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1、华中科技大学 博士学位论文 微纳光学环腔生物传感芯片的制备研究 姓名：陈曜 申请学位级别：博士 专业：微电子学与固体电子学 指导教师：于军;周治平 20090531 I 华华 中中 科科 技技 大大 学学 博博 士士 学学 位位 论论 文文 摘摘 要要 微纳光学环腔生物传感芯片，以其特有的光学谐振增强效应使得生物传感具有 极高的灵敏度，可以实现对微量生物物质的无标记探测。此外，该传感芯片通常可 设计成平面波导结构，可采用成熟的半导体平面工艺加工，易于实现同其它光电芯 片和微流控芯片的系统集成，并且进行化学表面处理。因此，微纳光学环腔生物传 感芯片是一类极具应用前景的光学微量生物传感器件。本文在
2、国家自然科学基金的 资助下，对微环生物传感芯片的设计理论、芯片制备、和功能测试进行了系统深入 的研究，同时在完成纳米级光学环腔结构工艺加工的基础上，对微环传感片上集成 器件的制备工作进行了研究，制备了纳米光栅耦合器件、富硅二氧化硅微盘器件和 微环光子晶体器件。 阐述了微纳光学环腔生物传感芯片的研究状况和其光谐振效应对生物物质进行 传感的机理，并利用耦合模理论对传感芯片的模型进行设计分析，得到传感芯片中 各参数的作用，其中，微环芯片的品质因数 Q 是决定探测灵敏度的一个重要因素。 对微纳光学环腔芯片的制备工艺进行了深入的研究，实现了氮化硅和硅波导两种材 料体系的微环芯片的制备工作。其中，利用热氧
3、化、低压化学气相沉积（LPCVD） 、 光学光刻、 电感耦合增强反应离子刻蚀 （ICP） 、 等离子体增强化学气相沉积 （PECVD） 等工艺，制备了最小线宽为 1 m，波导侧壁粗糙度小于 30 nm 的氮化硅/二氧化硅材 料结构的光学环腔传感芯片；利用电子束光刻（EBL） ，ICP 等工艺，制备了 silicon-on-insulator （SOI）材料体系的微纳光学环腔结构，最小结构尺寸为 160 nm， 波导侧壁粗糙度小于 10 nm。 在完成了微纳光学环腔生物传感芯片的制备工作后，利 用高精度精密调节架、宽谱光源、光谱仪等设备对微环芯片的光学特性进行了测试， 测得所制备的光学环腔芯片品
4、质因数 Q 高达 25000。 设计出相应的夹具对所制备的光学环腔芯片进行封装，使其成为密封的化学生 物传感芯片。并利用光学环腔传感芯片对不同折射率的溶液进行了探测。在测量中， 得到葡萄糖溶液的浓度响应曲线，探测灵敏度高达 10-4 RIU（折射率单元） 。采用表 II 华华 中中 科科 技技 大大 学学 博博 士士 学学 位位 论论 文文 面探测的机理，利用经过炭疽杆菌单链 DNA 探针绑定的光学环腔芯片，通过 DNA 杂交的原理， 实现该芯片对炭疽杆菌单链 DNA 浓度的测量， 得出炭疽杆菌单链 DNA 浓度的响应曲线，探测灵敏度达到纳摩尔每升。 对三种微环传感片上集成器件：纳米光栅耦合器
5、件、富硅二氧化硅微盘器件和 微环光子晶体器件的制备工艺进行了研究。其中，利用 EBL，ICP 等工艺，制备了 二元闪耀光栅耦合器件，其最小尺寸为 40 nm，波导侧壁粗糙度小于 10 nm；利用 PECVD、高温退火、电子束光刻、ICP 刻蚀和 RIE 刻蚀等工艺，实现了最小直径为 4 m 的富硅二氧化硅微盘器件的制备；利用原子层淀积（ALD） 、EBL、ICP 等工 艺，制备了具有纳米级自对准的微环光子晶体结构，实现精度为原子量级的自对准 工艺。 关键词：关键词：生物传感器 炭疽杆菌单链 DNA 微纳制造 光学谐振腔 探测灵敏度 III 华华 中中 科科 技技 大大 学学 博博 士士 学学
6、位位 论论 文文 Abstract Microring resonator biosensor shows promising because of its robustness, lable-free detection mechanism, mature CMOS fabrication technology, low cost and high sensitivity achieved by the long lifetime of photons that circle in the ring, which increases the probability of photons in
7、teracting with analytes. Based on planar waveguides, it not only allows surface chemical modifications, but can also be integrated with other optoelectronic devices and microfluidic handling, leading to highly integrated and intelligent sensing systmes. Furthermore, it offers a unique advantage of r
8、educing the device size without sacrificing the sensitivity by virtue of the resonance. Therefore, micoring resonator biosensor is highly sensitive that can detect minute amount of analytes. Supported by the National Science Foundation of China, the fabrication and sensing application of the microri
9、ng resonator are systematically studied in this thesis. The sensing mechanism of the microring resonator biosensor was intrudoced and the optical parameters were analyzed of which the Q factor determines the sensitivity. Fabrication of the microring resonator biosensors based on silicon nitride and
10、silicon waveguide systems was realized. By using thermal oxidation, Low pressure chemical vapor deposition (LPCVD), optical lithography, inductively coupled plasma etcher (ICP) and plasma enhanced chemical vapor deposition (PECVD) processes, the silicon nitride microring resonators with smallest fea
11、ture size of 1 m and waveguide sidewall roughness of less than 30 nm were fabricated and by using e-beam lithography (EBL) and ICP processes, the silicon microring resonators with smallest feature size of 160 nm and waveguide sidewall roughness of less than 10 nm were fabricated. Optical characteriz
12、ation of the as fabricated microring resonators based on transmission mechanism was done by using tunable light rource, optical transmission alignment system and optical spectrometer and Q factors of the devices as high as 25000 were measured. The microring resonators were later packaged to serve as
13、 a sealed chemical sensing system. Glucose solutions with various concentrations were detected by the system which results in a linear corresponding curve between the resonance wavelength shifts and the concentrations with a sensitivity of 10-4 RIU. Bacillus Anthracis ssDNA solutions with IV 华华 中中 科
14、科 技技 大大 学学 博博 士士 学学 位位 论论 文文 various concentrations by surface sensing mechanism with the microring resonators were detected and linear corresponding curves with sensitivity of n-mole per liter were achieved. Fabrication of nanoscale optical grating coupler, silicon rich silicon oxide microdisk and
15、annular photonic crystals (APC), which are supposed to be integrated with the microring biosensor as optical coupler, light source and polarization controller on chip, was discussed. Nanoscale optical grating coupler with smallest features of 40 nm in a dense fashion and waveguide sidewall roughness
16、 of less than 10 nm was realized. The fabrication process of silicon rich silicon oxide microdisk devices by using PECVD, high temperature annealing, e-beam lithography, ICP etching and RIE etching processes was studied and the microdisks with smallest diameter of 4 m were realized. Annular photonic crystals was fabricated by using atomic layer depositon (ALD), EBL, ICP, reactive ion etcher (RIE) and wet etching and a self-alignment technique was developed to achieve a precise nanoscal
