溶胶-凝胶SiO2减反膜的制备与光学性能研究

碱催化溶胶-凝胶多孔SiO₂减反膜具有优异的光学性能及抗激光损伤性能,是高功率激光装置中的重要组成部分,但其与光学元件之间的结合强度低,使得膜层易发生接触破坏。本研究以“神光II”高功率激光装置溶胶-凝胶多孔SiO₂减反膜为基础,通过提拉法在其表层涂覆致密的SiO₂薄层后得到机械强度提升的双层SiO₂减反膜(SiO₂-MTES),并与常用的单层氨固化SiO₂减反膜(SiO₂-HMDS)进行相关应用性能的综合比较。结果表明,涂覆SiO₂-MTES的熔石英在约800 nm处的峰值透过率大于99.6%,运用1-on-1激光损伤阈值测试方法测得该双层SiO₂减反膜的零几率激光损伤阈值为51.9 J/cm²(1064 nm, 9.1 ns),与涂覆SiO₂-HMDS的性能相当。同时, SiO₂-MTES膜层与水的接触角达到117.3°,...     

疏水耐环境型SiO2/TiO2/SiO2-TiO2太阳能宽光谱增透膜的制备及性能研究

利用TFCcal设计软件构建膜系结构, 采用溶胶-凝胶工艺和提拉法在超白玻璃上制备出厚度精确可控的宽光谱、高增透型SiO₂/TiO₂/SiO₂-TiO₂减反膜, 同时结合甲基三乙氧基硅烷(MTES)改性碱催化的SiO₂溶胶, 通过提拉法一次制备出高透过率疏水型薄膜。研究表明, 高增透型三层宽光谱减反膜的理论膜层厚度依次为: 80.9 nm(内层SiO₂-TiO₂)、125.0 nm(中间层TiO₂)、95.5 nm(外层SiO₂), 其在400~700 nm可见光范围内平均透过率实际可高达97.03%以上。多层膜经过退火处理后, 膜面的水接触角高达131.5°, 同时陈化两个月以后的多层膜透过率仅下降0.143%, 表明制备的SiO₂/TiO₂/ SiO₂-TiO₂多层减反膜具有优良的疏水和耐环境性能。     

ZrO2-SiO2薄膜对离子交换增强玻璃的光学和力学性能影响

采用溶胶-凝胶法在玻璃表面制备出ZrO₂-SiO₂薄膜, 然后通过离子交换形成镀膜增强玻璃, 研究了薄膜组成对离子交换增强玻璃的力学和光学性能的影响。利用紫外可见分光光度计、激光椭偏仪、纳米压痕、三点抗弯和能谱(EDX)分析了薄膜结构及性能。结果表明: 所有薄膜均连续均匀, 纯ZrO₂薄膜为四方相结构, 含Si薄膜为无定形结构; 薄膜具有较高弹性恢复率(>60%)以及H/E比(>0.1), 有利于强度增强; 随Si含量增加, 可见光透过率增大, 但表面硬度和杨氏模量随之降低; 0.5ZrO₂-0.5SiO₂薄膜综合性能最佳: 表面硬度为18 GPa, 抗弯强度为393 MPa, 厚度~45 nm时可见光透过率大于85%。     

辛基三甲氧基硅烷改性SiO2疏水减反膜的制备

以正硅酸乙酯为前驱体, 氨水为催化剂制备标准SiO₂溶胶, 然后在回流前后分别对普通SiO₂溶胶添加适量的辛基三甲氧基硅烷(OTMS)进行修饰, 得到OTMS改性SiO₂溶胶。用未进行OTMS修饰、回流前修饰和回流后修饰的溶胶分别制备减反膜, 并使用傅里叶变换红外光谱仪、核磁共振波谱仪、紫外-可见-近红外分光光度计、原子力显微镜和接触角测试仪对薄膜的结构和性能进行表征。结果表明: 回流前添加OTMS修饰剂制备的改性SiO₂减反膜具有最优异的耐潮湿环境稳定性能, 最高透过率可达99.7%以上; 与水的接触角达到120°, 在潮湿环境中放置4 w后, 透过率只下降0.23%。     

自清洁SiO2/TiO2减反膜的制备与性能研究

采用溶胶-凝胶技术制备了SiO₂溶胶和TiO₂溶胶，利用浸渍提拉法在光伏玻璃上制备了SiO₂/TiO₂减反膜。用光谱透射比测量仪和椭偏仪测定了薄膜的透光率和折射率，通过场发射扫描电子显微镜观察了薄膜的形貌结构，最后考察了薄膜的自洁性能和耐候性能。结果表明：随着溶胶中TiO₂浓度的升高，SiO₂/TiO₂减反膜的厚度不断增加，而透光率逐渐减小，折射率逐渐增大。在波长为600nm时，TiO₂浓度最低的减反膜(ST-300)的透光率为94.4%,折射率为1.33。ST-300减反膜的表面平整，结构致密。光催化2h后，ST-300减反膜可将10mg/L的甲基蓝溶液降解11.2%,经过耐候处理后，其透光率衰减值仅0.08%～0.15%。     

含Si-O-P键的减反膜结构及性能影响因素研究

采用SiO₂水溶胶(ACS)为硅源, H₃PO₄为桥联剂, H₂O₂为活化剂在玻璃表面成功制备了一种性能优异的新型减反膜。利用FTIR、XRD、FESEM、TEM、AFM对薄膜结构、形成机理及性能进行了研究, 结果表明, 在成胶过程中, H₂O₂的导入有效修复了SiO₂胶粒的表面羟基, 提高了SiO₂的反应活性; 而在焙烧过程中, H₃PO₄通过其自身脱水形成的偏磷酸链状体分别与SiO₂胶粒及玻璃基底表面的Si-OH进行了脱羟基缩聚, 构架了坚固的Si-O-P网络交联, 最终形成了稳定的磷硅酸盐凝胶网络结构, 提高了成膜质量。当n(H₃PO₄) : n(H₂O₂) : n(EtOH) : n(SiO₂)= 0.49: 0.52: 30: 1时, 制备的SiO₂减反膜在可见光区平均透光率高达98%, 硬度可达6H。     

磁控溅射镍膜催化生长石墨烯及迁移表征

在Si/SiO2衬底上将磁控溅射镍膜作为催化剂,利用化学气相沉积制备了大面积连续的石墨烯薄膜,得到的石墨烯为1～15层.将石墨烯薄膜迁移到玻璃衬底和Si/SiO2衬底上,测量了薄膜的可见光透过率和薄膜电阻,并讨论了石墨烯作为透明导电电极在光电器件上的应用.     

钴掺杂TiO2纳米管阵列薄膜的制备及其光催化还原性能

用磁控溅射法在ITO玻璃基底上制备Ti-Co合金薄膜,对其阳极氧化处理制备出钴掺杂TiO₂纳米管阵列薄膜,研究了钴掺杂对纳米管阵列薄膜的形貌、结构、吸收光谱以及光催化还原性能的影响。结果表明：钴掺杂TiO₂纳米管阵列薄膜为锐钛矿相,管状阵列的管径均一、排列规整。钴掺杂使薄膜形成(001)择优取向。随着钴掺杂量的提高,薄膜吸收可见光的能力提高。钴含量(原子分数)为0.19%的薄膜光催化性能最优,可见光照150 min后对Cr(VI)的还原率可达98.4%。     

基于SnO2∶Sb薄膜沉积工艺参数优化的支持向量回归分析

开发低成本高质量透明导电氧化物薄膜材料的生长技术对现代光电产业发展十分重要。面对多维的薄膜生长工艺参数空间，在寻求最优薄膜生长参数过程中如何有效降低时间、材料成本是研究人员迫切关注的问题。基于雾化辅助CVD法在石英衬底上制备SnO₂∶Sb薄膜，利用实验设计方法，获得不同工艺参数下制备的SnO₂∶Sb薄膜实验数据集。应用基于贝叶斯优化的支持向量回归方法，建立SnO₂∶Sb薄膜透明导电性能的支持向量回归预测模型，结合预测模型对整个工艺参数空间进行探索。利用有限27组工艺参数组合可在四维参数空间中找到高质量SnO₂∶Sb薄膜的有效制备参数。在最优工艺参数下制备薄膜的可见光透过率可达86.61%,方块电阻为21.1Ω·□^-1,膜厚约380 nm。为基于雾化辅助CVD法制备薄膜材料的最优制备工艺探索提供一条有效途径，可有效节约开发成本。     

五层纳米SiO2-Al2O3/聚酰亚胺复合薄膜的制备及性能

采用浸胶法制备了一系列SiO₂-Al₂O₃/聚酰亚胺（SiO₂-Al₂O₃/PI）五层耐电晕薄膜A_m A_n PA_n A_m,其中中间层（P）为纯PI薄膜,外层（A_m）、次外层（A_n）分别为SiO₂-Al₂O₃掺杂不同质量分数的纳米SiO₂-Al₂O₃/PI薄膜。采用TEM、FTIR、宽频介电谱仪、电导电流测试仪、耐电晕测试仪、介电强度测试仪和拉伸实验机对五层纳米复合PI耐电晕薄膜的微观结构、介电性能和力学性能进行了表征和测试。结果表明,SiO₂-Al₂O₃/PI复合薄膜掺杂层形成了分布均匀的有机/无机复合结构;SiO₂-Al₂O₃纳米粒子的保护作用是影响复合材料耐电晕性能的主要因素,复合薄膜A₃₂A₁₆PA₁₆A₃₂的耐电晕寿命最大,为23.4 h;外层掺杂量对五层SiO₂-Al₂O₃/PI复合材料的介电强度影响较大,复合薄膜A₂₀A₂₈PA₂₈A₂₀的介电强度最大,为302.3 kV/mm;通过对五层复合结构的设计,可以在兼顾材料力学性能的同时,提高其耐电晕寿命和介电强度。     

沉积时间对聚醚醚酮表面类金刚石薄膜的结构和性能的影响

采用直流磁控溅射技术在聚醚醚酮(PEEK)表面制备不同厚度的类金刚石(DLC)薄膜,研究了沉积时间对其表/界面结构、组分、疏水、力学和光透过性能的影响。结果表明,在平均沉积速率为5.71 nm/min的条件下,随着沉积时间的延长DLC薄膜的厚度线性增大、碳原子的致密性提高、界面互锁结构增强,而界面结合强度逐渐降低。沉积时间≤15 min时,基体结构的影响使拟合计算出的I_D/I_G值为0.23~0.25和sp²/sp³比值较小(0.58~0.74);沉积时间>15 min时基体的影响较小,I_D/I_G值突增大至0.81,sp²/sp³值也比较大(0.96~1.12)。沉积时间的延长使PEEK基体的温度逐渐升高,使膜内的sp²/sp³值逐渐增大。薄膜表面的氧含量先降低然后趋于平缓,部分C=O转化为C-O。随着沉积时间的延长,PEEK/DLC复合薄膜的硬度、弹性模量及防紫外线和阻隔红外线性能都逐渐提高,其表面粗糙度和疏水性的变化趋势是先提高后降低。沉积时间为32 min的薄膜,其表面粗糙度和水接触角达到最大值,分别为495 nm和108.29°。     

MBE growth and characterization of buried silicon oxide films on Si(100)

Silicon molecular beam epitaxy (Si-MBE) has been used to produce silicon oxide (SiO_x) films by evaporating Si on a heated Si(100) substrate in an ultra high vacuum system with an O₂ pressure of 10⁻⁶ to 10⁻⁴ mbar. Then the SiO_x films were overgrown with pure Si. The influence of the substrate temperature, the O₂ pressure and the Si deposition rate on the oxygen content in the SiO_x films and on the crystalline quality of the Si top-layer was investigated by Rutherford backscattering spectrometry and ion channeling. Epitaxial growth of the Si top-layer was observed up to a maximum concentration of ≈20 at.% oxygen content in the SiO_x film. Cross-sectional transmission electron microscopy shows that the structure of the SiO_x film changes duringa subsequent annealing procedure. Electron energy loss spectrometry proves that amorphous SiO₂ is formed and the development of holes indicates that the density of the as-grown SiO_x film is much lower than that of SiO₂. The specific for the as-grown SiO_x films was determined by I–V measurements.     

Measurement of the current transient in Ta2O5 films

Current vs. time (I−t) measurements were performed on Ta₂O₅-based devices. Charge build-up at the Ta₂O₅/SiO₂ interface was used to explain the transient. The interfacial charge density was calculated from the I−t curve and the maximum was found to be 398 nC cm^-2 and 317 nC cm^-2 for Al/Ta₂O₅/Si and Al/Ta₂O₅/SiO₂/Si capacitors respectively. The value for MTOS was comparable with the value obtained by quasi-static measurements.     

Effect of N2O/SiH4 ratio on the properties of low-temperature silicon oxide films from remote plasma chemical vapour deposition

Silicon oxide films have been deposited with remote plasma chemical vapour deposition (RPCVD) at low temperatures (<300 °C) from SiH₄---N₂O. The effect of a gas-phase reaction on the SiO₂ film properties and Si/SiO₂ interface was investigated. As the partial pressure ratio was increased above N₂O/SiH₄ = 4, a gas-phase reaction with powder formation was observed, which degraded film properties, increased surface roughness, and decreased deposition rate. When N₂O/SiH₄ <4, there was no detectable IR absorption in the film associated with hydrogen-related bonds (Si---OH and Si---H) but when N₂O/SiH₄ >4, the incorporation of Si---OH bond became significant and Si¹⁺, intermediate state silicon at the interface, was more abundant. The oxide fixed charge, interface trap density, surface roughness and leakage current were increased when there was powder formation in the gas phase. High plasma power also favoured the powder formation in the gas phase. C---V and I---V characteristics were measured and it was shown that these electrical properties were directly related to the process condition and material properties of the oxide and the Si/SiO₂ interface.     

雾化溅射干燥法制备氧化石墨烯-SiO2/天然橡胶复合材料

将天然胶乳（NRL）、氧化石墨烯（GO）分散液与SiO₂悬浮液3种液体通过机械搅拌充分混合,在高压气相雾化作用下,混合液先被打散成微小液滴,形成一次破碎;该液滴后经高温金属板表面溅射爆破,形成二次破碎,达到分散效果,然后液滴被瞬间脱水干燥获得GO-SiO₂/天然橡胶（NR）母胶。GO与SiO₂在雾化、溅射和爆破作用下,在NR中达到微观分散效果。结果表明,与普通絮凝湿法混炼工艺相比,雾化溅射干燥工艺可以使GO和SiO₂在NR基体中分散更均匀。Payne效应结果表明：雾化溅射工艺减弱了GO片层与SiO₂间的相互作用。雾化溅射干燥工艺制备的GO-SiO₂/NR硫化胶的拉伸强度提高了13.6%,撕裂强度提高了31.5%,耐磨性能提高了16.7%;动态力学性能结果表明,用该工艺制备的GO-SiO₂/NR复合材料在60℃左右损耗因子更低。     

CVD of hard DLC films in a radio frequency inductively coupled plasma source

Chemical vapor deposition (CVD) of hard diamond-like carbon (DLC) films on silicon (100) substrates from methane was successfully carried out using a radio frequency (r.f.) inductively coupled plasma source (ICPS). Different deposition parameters such as bias voltage, r.f. power, gas flow and pressure were involved. The structures of the films were characterized by Fourier transform infrared (FTIR) spectroscopy and Raman spectroscopy. The hardness of the DLC films was measured by a Knoop microhardness tester. The surface morphology of the films was characterized by atomic force microscope (AFM) and the surface roughness (R_a) was derived from the AFM data. The films are smooth with roughness less than 1.007 nm. Raman spectra shows that the films have typical diamond-like characteristics with a D line peak at 1331 cm⁻¹ and a G line peak at 1544 cm⁻¹, and the low intensity ratio of I_D/I_G indicate that the DLC films have a high ratio of sp³ to sp² bonding, which is also in accordance with the results of FTIR spectra. The films hardness can reach approximately 42 GPa at a comparatively low substrate bias voltage, which is much greater than that of DLC films deposited in a conventional r.f. capacitively coupled parallel-plate system. It is suggested that the high plasma density and the suitable deposition environment (such as the amount and ratio of hydrocarbon radicals to atomic or ionic hydrogen) obtained in the ICPS are important for depositing hard and high quality DLC films.     

Corrosion of tin in citric acid solution and the effect of some inorganic anions

The corrosion behaviour of tin in different concentrations of citric acid solutions (0.3–1.0 M, pH=1.8) was studied at 30 °C by potentiodynamic technique. The E/I profiles exhibit an active passive behaviour. The active dissolution involves one anodic peak A associated with a dissolution of the metals as Sn(II) species. The passivity is due to the formation of thin film of SnO₂ and or Sn(OH)₄ on the anode surface. The cathodic sweep shows a small peak C related to the reduction of the passive film. The peak current density I_p of peak A increases with increasing both acid concentration and sweep rate.

The effects of adding increasing concentrations of Na₂CrO₄, NaMoO₄, NaNO₃ and NaNO₂ on the corrosion of tin in 0.5 M citric acid at 30 °C were investigated. Both CrO₄²⁻ and MoO₄²⁻ ions inhibit the corrosion of tin and the extent of inhibition enhances with their concentrations. Addition of either NO₃⁻ or NO₂⁻ accelerates the corrosion of tin. NO₃⁻ ions are more aggressive than NO₂⁻ ions.