当缺陷含有棱边或尖角时,应力集中程度和最大主应力值都明显增加.由于KDP晶体易脆性开裂,随着最大主应力值的增大,开裂机率也增大.     

单晶蓝宝石球罩的磁控研磨试验研究

开展了金刚石磁性磨料在磁场控制下研磨加工单晶蓝宝石球罩的实验,研究了研磨压力、研磨时间、乙二胺浓度等因素对单晶蓝宝石球罩材料去除率及面粗糙度的影响.实验结果表明:随着研磨压力的增大,材料去除率增加但增幅减小,面粗糙度Sa也降低,降低幅度也减小.当乙二胺浓度为3;,研磨压力为25 kPa时,材料去除率在前30 min能保持在5μm·h-1以上,但在30 min之后,材料去除率开始出现较大幅度的下降,面粗糙度Sa在前30 min较为快速地降低到110 nm左右,后30 min略有降低.     

Fe3+对KDP晶体生长影响的研究

金属离子对KDP晶体的影响是多方面的.本文采用不同的过饱和度,在不同的Fe3+掺杂浓度的生长溶液中生长KDP晶体,定量地研究了Fe3+对KDP晶体生长的影响.实验发现,无论是在高过饱和度还是在低过饱和度下生长KDP晶体,在一定的浓度范围内,Fe3+的掺入既可以增加生长溶液的稳定性,又可以有效抑制晶体柱面的扩展,而且晶体基本不楔化,同时,对晶体光学性能的影响也不大.     

Improvement of growth habit and optical properties of rapidly grown KDP crystal by adding diethylene triamine pentacetate acid in growth solution

By altering the concentration of a new additive ‐ diethylene triamine pentacetate acid (DTPA) in the growth solution, a series of KDP crystals were obtained by the “point seed” rapid growth method. The growth rates up to about 20 mm/day. Effects of DTPA on the growth habit and optical properties of these as‐grown KDP crystals were investigated. The results reveal that, with the increase of DTPA concentration in growth solution, the contents of impurity metal ions incorporated into crystal and aspect ratio of crystal morphology were both decreased gradually, while the UV transmittance of crystal was enhanced continually. In the presence of moderate concentration of DTPA (100–200 ppm), the solution stability was increased and optical properties of crystal (including optical homogeneity, light scattering and laser damage threshold) were all improved. However excessive doping (>500 ppm) has opposite effects. The impact mechanism was also analyzed combining with the structure of KDP crystal and chemical characteristics of DTPA molecular.     

Single crystal growth,structural, optical,mechanical, dielectric and thermal studies of formic acid doped potassium dihydrogen phosphate crystal for NLO applications

Optically transparent formic acid (FA) doped potassium dihydrogen phosphate (KDP) crystal of dimension 21×15×9 mm³ has been grown by slow evaporation solution technique (SEST). The X‐ray diffraction (XRD) technique was used to confirm the cell parameters and the shifts in peak positions of identified reflecting planes. The incorporation of FA in KDP has been qualitatively analyzed by fourier transform infrared analysis. The UV‐visible absorption spectrum of crystals has been recorded in the range of 200 to 900 nm and the doped KDP crystal is found to have improved optical parameters than pure KDP. The color centered photoluminescence emission spectrum of grown crystal has been illustrated in visible region. The mechanical behavior of pure and doped KDP crystal has been investigated using the Vicker's microhardness analyzer and hardness parameters have been calculated. The effect of FA on thermal stability of KDP crystal was examined by means of thermogravimetric and differential thermal analysis. The temperature dependent dielectric behavior of crystals was studied.     

Measurement of three‐dimensional concentration gradients around a crystal growing from its aqueous solution using laser schlieren

Schlieren measurements of the gradients of the concentration field around a KDP crystal growing from its aqueous solution are reported. The measurement of the concentration gradient field is important for crystal growth because it controls the rate of solute transport from the bulk of the solution to the crystal surface. In the crystal vicinity, the concentration gradients have a three dimensional distribution. The concentration gradient field has been imaged using monochrome schlieren technique. Four view angles, namely 0, 45, 90 and 135° have been utilized. By interpreting the schlieren images as projection data of solute concentration gradient, the three‐dimensional concentration gradient field around the crystal has been determined using an algebraic reconstruction technique. At low supersaturation levels, the growth process is accompanied by weak fluid movement during which diffusion effects are significant. At higher levels of supersaturation and large crystal size, a well‐defined convective plume around the growing crystal is observed. Reconstruction of concentration gradients around the crystal explains the preferential growth rates of various faces of the crystal. The non‐circular shape of the crystal is seen to affect the symmetry of the distribution of concentration gradients in its vicinity. The effect of crystal morphology on the orientation of convection currents rising from the crystal surface has also been brought out on the basis of the reconstructed concentration gradients distribution in the growth chamber. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and high frequency dielectric study of pure and thiourea doped KDP crystals

Non linear optical (NLO) materials have acquired new significance with the advent of a large number of devices utilizing solid‐state laser sources. Several NLO materials have been used for this kind of technological applications. The Potassium di‐hydrogen phosphate (KDP) one of NLO material having superior non linear optical properties has been exploited for variety of applications. In the present investigation we have grown KDP crystals from aqous solution with thiourea, an organic non linear optical material. We could enhance the SHG efficiency of thiourea doped KDP crystal. It was 1.99 times more that of pure KDP. We observed more enhancements in nonlinearity for low concentration of thiourea.The crystal structure and cell parameters of grown crystal were determined from Powder XRD.The incorporation of thiourea in the grown crystals was qualitatively analyzed from FT‐IR study. The absorption spectra of pure and thiourea doped KDP crystal reveal that thiourea doped KDP crystals would be a better nonlinear optical (NLO) material for second harmonic generation (SHG) than pure KDP. The thermal decomposition and weight loss of pure and thiourea doped KDP crystal was observed by thermogravimetric (TGA) analysis and Differential Scanning Calorimetry (DSC). The high frequency dielectric study of pure KDP crystal, thiourea doped KDP crystals and organic additive thiourea was carried out using X‐band at frequency 8GHZ and 12GHZ by transmission line wave guide method. We observed low dielectric constant of thiourea doped KDP crystal when it is doped with 2mole% of thiourea. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

KDP晶体生长的溶液流动和物质输运计算

本文采用有限容积法,对KDP晶体生长过程中溶液的流动和物质输运进行了数值模拟.结果表明:随着入口溶液流动速度的增大,籽晶的上表面因自然对流而引起的抽吸作用减小,表面过饱和度的最小值沿x正向发生右移,其上表面的剪切力先减小后增大.随着入口溶液过饱和度的增大,籽晶上表面剪切力增大.不同尺寸的籽晶表面过饱和度的分布差异较大.籽晶的生长边界层厚度与溶液流动密切相关,入口溶液流动速度越大,厚度越小,但其受入口溶液过饱和度的影响较小.     

KDP single crystal growth via three‐dimensional motion growth method

A novel system for rapid crystal growth, namely three‐dimensional motion growth method (“3D MGM”) was proposed. Using this system, a potassium dihydrogen phosphate (KDP) seed was grown to a single crystal with a final size of 50×55×85 mm³. The KDP crystal was characterized by Raman spectroscopy, UV‐vis‐NIR spectroscopy, extinction ratio, laser damage threshold, and etching studies. Raman spectrum shows KDP crystal grown by “3D MGM” maintains good crystallinity as that grown by rotating‐crystal method (“RCM”). The “3D MGM” grown KDP crystal has much better transmittance, higher extinction ratio, higher damage threshold and less dislocation density, compared to “RCM” grown crystal.     

泥浆中磨粒对Al2O3增强Y-TZP复合陶瓷材料耐磨性的影响

在不同磨粒的5;NaOH泥浆中,采用销-盘式摩擦磨损试验机考察了磨粒对氧化铝增强四方氧化锆多晶陶瓷材料(ADZ)耐磨性的影响进行了研究.结果表明:尖锐SiO2磨粒对ADZ复合陶瓷材料磨损的影响要比球形SiO2磨粒严重得多,磨料硬度是影响陶瓷材料磨损率的重要因素,磨损率随磨粒硬度的提高而增大.在不同形状的SiO2磨粒的泥浆中,ADZ陶瓷材料的主要磨损机理为塑性变形和微犁削.在高硬度Al2O3磨料的泥浆中,ADZ陶瓷材料磨损表面以断裂机制占主导地位.