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Femtosecond laser two-photon polymerization three-dimensional micro-nanofabrication technology
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摘要:
飞秒激光双光子聚合微纳加工技术作为重要的三维微纳结构制备手段，已成为国际前沿研究热点。该技术利用激光与物质相互作用的双光子非线性吸收效应和阈值效应，可以突破经典光学理论衍射极限，实现纳米尺度的激光加工分辨力，在三维功能性微纳器件制备领域正在发挥着十分重要的作用。本文在介绍飞秒激光双光子聚合三维微纳加工技术的光物理和光化学过程基本原理的基础上，重点回顾人们在改善加工线宽及分辨力、提高加工效率等方面的研究进展与发展概况。该技术所制备的各种微光学器件、集成光学器件、微机电系统以及生物医学器件，不仅充分展示了飞秒激光双光子聚合三维微纳加工技术的高空间分辨力和真三维加工特点，也为其在相关前沿领域的应用提供具有启发性的思路。最后，对该技术实现高精度、高效率、低成本、大面积、多功能的三维微纳结构加工所存在的挑战和未来发展方向，进行了讨论和展望。
Abstract:Femtosecond laser two-photon polymerization (TPP) micro-nano fabrication technology, as an important method for the preparation of three-dimensional (3D) micro-nanostructures, has become a hot spot of international frontier research. Using the two-photon absorption effect and the threshold effect of the interaction between laser and matter, this technology can break through the diffraction limit of classical optical theory and achieve nanoscale laser fabrication resolution. It is expected to play an important role in the field of 3D functional micro-nano device fabrication. In this paper, the basic principles of photophysical and photochemical processes in femtosecond pulsed laser TPP fabrication technology will be described, and the research progress and development of this technology in improving line width and fabrication resolution, and improving fabrication efficiency will be reviewed. Then, using the high spatial resolution and true 3D fabrication characteristics of femtosecond laser TPP micro-nano fabrication technology, the researchers prepared various micro-optical devices, integrated optical devices, micro-electromechanical systems, and biomedical devices, fully demonstrating the application prospect of this technology. Finally, how to achieve high-precision, high-efficiency, low-cost, large-area, multi-functional materials and microstructure fabrication, as well as existing challenges and future development directions are discussed and prospected.
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Key words:
- femtosecond laser /
- two-photon polymerization /
- optical diffraction limit /
- resolution /
- efficiency
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Overview: Femtosecond laser two-photon polymerization (TPP) micro-nanofabrication technology is a new type of three-dimensional lithography technology that integrates nonlinear optics, ultra-fast pulsed laser, microscopic imaging, ultra-high-precision positioning, three-dimensional (3D) graphics CAD modeling, and photochemical materials. It has the characteristics of simplicity, low cost, high resolution, true 3D, and so on. Different from the technical route of shortening the wavelength of the traditional lithography, this TPP technology breaks through the optical diffraction limit using the ultrafast laser in the near-infrared and the nonlinear optical effect of the interaction between the laser and the material. TPP can achieve true 3D fabrication of complex 3D structures. After the femtosecond pulse laser is tightly focused in space, photopolymerization is initiated by the two-photon absorption(TPA), which can limit the fabrication area in the center of the focus. The interaction time of the ultrashort pulse with the material is much lower than the thermal relaxation of the material, avoiding the photothermal effect. The lateral linewidth can be reduced to about 100 nm due to the strong threshold characteristics of the two-photon absorption process. Thus, TPP is an ideal fabrication method in the field of 3D micro-nanostructure. Since 2001, Kawata’s team has used a near-infrared femtosecond laser with a wavelength of 780 nm to fabricate a "nanobull" with the size of red blood cells. It fully demonstrated the advantages of TPP in the preparation of three-dimensional micro-nano structures. At the same time, a polymer nanodot with a size of 120 nm was fabricated, which was only 1/7 of the laser wavelength, breaking the optical diffraction limit in this study. Since then, scientists from various countries have improved the line width, resolution, and other parameters of 3D structure by continuously improving the materials, structure, processing technology and light field control, and other aspects. At the same time, with the continuous development and improvement of the 3D nanostructure fabrication technology, the advantages of TPP technology are also reflected in some application fields, such as micro-optical devices, integrated optical devices, micro-electromechanical systems, and biomedical devices. This paper will systematically introduce the femtosecond laser TPP micro-nanofabrication technology, including the fabricating principle, the development of fabricating methods, and its research overview in many application fields. Finally, its existing problems and future development and application prospects are discussed.
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图 2 光聚合交联过程及单体转化度。(a) 光刻胶中单体分子聚合和交联过程示意图[64]; (b) 在商业(丙烯酸酯基)光刻胶 IP-L 780 中不同扫描速度下拉曼光谱计算的单体转化度[67]
Figure 2. Cross-linking process and degree of conversion. (a) Schematic diagram of the polymerization and cross-linking process of monomer molecules[64]; (b) Degree of conversion calculated from the Raman spectra for TPP with different scanning velocities in the commercial (acrylate-based) photoresist IP-L 780[67]
图 3 光聚合阈值和破坏阈值分布图。(a) 激光曝光阈值强度随着曝光时间变化关系[71]；(b) 暗场显微镜测量的不同扫描速度下聚合阈值和破坏阈值激光强度[47]；(c) 暗场和原位显微镜测量单次和多次曝光下阈值激光强度[47]
Figure 3. Distribution of the photopolymerization threshold and the damage threshold. (a) Laser exposure threshold intensity as a function of exposure time[71]; (b) Laser power threshold at different scan speeds measured by darkfield microscopy[47]; (c) Threshold laser intensities at single and multiple exposures measured by darkfield and in situ microscopy[47]
图 4 双光子聚合加工超衍射特征尺寸结构，以及加工聚合体元(Voxel)形貌模型。(a) 双光子聚合加工示意图[15]；(b) 制备的“纳米牛”[19]；(c) 线宽与曝光时间的非线性关系[19]；(d) 双光子聚合加工焦点处光强度分布，其中虚线为光强度的平方[47]；(e) 体元长度与曝光功率关系[78]；(f) 体元线宽与曝光功率关系[78]
Figure 4. Sub-diffractive feature-scale structures by TPP and topography models of Voxel. (a) Schematic diagram of the TPP[15]; (b) The prepared "nano bull"[19]; (c) The nonlinear relationship between line width and exposure time[19]; (d) Light intensity distribution of the focus, where the dotted line is the square of light intensity[47]; (e) The relationship between voxel length and exposure power[78]; (f) The relationship between voxel linewidth and exposure power[78]
图 5 双光子聚合加工系统示意图。(a) 典型的基于压电位移台扫描的双光子加工系统光路图[49]；(b) 不同加工衬底对应不同的扫描策略示意图[17]；(c) 振镜扫描、(d) 浸入式扫描、(e) 基于STED技术和 (f) 基于SLM的双光子加工系统示意图[17]
Figure 5. Schematic diagram of the TPP system. (a) Optical path diagram of a typical TPP based on the piezoelectric stage scanning[49]; (b) Schematic diagram of different scanning strategies on different substrates[17]; (c) Galvanometer scanning, (d) immersion scanning, (e) STED assised and (f) SLM based TPP system[17]
图 6 双光子聚合加工极限尺度纳米点、线结构。(a) 120 nm[19]、(b) 100 nm[98]、(c) 80 nm[100]、(d) 90 nm[101]、(e) 50 nm[103]、(f) 35 nm[74]、(g) 30 nm[104]、(h) 23 nm[105]、(i) 7 nm、8 nm和9 nm[106]特征尺度纳米点、线结构
Figure 6. The nanodots/wires structures fabricated by TPP.(a) 120 nm[19], (b) 100 nm[98], (c) 80 nm[100], (d) 90 nm[101], (e) 50 nm[103], (f) 35 nm[74], (g) 30 nm[104], (h) 23 nm[105], (i) 7 nm, 8 nm and 9 nm[106] feature size in the nanodots/wires structures
图 7 基于STED双光子聚合加工极限尺度纳米线结构。(a) 基于STED双光子加工示意图及制备的结构最小纵向尺寸40 nm[110]；(b) 纳米线线宽与532 nm 连续激光抑制光束功率的关系图及制备的95 nm、65 nm、90 nm和145 nm宽度的纳米线[111]；(c) 聚合光束和抑制光束截面强度分布图，及制备的54 nm宽度纳米线[112]；(d) 通过增加抑制光强提高分辨力的原理图及加工的9 nm特征尺度纳米线结构[113]
Figure 7. The nanowires structures fabricated by STED-TPP. (a) Schematic diagram of the STED-TPP and the minimum longitudinal size of 40 nm[110]; (b) The relationship between the line width and the 532 nm CW laser and the fabricated nanowires with widths of 95 nm, 65 nm, 90 nm, and 145 nm[111]; (c) Cross-sectional intensity distributions of the initiation and inhibition laser beam, and the fabricated nanowires with width of 54 nm[112]; (d) Schematic diagram of improving resolution by increasing inhibition intensity and the fabricated nanowires with the minimum size of 9 nm[113]
图 8 基于多光束并行加工制备的周期性三维结构。(a,b) 基于衍射元件直写加工的微齿轮和微米牛组合结构[120]；(c) 基于DMD投影拼接的二维阵列结构[121]；(d) 基于SLM直写加工的抛物面镜结构[122]；(e-g) 基于衍射元件直写加工三维力学超材料[123]
Figure 8. Periodic 3D structures fabricated based on multi-beam parallel fabrication technology.(a,b) Micro-gear and micro-bull combined structures fabricated by TPP with diffractive elements[120]; (c) 2D array structure fabricated by TPP with DMD projection[121]; (d) Parabolic mirror structure based on SLM-TPP[122]; (e-g) 3D mechanical metamaterials fabricated by TPP with diffractive elements[123]
图 9 基于DMD双光子加工制备的高精度、大尺寸结构。(a) DMD全息多焦点3D双光子打印方法，及打印的高分辨“桥”结构，二元全息产生单焦点、双焦点、三焦点制备的木堆结构[125]；(b) 基于DMD飞秒投影双光子光刻技术及制备的具有亚微米特征尺度的厘米级三维结构，微纳悬臂结构[126]；(c) 基于时空聚焦DMD投影双光子光刻技术及制备的微纳悬线结构，宏观超材料结构[127]；(d) 基于DMD飞秒面投影纳米光刻技术及制备的纳米线、点结构，跨尺度微纳结构[128]
Figure 9. High-precision, large-scale structures fabricated by DMD TPP technology.(a) DMD holographic multi-focus 3D TPP method and the fabricated high-resolution "bridge" structure, and woodpile structures[125]; (b) The prepared Millimeter-scale structure with sub-micrometer features, micro-nano bridge structures by FP-TPL technology[126]; (c) The prepared micro-nano suspended lines and micro-metamaterial structures by projection TPP with the spatiotemporal focusing technology[127]; (d) The prepared nanowires and nanodots structures, cross-scale structures by femtosecond projection nanolithography technology[128]
图 10 光子晶体、超材料与器件。(a) 木堆结构光子晶体[131]；(b) 金刚石结构光子晶体[133]；(c) 热收缩的木堆光子晶体[134]；(d) 手性螺旋超材料[135]；(e) 光波段的三维隐身衣结构[136]；(f) 光束偏转器[137]；(g) 复合手性光子晶体材料[138]；(h) 圆偏振光分光器[139]
Figure 10. Photonic crystals, metamaterials, and devices. (a) Woodpile photonic crystal[131]; (b) Diamond photonic crystal[133]; (c) Heat shrinkable woodpile photonic crystal[134]; (d) Chiral helical metamaterial[135]; (e) 3D invisibility cloak structure in optical band[136]; (f) Beam deflector[137]; (g) Composite chiral photonic crystal material[138]; (h) Circularly polarized beam splitter[139]
图 11 超表面透镜器件。(a) 混合消色差超透镜宽带聚焦示意图[141]；(b) 混合消色差超透镜的结构图[141]；(c) 局部放大图[141]；(d) 宽带近红外光成像效果[141]；(e) 基于纳米孔相位板的宽带超透镜[142]；(f) 测量的宽带聚焦光斑[142]；(g) 可调焦距的 3D 双级联超透镜[146]；(h) 测量的变焦距聚焦光斑[146]
Figure 11. Metalens device. (a) Schematic diagram of the broadband focusing of the hybrid achromatic metalens[141]; (b) The structure of the hybrid achromatic metalens[141]; (c) The partial enlarged view[141]; (d) The imaging of the broadband near-infrared light[141]; (e) The broadband metalens, which combines nanoholes with a phase plate[142]; (f) Measured broadband focusing spot[142]; (g) The tunable multifocal 3D metalens[146]; (h) Measured zoom focusing spot[146]
图 12 集成光子学器件。(a) 微型棱镜耦合器[148]；(b) 低损耗光纤-片上耦合器[149]；(c) 偏振旋转的聚合物矩形波导[150]；(d) 光纤-片上连接器[153]；(e) 芯片-芯片光连接器[153]；(f) 片上器件-器件光连接器[153]；(g) 微盘腔结构和光互联波导结构[154]；(h) 三维弯曲表面光子微腔结构[155]
Figure 12. Integrated photonics device. (a) Miniature prism coupler[148]; (b) Low-loss fiber-on-chip coupler[149]; (c) Polarization-rotated polymer rectangular waveguide[150]; (d) Fiber-on-chip connector[153]; (e) Chip-on-chip optical connector[153]; (f) On-chip device-device optical connector[153]; (g) Microdisk cavity structure and optical interconnect waveguide structure[154]; (h) 3D curved surface photonic microcavity structure[155]
图 14 逆向设计微纳光学器件。(a) 自由形式近红外偏振分束器[163]；(b) 光谱分离超表面透镜[164]；(c) 3D圆对称超透镜[165]；(d) 多层超透镜[166]
Figure 14. Inverse-designed micro-nano optics devices. (a) Free-form NIR polarizing beamsplitter[163]; (b) Spectral splitting metalens[164]; (c) 3D circularly symmetric metalens[165]; (d) Multilayer metalens[166]
图 15 力学超材料结构与器件。(a) 剪切模量消隐的五模式反膨胀力学超材料及上下两个直径不同相连接的双圆锥结构单元[168]；(b) 无触感的弹性机械波斗篷[170]；(c) 扭转机械超材料[171]
Figure 15. Mechanical metamaterial structures and devices.(a) Pentamode metamterials and structural unit of two connected truncated cones[168]; (b) An elasto-mechanical unfeelability cloak made of metamaterials[170]; (c) A twist mechanical metamaterials[171]
图 16 可驱动的微机械器件。(a) 可远程磁驱动的微型转子、微型盾构机和三维螺旋推进器[176]；(b) pH响应蜘蛛微型机器人和智能微型抓手[179]；(c) 基于液晶弹性体的微型步行者[180]；(d) 基于光镊驱动的微机械转子[181-182]
Figure 16. Drivable micromechanical devices. (a) Remote magnetically actuated micro-rotor, micro-shield machine and 3D helical thruster[176]; (b) The pH-responsive spider micro-robot and smart micro-gripper[179]; (c) The liquid crystal elastomer-based micro-walker[180]; (d) Optical tweezers-driven micromechanical rotor[181-182]
图 17 微流道器件。(a) 微泵[185]；(b) 微涡轮[186]；(c) 微筛[188]；(d) 微过滤器[189]；(e) 微阀门[190]；(f) 微混合器[191]；(g) 微混合器和过滤器[191]；(d) 微立交桥器件[192]
Figure 17. Microfluidic device. (a) Micropump[185]; (b) Microturbines[186]; (c) Microsieves[188]; (d) Microfilters[189]; (e) Microvalve[190]; (f) Micromixer[191]; (g) Micromixer and filters[191]; (d) Micro-overpass devices[192]
聚合类型 自由基聚合 阳离子聚合 光解离 PI$ \begin{array}{*{20}{c}} {}&{\xrightarrow{{\begin{array}{*{20}{c}} 2 \hbar v \end{array}}}}&{}&{} \end{array} $PI* → R* PI$ \begin{array}{*{20}{c}} {}&{\xrightarrow{{\begin{array}{*{20}{c}} 2 \hbar v \end{array}}}}&{}&{} \end{array} $PI* → K+ 引发聚合 R* + M → RM* K+X− + M → KM+X− 链增长 RM* → RMM* → RMnR KM+X− + M → KMn+X− 链终止 Primary radical termination: RM* + R* → RMnRRecombination: RMn* + RMm* → RMn+mRDisproportionation: RMn* + RMm* → RMn+RMm Ionic rearrangement: KMn+X− → KMn + H+X−Chain transfer: KMn+X− + M → KMn + HM+X− 常见材料 (甲基)丙烯酸酯、乙烯基、硫醇、水凝胶、有机-无机杂化材料 主要是环氧树脂 商用光刻胶 SCR500, IP-L, IP-G, IP-Dip, SZ2080, PEG-DA,
PETA, OrmoComp, Ormocer, PDMSSU-8, SCR-701 
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