溶胶-凝胶ZrO2-TiO2高折射率光学膜层的抗激光损伤性能研究

采用溶胶-凝胶方法制备了ZrO₂-TiO₂(Ti含量为0—100mol%)高折射率光学薄膜. 借助激光动态光散射技术研究溶胶微结构. 采用傅里叶变换红外光谱、原子力显微镜、薄膜光学常数分析仪、漫反射吸收光谱及强激光辐照实验，对膜层的结构、光学性能及抗激光损伤性能进行了系统表征. 结果显示，溶胶-凝胶工艺可以在部分牺牲折射率的情况下，使膜层的抗激光损伤性能得到大幅度提升. 随Ti含量从0mol%增加至100mol%，膜层的平均损伤阈值呈下降趋势，当Ti含量从0mol%增加至60mol%时，平均损伤阈值从57.1J/cm²下降到21.1J/cm²(辐照激光波长为1053nm，脉冲宽度为10ns，“R/1”测试模式)，当Ti含量从60mol%增加至100mol%时，平均损伤阈值变化很小. 综合溶胶微结构、膜层光学性能和损伤实验结果可以推断，强激光诱导多光子吸收是引起膜层损伤的主要原因. 不同配比的复合膜之间光学带隙的显著差异导致相同辐照激光情况下多光子吸收的概率发生变化，从而导致损伤阈值的规律性变化. 关键词： 2-TiO₂薄膜')" href="#">ZrO₂-TiO₂薄膜 溶胶-凝胶 激光诱导损伤 光学带隙     

溶胶-凝胶法制备高折射率TiO2薄膜

 采用溶胶- 凝胶法制备了TiO₂纳米晶溶胶，并以旋涂法（spin-coating）镀制了高折射率光学薄膜。借助光散射技术和透射电镜研究了溶胶的微结构。采用原子力显微镜、场发射扫描电镜、紫外-可见-近红外光谱仪、椭偏仪、漫反射吸收光谱及强激光辐照实验，对膜层的结构、光学性能及抗激光损伤性能进行了系统的表征。结果显示:纳米晶薄膜的折射率达到了1.9，而传统的溶胶-凝胶薄膜折射率只有1.6；同时纳米晶薄膜的抗激光损伤阈值与传统的溶胶-凝胶薄膜相差不大，在1 064 nm处分别为16.3 J/cm²(3 ns脉冲) 和16.6 J/cm²(3 ns脉冲);纳米晶溶胶薄膜可以在保持较高抗激光损伤阈值情况下，大幅度提高薄膜折射率。     

PVP掺杂-ZrO2溶胶-凝胶工艺制备多层激光高反射膜的研究

以丙醇锆(ZrPr)为锆源，二乙醇胺(DEA)为络合剂，原位引入聚乙烯吡咯烷酮(PVP)，在乙醇体系中成功地合成了PVP掺杂-ZrO₂溶胶.采用旋涂法在K9玻璃基片上制备了PVP-ZrO₂单层杂化薄膜.用不同掺杂量的PVP-ZrO₂高折射率膜层与相同的SiO₂低折射率膜层交替沉积四分之一波堆高反射膜.借助小角X射线散射研究胶体微结构，用红外光谱、原子力显微镜、紫外/可见/近红外透射光谱、椭圆偏振仪以及1064nm的强激光辐照实验对薄膜的结构、光学和抗激光损伤性能进行表征.研究发现，体系组成的适当配置可以在溶胶稳定的前提下实现ZrPr的充分水解，赋予薄膜良好的结构、光学和抗激光损伤性能.杂化体系中，DEA与ZPr之间强的配合作用大大降低了ZrO₂颗粒表面羟基的活性，使得PVP大分子只是以微弱的氢键与颗粒的表面羟基作用而均匀分散于ZrO₂颗粒的周围，对颗粒的形成和生长无显著影响.因而在实验研究范围内，随PVP含量的增大，PVP-ZrO₂杂化膜层的折射率和激光损伤阈值均无显著变化.但是，薄膜中均匀分布的PVP柔性链可以有效促进膜层应力松弛，显著削弱不同膜层之间的应力不匹配程度、大大方便多层光学薄膜的制备.当高折射率膜层中PVP的质量分数达到15%—20%时，膜层之间良好的应力匹配使得多层高反射膜的沉积周期数可达到10以上.沉积10个周期的多层反射膜，在中心波长1064nm处透射率约为1.6%—2.1%，接近全反射特征，其激光损伤阈值为16.4—18.2J/cm²(脉冲宽度为1ns). 关键词： 溶胶-凝胶 2')" href="#">PVP-ZrO₂ 高反射膜 激光损伤     

大气常压等离子射流清洗溶胶-凝胶SiO_2膜表面油脂污染物

采用大气常压等离子射流技术对溶胶-凝胶SiO2膜表面的油脂污染物进行清洗。利用分光光度计、扫描电子显微镜、红外光谱仪对溶胶-凝胶SiO2膜透过率、表面形貌、化学结构进行表征,并分析清洗前后溶胶-凝胶SiO2膜的激光损伤阈值变化。损伤阈值测试表明,1064nm波长的激光损伤阈值由污染后的16.08J/cm2上升到24.41J/cm2,与污染前24.72J/cm2的损伤阈值相当。同时还获取清洗的最佳时间为10s。清洗前后,溶胶-凝胶SiO2膜保持完好,且未产生新的有机污染物。研究结果表明:大气常压等离子射流技术可对溶胶-凝胶SiO2膜表面的油脂污染物进行有效地清洗,从而提高溶胶-凝胶SiO2膜的透过率和激光损伤阈值,为高功率激光装置的稳定运行提供保障。     

PVP掺杂-ZrO2溶胶-凝胶工艺制备多层激光高反射膜的研究

以丙醇锆(ZrPr)为锆源,二乙醇胺(DEA)为络合剂,原位引入聚乙烯吡咯烷酮(PVP),在乙醇体系中成功地合成了PVP掺杂-ZrO2溶胶.采用旋涂法在K9玻璃基片上制备了PVP-ZrO2单层杂化薄膜.用不同掺杂量的PVP-ZrO2高折射率膜层与相同的SiO2低折射率膜层交替沉积四分之一波堆高反射膜.借助小角X射线散射研究胶体微结构,用红外光谱、原子力显微镜、紫外/可见/近红外透射光谱、椭圆偏振仪以及1064nm的强激光辐照实验对薄膜的结构、光学和抗激光损伤性能进行表征.研究发现,体系组成的适当配置可以在溶胶稳定的前提下实现ZrPr的充分水解,赋予薄膜良好的结构、光学和抗激光损伤性能.杂化体系中,DEA与ZrPr之间强的配合作用大大降低了ZrO2颗粒表面羟基的活性,使得PVP大分子只是以微弱的氢键与颗粒的表面羟基作用而均匀分散于ZrO2颗粒的周围,对颗粒的形成和生长无显著影响.因而在实验研究范围内,随PVP含量的增大,PVP-ZrO2杂化膜层的折射率和激光损伤阈值均无显著变化.但是,薄膜中均匀分布的PVP柔性链可以有效促进膜层应力松弛,显著削弱不同膜层之间的应力不匹配程度、大大方便多层光学薄膜的制备.当高折射率膜层中PVP的质量分数达到15%-20%时,膜层之间良好的应力匹配使得多层高反射膜的沉积周期数可达到10以上.沉积1O个周期的多层反射膜,在中心波长1064nm处透射率约为1.6%-2.1%,接近全反射特征,其激光损伤阈值为16.4-18.2J/cm2(脉冲宽度为1ns).     

聚乙二醇对溶胶-凝胶SiO2增透膜激光损伤行为的影响

 采用溶胶-凝胶工艺制备了聚乙二醇（PEG）改性SiO₂单层增透膜，用输出波长1.06 μm，脉宽3 ns的调Q激光系统产生的强激光进行辐照实验。观察了添加PEG前后的膜层的微结构、表面形貌以及激光损伤行为的变化，讨论了PEG对薄膜激光损伤行为产生影响的机制。结果表明：添加的PEG可以修饰、导向溶胶簇团的生长和交联，并使之有序，由此制备的薄膜结构规整，微缺陷减少，这就提高了膜层的激光损伤阈值；在激光辐照过程中，膜料吸收激光能量，膜层温度升高，膜层的PEG分子受热逐步分解挥发，膜层产生损伤。     

溶胶-凝胶SiO2酸性膜与碱性膜的激光损伤行为

 采用溶胶-凝胶技术分别在K9基片上镀制了光学厚度相近的单层SiO₂酸性膜和碱性膜。测试了两类薄膜的激光损伤阈值；分别采用透射式光热透镜技术、椭偏仪、原子力显微镜、扫描电镜和光学显微镜研究了两类薄膜的热吸收、孔隙率、微观表面形貌、激光辐照前薄膜的杂质和缺陷状况以及激光辐照后薄膜的损伤形貌。实验结果表明：相对于碱性膜，酸性膜有更大的热吸收和更小的孔隙率，因此其激光损伤阈值较小；两类薄膜不同的损伤形貌与薄膜的热吸收系数与微观结构有关。     

溶胶-凝胶方法制备ZrO2及聚合物掺杂ZrO2单层光学增反射膜

以丙醇锆(Zr(OPr)4)为原料,乙酸(HAc)为络合剂,聚乙二醇(PEG200)和聚乙烯吡咯烷酮(PVP)为大分子添加剂,在乙醇体系中成功合成了ZrO2及聚合物掺杂ZrO2溶胶.用旋涂法在K9玻璃基片上制备单层光学增反射膜.借助小角X射线散射和激光动态光散射技术研究胶体的微结构.采用傅里叶变换红外光谱、差示扫描量热分析、X射线衍射分析、原子力显微镜、紫外/可见/近红外透射光谱以及椭偏仪对薄膜的结构和光学性能进行表征.用输出波长为1064 nm的强激光,采用"R/1"模式测试薄膜的抗激光损伤性能.研究发现,改变体系中HAc和H2O的量,可以方便地调节HAc配合反应和H2O分子亲核取代反应发生的概率,从而调控溶胶的稳定性与微结构.在HAc和H2O量配置适当的情况下,原位引入适量的PEG200和PVP可以明显修饰溶胶-凝胶过程,提高溶胶稳定性,促进胶粒之间相互联结成均匀的网络状结构.与溶胶的微结构密切相关,添加PEG200和PVP的薄膜具有更加平整的表面,而膜层均匀的结构及网络状特征赋予薄膜良好的抗激光损伤性能.添加质量分数为10% PEG200和15% PVP的聚合物掺杂ZrO2薄膜,激光损伤阈值可达24.5 J/cm2(脉冲宽度为1 ns);在中心波长λ0处,由反射引起的透射率降低约为2%,显示良好的增反射性能.     

氧分压对ZrO2薄膜激光损伤阈值的影响

 在不同的氧分压下用电子束热蒸发的方法制备了ZrO₂薄膜。分别通过X射线衍射、光学光谱、热透镜技术、抗激光辐照等测试，对所制备样品的微结构、折射率、吸收率及激光损伤阈值进行了测量。实验结果表明，薄膜中晶粒主要是四方相为主的多晶结构，并且随着氧分压的增加，结晶度、折射率以及弱吸收均逐渐降低。薄膜的激光损伤阈值开始随着氧分压增加从18.5J/cm²逐渐增加，氧分压为9×10^-3Pa时达到最大，值为26.7 J/cm²，氧分压再增加时则又降低到17.5 J/cm²。由此可见，氧分压引起的薄膜微结构变化是ZrO₂薄膜激光损伤阈值变化的主要原因。     

辐照激光能量对SiO2薄膜特性及结构的影响

 为了认识SiO2薄膜在激光辐照下的变化,本文以K9玻璃为基底,采用电子束热蒸发方法制备了SiO2薄膜,并将此组在相同实验条件下制备的薄膜加以不同能量的激光辐照,研究在激光辐照前后样片的透射率、折射率、消光系数、膜厚、表面形貌及激光损伤阈值（LIDT）的变化。结果表明,样片膜厚随激光能量的增加而减小,辐照激光能改善薄膜表面形貌,并使样片LIDT值提高,最终能使样片的LIDT值从16.96 J/cm2提高至18.8 J/cm2。     

Magnetic ordering in HoRu2Si2, HoRh2Si2, TbRh2Si2 and TbIr2Si2 by neutron diffraction

Neutron diffraction study of polycrystalline HoRu₂Si₂, HoRh₂Si₂, TbRh₂Si₂, and TbIr₂Si₂ was performed in the temperature range between 4.2 and 300 K. For HoRu₂Si₂ the magnetic spin alignment of a linear transverse wave mode below the Néel temperature 19 K is observed. This static moment wave is propagating along the b-axis with k=(0, 0.2, 0) and is polarized in the c-axis. The root-mean-square and maximum saturation moments per Ho atom are 9.26 and 13.09μ_B, respectively. HoRh₂Si₂, TbRh₂Si₂ an TbIr₂Si₂ are simple collinear antiferromagnets of +-+- type with Néel temperatures of (27±1), (98±2) and (72±3) K, respectively. For TbRh₂Si₂ and TbIr₂Si₂ magnetic moments are localized on RE ions only and are aligned along the tetragonal axis, while for HoRh₂Si₂ they form an angle ø = (28±3)°.     

μ+SR study of LaNi2As2, URh2Si2 and CeRh2Si2

Muon spin relaxation experiments have been carried out in the paramagnetic and magnetically ordered states of URh₂Si₂ and CeRh₂Si₂. As the magnetic structure of these compounds is well known, these measurements can help to characterise their magnetic properties probed by μSR and to understand the μSR results of the heavy fermion compounds of the same crystallographic family. Our measurements show that the muons occupy two different crystallographic sites. The spectra of URh₂Si₂ and CeRh₂Si₂ in the magnetically ordered states are very different, probably reflecting their different magnetic structures. The spectra obtained on CeRh₂Si₂ are similar to the published spectra of the heavy fermion compound CeCu_2.1 Si₂. Muon spin rotation measurements on LaNi₂As₂ indicate that the muon is diffusing at 150 K.     

13C-selective IRMPD of CBr2F2/Cl2 and CCl2F2/Br2 systems

The CO₂ TEA laser irradiation of CBr₂F₂ in the presence of Cl₂ yielded ¹³C-enriched CBrClF₂ and ¹³C-enriched CCl₂F₂ under selected experimental conditions. As the photolysis proceeded, the ¹³C concentration of CBrClF₂ decreased gradually and that of CCl₂F₂ increased up to 90% or higher. These results can be explained by the mechanism involving the secondary ¹³C-selective IRMPD of the primary product CBrClF₂. On the other hand, the carbon-containing product for a CCl₂F₂/Br₂ system was only CBrClF₂; the further IRMPD of which probably regenerated CBrClF₂ in the presence of Br₂. The decomposition probabilities of ¹²C- and ¹³C-containing molecules in both systems were measured as functions of laser line, laser fluence, and reactant pressures.     

Magnetostriction of SmMn2Ge2 and GdMn2Ge2 intermetallic compounds

Longitudinal and transverse magnetostrictions of polycrystalline samples of intermetallic compounds RMn₂Ge₂ (R=Sm or Gd) are measured in pulsed magnetic fields up to 250 kOe. It is found that linear magnetostrictive strains of about 10^?3 arise in a temperature range in which the magnetic field causes a change in the magnetic state of a manganese magnetic subsystem. The results obtained are described within the model of a two-sublattice ferrimagnet with a negative exchange interaction in the manganese subsystem in terms of a strong dependence of this interaction on interatomic distances.     

Polar optic phonons in Hg2Cl2 and Hg2Br2

Far infrared (30–430 cm^?1) reflectivity measurements of Hg₂Cl₂ and Hg₂Br₂ single crystals have been performed in polarized light. The spectra, which are in agreement with group-theoretical predictions, were analyzed by the oscillator fitting procedure and Kramers-Kronig method. The results are compared with the existing data from other measurements and the large anisotropy of polar modes is briefly discussed. The polarization vectors of all long-wavelength symmetry modes were determined group-theoretically.     

Superconductivity in LaPd_2Bi_2 with CaBe_2Ge_2-type structure

正Since the discovery of superconductivity in LaFeAsO_(1-x)F_x,the high-T_c iron-based superconductors have been extensively studied from both experimental and theoretical viewpoints [1-8]. However, the mechanism of the unconventional superconductivity is still to be resolved. To     

Structural,magnetic and neutron diffraction studies on TbFe2-TbAl2, TbCo2-TbAl2 and HoCo2-HoAl2

Both pseudobinary systems exhibit large homogeneous regions of cubic and hexagonal Laves phases. Ordering tendencies on crystallographic sites between Al and the transition metals are observed in the hexagonal type.Electron transfer to the transition metals quenches their moments so that they become nonmagnetic at high Al concentrations. The peculiarities in the mechanism of magnetization which appear in rare earth dialuminides when Al is replaced by a transition metal have been studied in detail at cryogenic temperatures.The first replacement of Al results in a decrease in saturation moment. Neutron diffraction verifies the low ordered rare earth sublattice moments and reveals the ‘lost part’ as a disordered component. Considerable magnetic hardness develops in certain regions of concentration often connected with spontaneous increases in magnetization with field. All available evidence suggests the presence of unusual domain wall effects to be responsible for this effect. High remanences develop in both the hexagonal and in the cubic structures in the intermediate region. The development of disordered magnetic components is connected either with the disorder on crystallographic sites or changes in the free electron concentration.