DKDP系列晶体制备及性质研究
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摘要
惯性受约核聚变(Inertial confinement fusion,简称ICF)是一种可控制的热核爆炸,是未来获取核能环保能源最有前途的手段之一。从长远看,ICF工程在解决人类未来能源短缺的问题方面具有实际的应用前景,已经受到世界各国的普遍关注。强激光频率转换晶体是ICF系统中高功率激光器的重要光学元件,尽管目前新型的非线性光学晶体材料不断涌现,但综观其光学性能和生长特性,到目前为止,能满足ICF研究所需要的高激光损伤阈值大尺寸晶体,也仅有磷酸二氢钾/氘化磷酸二氢钾(KDP/DKDP)晶体。DKDP晶体在ICF工程中作为三倍频晶体最大优点在于其可以有效降低高功率密度激光下所产生的受激拉曼散射波(SRS)。但是目前生长出来的晶体的激光损伤阈值还是比理论计算出来的结果低一个数量级,这严重限制了激光输出的能量密度和晶体使用寿命,成为制约惯性约束聚变发展和应用的瓶颈。如何提高DKDP晶体的光损伤阈值一直是国内外研究的热点。
激光引起光学元件的损伤是一个复杂的过程,它由激光参数和元件性质两方面决定。光学材料的物理性质对其激光损伤有明显影响,目前对它们之间的关系还未完全了解,但是有些研究结论还是得到了较普遍的肯定。了解材料和元件的物理参数对预测激光诱导损伤的可能性非常重要。本文生长制备了系列氘含量DKDP晶体,并按照“0902”要求利用不同原料和方法生长了晶体氘含量为80%的DKDP晶体；从DKDP晶体材料力学、热学、电学、光学等基本性能与结构之间的关系入手,探讨三倍频DKDP晶体损伤产生的材料影响因素,结合对特定激光参数下DKDP晶体的损伤特性规律研究,为使用者提供参考。
1.采用点籽晶快速法生长了系列不同氘含量DKDP晶体,其次采用不同原料、不同生长方法生长了80%DKDP晶体,对这些晶体的生长过程进行了研究,同时还对系列氘含量晶体的晶胞参数和结构完整性进行了分析。
A原料所配置的溶液稳定性不高,生长过程中容易出杂晶,并且杂晶生长较快；B原料料所配溶液稳定性较好,后期溶液中出现絮状不溶物,但是溶液中没有出现杂晶,晶体正常生长；C原料溶液中后期也出现杂晶,但是杂晶生长速度较慢,对晶体生长影响较小。对比研究发现,原料纯度较高时,杂质离子含量低,对晶体柱面的阻碍作用较小,有利于晶体的快速生长。
快速生长的晶体中吸附的杂质金属离子含量要明显多于传统法生长的晶体。传统晶体中杂质金属离子含量分布较均匀,锥头和帽区附近金属离子含量没有明显的差别。而对于快速生长的晶体,柱面区杂质金属离子含量相对于锥面区明显更高。
低氘晶体和高氘晶体可以分别看作是低掺氘KDP晶体和低掺氢DKDP晶体,这说明少量的掺杂会降低晶体的结构完整性。而处于中间浓度的晶体结晶完整性较好。
2.测定了点籽晶技术生长的系列氘含量DKDP晶体的(001)面、(100)面和三倍频面在载荷从5g到100g的变化范围内的维氏硬度指数。基于KDP晶体力学性质分析了不同载荷、不同面上的压痕。随着晶体中氘含量的增加,晶体不同面的维氏硬度逐渐较小。这种结果主要是由于氢键在氘对氢取代之后结合力变弱所致。我们认为氢键对影响晶体硬度起到主要的作用。由于O-H键平行于[100]和[010]方向,不同面的硬度出现了明显的各向异性。K(H1-xDx)2PO4晶体的加工硬化系数随着晶体氘含量的增加而逐渐增大,这跟实验得到的维氏硬度结果是相一致的。
3.对不同氘含量DKDP晶体的热学性质进行了详细的测试,包括比热、热膨胀、热导率等。实验发现,受生长条件的影响,氘含量对晶体热学性质的影响不明显。我们测试所得的系列氘含量晶体的比热与理论计算(135.97g·mol-1)相差不多,这表明在测试的温度范围之内,K(H1-xDx)2PO4晶体的比热符合杜隆—珀替定律和柯普定律。此外随着氘含量的增加,晶体的相转变温度和相变潜热基本有一个下降的趋势。
随着温度的升高,晶体a方向和c方向的热膨胀系数先缓慢增大,最后趋于平稳。随着晶体氘含量的增加,晶体的两个方向上的热膨胀系数比率(c/a)有增大的趋势。这表明,在晶体中掺入氘量增大,晶体的各向异性增大,在生长或者切割过程中受开裂影响更大。
4.测试了点籽晶快速法生长的系列氘含量DKDP晶体的电学性质,包括电导率、介电常数、弹性常数、压电常数。
DKDP晶体的电导率随着晶体中氘含量的增加而增大。而且,根据电导率的变温测试结果,晶体电导活化能随着氘含量的增加逐渐减小。目前的结果证实了氘原子在氢键上隧穿频率要比氢原子小,这可能是导致KDP晶体的电导率在氘取代氢之后增大的原因。
DKDP晶体的介电常数随着晶体中氘含量的增加而逐渐增大,沿着a方向的相对介电常数大于沿着c方向的介电常数,但沿着c方向的相对介电常数增大的更快。随着外加电场频率的增大,各氘含量晶体的相对介电常数是逐渐增大的,并且相对介电常数ε11比ε33增大的更快。
实验确认了KDP晶体的弹性顺度常数sll约为31pm2N-1,这与前人报道有一定区别。在所有弹性常数中s11，s44,和s66相对较大。而且,随着晶体氘含量的增加,s11，s44,和s66逐渐的增大,但是s12,s13,和s33没有明显的变化。
DKDP晶体的压电常数d36随着晶体中氘含量的增加而增大,但是d14的这种趋势很微小。这是由于氘取代氢之后,P04四面体中P-O键长增大P04更容易发生变形所致。随着氘含量的增加,压电应变常数e36逐渐增大,e14基本没有变化。机电耦合系数kij的变化遵循相同的规律。
5.对系列氘含量DKDP晶体和不同原料、方法生长的80%DKDP晶体的光学性质,包括透过光谱、系列氘含量晶体的拉曼光谱、激光损伤阈值和损伤特性进行了研究。
随着晶体氘含量的增加,晶体的透过光谱范围变大,红外部分透过向更长波长处移动,这种变化是由于氢键中氢原子被氘原子取代所致,D-O键相比于H-O键的结合力更弱。对于80%DKDP晶体,传统法生长的晶体在紫外区域的透过率要比快速法生长的晶体明显要高。在800～1900nm波长范围内传统法生长的晶体比快速法生长的晶体的透过范围更宽。
系列氘含量DKDP晶体的偏振拉曼光谱测试表明,随着氘含量的增加,(H/D)2PO4阴离子基团内振动模的拉曼峰出现红移,这是由于氘取代氢之后P-O键的结合力变弱所致。此外,随着晶体中氘含量的增加,X(YY) X和X(ZZ)X两种配置下最强峰的峰强呈现先减后增的趋势,在晶体氘含量约为74%时达到最小值。从应用的角度看,这个结果对选择何种氘含量的DKDP晶体作为高功率大口径激光系统中三倍频晶体有一定的参考价值。
z切样品的阈值高于三倍频切样品,我们推测DKDP晶体的本征力学性能各向异性和晶体中非球吸收体的存在导致了激光损伤阈值的方向性。DKDP晶体的激光损伤阈值随着氘化程度的增加而降低,这种结果归因于随着氘化程度增加晶体结构中主要方向上化学键强度的逐渐降低。在相同的生长温度下,DKDP晶体的激光损伤阈值与原料(主要金属杂质含量在lppm以下)的纯度关系不大,但是采用高纯原料有助于晶体均匀性的提高。对于传统生长的晶体,从低密度区域(靠近锥头)取出的样品的激光损伤阈值更高。
1064nm激光作用下,损伤点是由中心点、定向裂纹和周围微变化区域组成,中心点空洞尺寸在2-30μm之间,主要为6-81μm。355nm激光作用下损伤点也是由中心点、周围微变化区域组成,偶尔会存在定向裂纹,中心点的尺寸1-10μm,大部分在5μm以下。相比较1064nm光损伤,355nm光损伤点密度更大,尺寸更小。此外,单晶中激光诱导损伤的形状有一定规律,这跟晶体的弹性对称性有关。拉曼测试表明,表损伤点的物质形态有一定变化但还不明确,有待进一步实验研究。
Inertial Confinement Fusion (ICF) is a kind of heat nuclear explosion that can be controlled in the laboratory, which will be one of the most promising methods for generating environmentally safe energy in the future. In the long tern, the ICF has the practical applied prospect in overcoming the shortage of energy for human being. The frequency conversion crystal is an important optical element in the high power laser system for ICF. At present, a large number of novel nonlinear optical crystals are constantly emerging. However, KDP and DKDP crystal is only one crystal with high laser induced damage threshold and large size that could meet the requirement of ICF research. The advantage of DKDP crystal used as third harmonic generation (THG) crystal in ICF project is for minimizing the stimulated Raman scattering caused by high power laser. Whereas the intrinsic breakdown of pure material is one order of magnitude above the maximum laser energy considered in these facilities, experiments showed that laser damage actually occurs at fluences below the maximum energy delivered. This problem greatly limits the fluence of output laser and the crystal's useful life. The way to improve the laser induced damage resistance of as-grown crystals is by far the most challenging problem for DKDP performance.
Laser induced damage of optics has a very complex process, which decided by both laser parameters and properties of material. The physical properties of optical material have an obvious influence on the laser damage. Although the relationship between the properties of material and laser damage has not been cleared yet, some results have been widely confirmed. The study on the properties of material and the physical parameters of optical element is important for forecasting possibility of laser induced damage. In present work, a series of DKDP crystals with different deuteration levels and80%DKDP crystals grown with different KH2PO4raw materials by two growth methods were prepared. The mechanical, thermal, electrical and optical property of DKDP crystal were measured and analyzed with its structure for investigating the effect of material on laser damage of DKDP crystal for THG. The behavior of laser damage with specified laser parameter was investigated to provide references for users.
1. A series of DKDP crystals with different deuteration levels were rapidly grown by point seed technique. In addition,80%DKDP crystals were grown by both traditional method and rapid method with different raw material. The growth phenomenon of these crystals was described and summarized. The cell parameters and crystalline perfection of DKDP crystals with different deuteration levels were measured.
The stability of growth solution prepared with high pure raw material is poor with respect to other two low pure materials. The content of metalline ion impurities in rapid growth crystal is obviously higher than that of crystal grown by traditional method. The distribution of metalline ion impurities in crystal grown by traditional method is uniform. The content of impurities in prismatic sector of the rapid crystal is higher with respect to pyramidal sector. The crystalline perfection of crystals with low deuteration level and high deuteration level is inferior compared to that of the crystals with in-between deuteration level.
2. The Vickers hardness of (100),(001), and so called "tripler" faces for DKDP crystals with different deuteration levels were measured with load in the range from5to100g. The indentations made by different loads or indented on different faces were observed. The formation of cracks was analyzed. Initially the hardness number of (001) face for each crystal increases with the increase of the applied load until it reaches25g. With further increase in load, the hardness number decreases gradually. The hardness numbers decline with the increase in deuterium content. These composition dependences are expected since the bond strength is weakened by the substitution of deuterium for hydrogen. The hydrogen bond is considered to play the key role in effecting the crystal's hardness. The visible hardness anisotropy of the different faces is attributed to the inhomogeneous distribution of the oxygen-hydrogen bond on these faces.
3. The thermal parameters such as specific heat, thermal expansion and thermal conductivity of DKDP crystals with different deuterium contents were measured. The results show that the effect of deuteration level on the thermal property of DKDP crystal is obscure influenced by growth conditions. In test temperature range, the measured specific heat of K(H1-xDx)2PO4crystals is in accord with the value calculated on the basis of Dulong-Petit law and Neumann-Kopp law. With the increase of deuterium content, the phase transition temperature and the phase transition latent heat of DKDP crystal show a decreasing trend. Moreover, the thermal expansion ratio (c/a) is increasing. It means that the mechanical anisotropy of DKDP increases with increasing deuteration level.
4. The electrical conductivity, dielectric constants, elastic constants, piezoelectric constants of DKDP crystals with different deuteration levels were measured.
The electrical conductivities of these crystals were measured along a and c directions at room temperature. The electrical conductivity increases with the increase for deuterium content. Also the electrical conductivities of certain crystals were measured at various temperatures ranging from20to130℃. The values of activation energy decrease as the increase of deuterium content. The present study indicates that the deuterium tunneling frequency is smaller than that of hydrogen, which may be the reason why the variation of electrical conductivity happens after the substitution of deuterium for hydrogen in KDP crystal.
With the increase of deuterium content, the dielectric constants of these DKDP crystals increase gradually. The dielectric constants along a direction are larger that those along c direction. The dielectric constant along a direction increases more rapidly than that along c direction. Moreover, the dielectric constant increases with the increase of frequency of applied electrical field. Similarly, the dielectric constant along a direction increases more rapidly.
The elastic compliant constant s11of KDP crystal is measured and certified approximately as31pm2N-1by many tests, which is different with the values reported previously. In all elastic constants, the s11, s44, s66are larger than the others. With the content of deuterium increasing, s11, s44, s66gradually increase respectively, whereas s12, s13, S33have no demonstrable variation.
The d36of DKDP crystal increases with the increase in deuterium content, and this trend for d14is slight. The length of the P-O bond increases with increasing deuterium content, which may be the cause of the variation of piezoelectric properties with the increase in deuterium content. The piezoelectric stress constant e14has no change, while e36increases with increasing content of deuterium. The electromechanical coupling coefficients kij follow a similar rule.
5. The transmission spectra of DKDP crystals with different deuteration levels and80%DKDP crystals are measured. With the increase of deuterium content, the transmission spectra become wide and the infrared regions shift to longer wavelength. This variation arises from the substitution from Hydrogen to Deuterium in bonds with oxygen atoms. For80%DKDP crystal, the transmission in the UV region of crystal grown by traditional method is clearly higher than that of crystal grown by rapid technique. Moreover, the transmission in the range from800to1900nm of crystal grown by traditional method is wider than that of crystal by rapid method.
The polarized Raman spectra of DKDP crystals with different deuterium concentrations were measured. With the increasing deuterium content, the red-shift of the Raman peaks which are assigned as the internal vibrations of the (H/D)2PO4-anion is contributed to the decrease in the bonding force of P-O bond influenced by the substitution of deuterium for hydrogen. Moreover, the intensity of the strongest peak of these crystals decreases first, and increases with the increasing deuterium concentration. It reaches its minimum value while the mole percentage of the deuterium content in the crystal is about74%.
The laser induced damage thresholds of z cut and tripler cut samples for DKDP crystals with different deuterium contents were measured by1-on-1test at355nm. Laser induced damage threshold of z cut sample is higher than that of tripler cut sample. The intrinsic mechanical anisotropy of DKDP crystals and the existence of non-spherical absorbers are speculated to analyze the orientation dependence of laser induced damage threshold. In addition, the laser induced damage threshold decreases with the increase of deuterated degree. The dependence of laser induced damage threshold on deuterium content is mainly due to the decline of bond strength in primary crystallographic directions with the increase of deuterated degree. At constant growth temperature, damage resistance in DKDP is fairly independent of raw material with the mass content of main metallic ionic impurity below1ppm. However, DKDP crystal grown with high pure material has an excellent homogeneity. The samples cut from pyramidal head region have higher laser induced damage threshold with respect to those cut from other regions.
The1064nm laser damage morphology consists of three distinct regions:a core, some oriented cracks spreading from the core, and a region of modified material surrounding the core. The size of the core is about2-30μm. Most of the355nm laser damage sites consist of two distinct regions:a core and a region of modified area surrounding the core. A few of355nm laser damage sites contain the oriented crack, which occurred frequently in1064nm laser damage sites. Moreover, the morphology of laser damage sites in single crystal is dependent on the crystallographic symmetry. The Raman tests show that the material in the damage site has been modified from the bulk material. However, the results are not clear and need to be studied further.
激光引起光学元件的损伤是一个复杂的过程,它由激光参数和元件性质两方面决定。光学材料的物理性质对其激光损伤有明显影响,目前对它们之间的关系还未完全了解,但是有些研究结论还是得到了较普遍的肯定。了解材料和元件的物理参数对预测激光诱导损伤的可能性非常重要。本文生长制备了系列氘含量DKDP晶体,并按照“0902”要求利用不同原料和方法生长了晶体氘含量为80%的DKDP晶体；从DKDP晶体材料力学、热学、电学、光学等基本性能与结构之间的关系入手,探讨三倍频DKDP晶体损伤产生的材料影响因素,结合对特定激光参数下DKDP晶体的损伤特性规律研究,为使用者提供参考。
1.采用点籽晶快速法生长了系列不同氘含量DKDP晶体,其次采用不同原料、不同生长方法生长了80%DKDP晶体,对这些晶体的生长过程进行了研究,同时还对系列氘含量晶体的晶胞参数和结构完整性进行了分析。
A原料所配置的溶液稳定性不高,生长过程中容易出杂晶,并且杂晶生长较快；B原料料所配溶液稳定性较好,后期溶液中出现絮状不溶物,但是溶液中没有出现杂晶,晶体正常生长；C原料溶液中后期也出现杂晶,但是杂晶生长速度较慢,对晶体生长影响较小。对比研究发现,原料纯度较高时,杂质离子含量低,对晶体柱面的阻碍作用较小,有利于晶体的快速生长。
快速生长的晶体中吸附的杂质金属离子含量要明显多于传统法生长的晶体。传统晶体中杂质金属离子含量分布较均匀,锥头和帽区附近金属离子含量没有明显的差别。而对于快速生长的晶体,柱面区杂质金属离子含量相对于锥面区明显更高。
低氘晶体和高氘晶体可以分别看作是低掺氘KDP晶体和低掺氢DKDP晶体,这说明少量的掺杂会降低晶体的结构完整性。而处于中间浓度的晶体结晶完整性较好。
2.测定了点籽晶技术生长的系列氘含量DKDP晶体的(001)面、(100)面和三倍频面在载荷从5g到100g的变化范围内的维氏硬度指数。基于KDP晶体力学性质分析了不同载荷、不同面上的压痕。随着晶体中氘含量的增加,晶体不同面的维氏硬度逐渐较小。这种结果主要是由于氢键在氘对氢取代之后结合力变弱所致。我们认为氢键对影响晶体硬度起到主要的作用。由于O-H键平行于[100]和[010]方向,不同面的硬度出现了明显的各向异性。K(H1-xDx)2PO4晶体的加工硬化系数随着晶体氘含量的增加而逐渐增大,这跟实验得到的维氏硬度结果是相一致的。
3.对不同氘含量DKDP晶体的热学性质进行了详细的测试,包括比热、热膨胀、热导率等。实验发现,受生长条件的影响,氘含量对晶体热学性质的影响不明显。我们测试所得的系列氘含量晶体的比热与理论计算(135.97g·mol-1)相差不多,这表明在测试的温度范围之内,K(H1-xDx)2PO4晶体的比热符合杜隆—珀替定律和柯普定律。此外随着氘含量的增加,晶体的相转变温度和相变潜热基本有一个下降的趋势。
随着温度的升高,晶体a方向和c方向的热膨胀系数先缓慢增大,最后趋于平稳。随着晶体氘含量的增加,晶体的两个方向上的热膨胀系数比率(c/a)有增大的趋势。这表明,在晶体中掺入氘量增大,晶体的各向异性增大,在生长或者切割过程中受开裂影响更大。
4.测试了点籽晶快速法生长的系列氘含量DKDP晶体的电学性质,包括电导率、介电常数、弹性常数、压电常数。
DKDP晶体的电导率随着晶体中氘含量的增加而增大。而且,根据电导率的变温测试结果,晶体电导活化能随着氘含量的增加逐渐减小。目前的结果证实了氘原子在氢键上隧穿频率要比氢原子小,这可能是导致KDP晶体的电导率在氘取代氢之后增大的原因。
DKDP晶体的介电常数随着晶体中氘含量的增加而逐渐增大,沿着a方向的相对介电常数大于沿着c方向的介电常数,但沿着c方向的相对介电常数增大的更快。随着外加电场频率的增大,各氘含量晶体的相对介电常数是逐渐增大的,并且相对介电常数ε11比ε33增大的更快。
实验确认了KDP晶体的弹性顺度常数sll约为31pm2N-1,这与前人报道有一定区别。在所有弹性常数中s11，s44,和s66相对较大。而且,随着晶体氘含量的增加,s11，s44,和s66逐渐的增大,但是s12,s13,和s33没有明显的变化。
DKDP晶体的压电常数d36随着晶体中氘含量的增加而增大,但是d14的这种趋势很微小。这是由于氘取代氢之后,P04四面体中P-O键长增大P04更容易发生变形所致。随着氘含量的增加,压电应变常数e36逐渐增大,e14基本没有变化。机电耦合系数kij的变化遵循相同的规律。
5.对系列氘含量DKDP晶体和不同原料、方法生长的80%DKDP晶体的光学性质,包括透过光谱、系列氘含量晶体的拉曼光谱、激光损伤阈值和损伤特性进行了研究。
随着晶体氘含量的增加,晶体的透过光谱范围变大,红外部分透过向更长波长处移动,这种变化是由于氢键中氢原子被氘原子取代所致,D-O键相比于H-O键的结合力更弱。对于80%DKDP晶体,传统法生长的晶体在紫外区域的透过率要比快速法生长的晶体明显要高。在800～1900nm波长范围内传统法生长的晶体比快速法生长的晶体的透过范围更宽。
系列氘含量DKDP晶体的偏振拉曼光谱测试表明,随着氘含量的增加,(H/D)2PO4阴离子基团内振动模的拉曼峰出现红移,这是由于氘取代氢之后P-O键的结合力变弱所致。此外,随着晶体中氘含量的增加,X(YY) X和X(ZZ)X两种配置下最强峰的峰强呈现先减后增的趋势,在晶体氘含量约为74%时达到最小值。从应用的角度看,这个结果对选择何种氘含量的DKDP晶体作为高功率大口径激光系统中三倍频晶体有一定的参考价值。
z切样品的阈值高于三倍频切样品,我们推测DKDP晶体的本征力学性能各向异性和晶体中非球吸收体的存在导致了激光损伤阈值的方向性。DKDP晶体的激光损伤阈值随着氘化程度的增加而降低,这种结果归因于随着氘化程度增加晶体结构中主要方向上化学键强度的逐渐降低。在相同的生长温度下,DKDP晶体的激光损伤阈值与原料(主要金属杂质含量在lppm以下)的纯度关系不大,但是采用高纯原料有助于晶体均匀性的提高。对于传统生长的晶体,从低密度区域(靠近锥头)取出的样品的激光损伤阈值更高。
1064nm激光作用下,损伤点是由中心点、定向裂纹和周围微变化区域组成,中心点空洞尺寸在2-30μm之间,主要为6-81μm。355nm激光作用下损伤点也是由中心点、周围微变化区域组成,偶尔会存在定向裂纹,中心点的尺寸1-10μm,大部分在5μm以下。相比较1064nm光损伤,355nm光损伤点密度更大,尺寸更小。此外,单晶中激光诱导损伤的形状有一定规律,这跟晶体的弹性对称性有关。拉曼测试表明,表损伤点的物质形态有一定变化但还不明确,有待进一步实验研究。
Inertial Confinement Fusion (ICF) is a kind of heat nuclear explosion that can be controlled in the laboratory, which will be one of the most promising methods for generating environmentally safe energy in the future. In the long tern, the ICF has the practical applied prospect in overcoming the shortage of energy for human being. The frequency conversion crystal is an important optical element in the high power laser system for ICF. At present, a large number of novel nonlinear optical crystals are constantly emerging. However, KDP and DKDP crystal is only one crystal with high laser induced damage threshold and large size that could meet the requirement of ICF research. The advantage of DKDP crystal used as third harmonic generation (THG) crystal in ICF project is for minimizing the stimulated Raman scattering caused by high power laser. Whereas the intrinsic breakdown of pure material is one order of magnitude above the maximum laser energy considered in these facilities, experiments showed that laser damage actually occurs at fluences below the maximum energy delivered. This problem greatly limits the fluence of output laser and the crystal's useful life. The way to improve the laser induced damage resistance of as-grown crystals is by far the most challenging problem for DKDP performance.
Laser induced damage of optics has a very complex process, which decided by both laser parameters and properties of material. The physical properties of optical material have an obvious influence on the laser damage. Although the relationship between the properties of material and laser damage has not been cleared yet, some results have been widely confirmed. The study on the properties of material and the physical parameters of optical element is important for forecasting possibility of laser induced damage. In present work, a series of DKDP crystals with different deuteration levels and80%DKDP crystals grown with different KH2PO4raw materials by two growth methods were prepared. The mechanical, thermal, electrical and optical property of DKDP crystal were measured and analyzed with its structure for investigating the effect of material on laser damage of DKDP crystal for THG. The behavior of laser damage with specified laser parameter was investigated to provide references for users.
1. A series of DKDP crystals with different deuteration levels were rapidly grown by point seed technique. In addition,80%DKDP crystals were grown by both traditional method and rapid method with different raw material. The growth phenomenon of these crystals was described and summarized. The cell parameters and crystalline perfection of DKDP crystals with different deuteration levels were measured.
The stability of growth solution prepared with high pure raw material is poor with respect to other two low pure materials. The content of metalline ion impurities in rapid growth crystal is obviously higher than that of crystal grown by traditional method. The distribution of metalline ion impurities in crystal grown by traditional method is uniform. The content of impurities in prismatic sector of the rapid crystal is higher with respect to pyramidal sector. The crystalline perfection of crystals with low deuteration level and high deuteration level is inferior compared to that of the crystals with in-between deuteration level.
2. The Vickers hardness of (100),(001), and so called "tripler" faces for DKDP crystals with different deuteration levels were measured with load in the range from5to100g. The indentations made by different loads or indented on different faces were observed. The formation of cracks was analyzed. Initially the hardness number of (001) face for each crystal increases with the increase of the applied load until it reaches25g. With further increase in load, the hardness number decreases gradually. The hardness numbers decline with the increase in deuterium content. These composition dependences are expected since the bond strength is weakened by the substitution of deuterium for hydrogen. The hydrogen bond is considered to play the key role in effecting the crystal's hardness. The visible hardness anisotropy of the different faces is attributed to the inhomogeneous distribution of the oxygen-hydrogen bond on these faces.
3. The thermal parameters such as specific heat, thermal expansion and thermal conductivity of DKDP crystals with different deuterium contents were measured. The results show that the effect of deuteration level on the thermal property of DKDP crystal is obscure influenced by growth conditions. In test temperature range, the measured specific heat of K(H1-xDx)2PO4crystals is in accord with the value calculated on the basis of Dulong-Petit law and Neumann-Kopp law. With the increase of deuterium content, the phase transition temperature and the phase transition latent heat of DKDP crystal show a decreasing trend. Moreover, the thermal expansion ratio (c/a) is increasing. It means that the mechanical anisotropy of DKDP increases with increasing deuteration level.
4. The electrical conductivity, dielectric constants, elastic constants, piezoelectric constants of DKDP crystals with different deuteration levels were measured.
The electrical conductivities of these crystals were measured along a and c directions at room temperature. The electrical conductivity increases with the increase for deuterium content. Also the electrical conductivities of certain crystals were measured at various temperatures ranging from20to130℃. The values of activation energy decrease as the increase of deuterium content. The present study indicates that the deuterium tunneling frequency is smaller than that of hydrogen, which may be the reason why the variation of electrical conductivity happens after the substitution of deuterium for hydrogen in KDP crystal.
With the increase of deuterium content, the dielectric constants of these DKDP crystals increase gradually. The dielectric constants along a direction are larger that those along c direction. The dielectric constant along a direction increases more rapidly than that along c direction. Moreover, the dielectric constant increases with the increase of frequency of applied electrical field. Similarly, the dielectric constant along a direction increases more rapidly.
The elastic compliant constant s11of KDP crystal is measured and certified approximately as31pm2N-1by many tests, which is different with the values reported previously. In all elastic constants, the s11, s44, s66are larger than the others. With the content of deuterium increasing, s11, s44, s66gradually increase respectively, whereas s12, s13, S33have no demonstrable variation.
The d36of DKDP crystal increases with the increase in deuterium content, and this trend for d14is slight. The length of the P-O bond increases with increasing deuterium content, which may be the cause of the variation of piezoelectric properties with the increase in deuterium content. The piezoelectric stress constant e14has no change, while e36increases with increasing content of deuterium. The electromechanical coupling coefficients kij follow a similar rule.
5. The transmission spectra of DKDP crystals with different deuteration levels and80%DKDP crystals are measured. With the increase of deuterium content, the transmission spectra become wide and the infrared regions shift to longer wavelength. This variation arises from the substitution from Hydrogen to Deuterium in bonds with oxygen atoms. For80%DKDP crystal, the transmission in the UV region of crystal grown by traditional method is clearly higher than that of crystal grown by rapid technique. Moreover, the transmission in the range from800to1900nm of crystal grown by traditional method is wider than that of crystal by rapid method.
The polarized Raman spectra of DKDP crystals with different deuterium concentrations were measured. With the increasing deuterium content, the red-shift of the Raman peaks which are assigned as the internal vibrations of the (H/D)2PO4-anion is contributed to the decrease in the bonding force of P-O bond influenced by the substitution of deuterium for hydrogen. Moreover, the intensity of the strongest peak of these crystals decreases first, and increases with the increasing deuterium concentration. It reaches its minimum value while the mole percentage of the deuterium content in the crystal is about74%.
The laser induced damage thresholds of z cut and tripler cut samples for DKDP crystals with different deuterium contents were measured by1-on-1test at355nm. Laser induced damage threshold of z cut sample is higher than that of tripler cut sample. The intrinsic mechanical anisotropy of DKDP crystals and the existence of non-spherical absorbers are speculated to analyze the orientation dependence of laser induced damage threshold. In addition, the laser induced damage threshold decreases with the increase of deuterated degree. The dependence of laser induced damage threshold on deuterium content is mainly due to the decline of bond strength in primary crystallographic directions with the increase of deuterated degree. At constant growth temperature, damage resistance in DKDP is fairly independent of raw material with the mass content of main metallic ionic impurity below1ppm. However, DKDP crystal grown with high pure material has an excellent homogeneity. The samples cut from pyramidal head region have higher laser induced damage threshold with respect to those cut from other regions.
The1064nm laser damage morphology consists of three distinct regions:a core, some oriented cracks spreading from the core, and a region of modified material surrounding the core. The size of the core is about2-30μm. Most of the355nm laser damage sites consist of two distinct regions:a core and a region of modified area surrounding the core. A few of355nm laser damage sites contain the oriented crack, which occurred frequently in1064nm laser damage sites. Moreover, the morphology of laser damage sites in single crystal is dependent on the crystallographic symmetry. The Raman tests show that the material in the damage site has been modified from the bulk material. However, the results are not clear and need to be studied further.
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