中国光学十大进展:三维无机微纳结构的激光加工与应用(特邀)‡【增强内容出版】
1 引言
无机材料具有优异的热稳定性和化学稳定性,较高的刚度和硬度,出色的光、电、磁学特性,在科研生产和日常生活中日益发挥重要作用。基于无机材料所制备的三维(3D)无机微纳结构具有小尺度、高精度等特点,能够适应高温、高压等极端环境。因此,3D无机微纳结构在光学微器件[1-2]、光数据存储和信息加密[3-4]、量子芯片[5-6]、航空航天[7-8]、微流控系统[9-10]和仿生学[11-12]等领域有着广泛的应用前景。
3D无机微纳结构的传统制备方法如化学刻蚀[13-14]、溶胶-凝胶法[15-16]、模板法[17-18]等,大多存在过程繁琐、复杂图案受限、精度较低、加工时间长等问题。因此,研究人员开发了一系列新的无机微结构加工技术:利用熔融沉积成型[19-20]制备机械性能良好的陶瓷,形成曲面、齿轮、牙齿等复杂结构;诱导自组装[21-22]析出晶体结构,产生特定形貌特征;通过墨水直写技术[23-25],将特制纳米复合油墨从喷嘴挤出,打印出具有良好的光学性能和折射率梯度的无机平板光学微器件;使用数字光3D打印技术[26]加工出具有复杂3D形状的陶瓷刀具。这些微纳加工技术增强了对复杂微图案的设计加工能力,但尚难以精准构筑具有高精度和高分辨率的复杂3D无机微结构,仍无法满足各领域对3D无机微结构微型化、集成化和高性能化的新需求。
激光加工技术作为制备3D微纳结构的重要手段,能够实现真3D、高分辨、多尺度3D微纳结构加工,包括连续激光加工技术和超快脉冲激光加工技术。连续激光加工技术是以连续激光作为光源,经过聚焦后作用于加工对象,属于“热加工”技术[27-28]。超快激光加工技术作为一种新兴技术手段,具有超短激光脉冲、超高能量密度的特点[29-31],有望加工出具有复杂结构和高分辨率的3D无机微纳结构。由于与材料相互作用的时间极短,超快激光辐照区域的热效应几乎可以忽略不计,被认为是“冷加工”技术。超快激光加工技术可以通过加工纯无机材料、有机-无机杂化材料以及聚合物模板辅助等途径得到3D无机微纳结构。Liu等[32]利用超快飞秒激光诱导化学键合,以超越衍射极限的分辨率直接打印出任意3D量子点结构,有望应用于制造自由形态的量子点光电器件。Bauer等[33]采用有机-无机低聚倍半硅氧烷(POSS)光刻胶,利用飞秒激光结合高温烧结,形成3D高精度石英玻璃微纳结构和光子学器件。激光加工3D无机微纳结构无需掩模版、无污染、零接触、适合材料范围广,可以用来制备结构紧凑、尺寸小的集成化微结构,在光学器件[34]、微流控[35]、量子芯片[36]、仿生学[37-38]等领域有着广阔的前景。
本文介绍了激光加工3D无机微纳结构的研究进展与发展现状。首先简要概括了连续激光、皮秒激光加工制备的3D无机微结构,进一步详细讨论了基于纯无机材料体系、有机-无机杂化体系以及聚合物模板辅助等的飞秒激光加工3D无机微纳结构的研究现状。随后,本文总结了激光加工3D无机微纳结构在光学器件、量子芯片、信息存储与防伪、航空航天以及仿生学等领域的应用。最后,对激光加工3D无机微纳结构的未来发展趋势进行了展望。
2 3D无机微纳结构的激光加工技术
激光加工技术具有高精度、非接触、可控性强、材料适应性广等特点,通过光与物质相互作用,实现对材料的切割、打孔、雕刻和微结构加工等。激光加工技术按照使用的光源类型可分为连续激光加工技术和脉冲激光加工技术,其中脉冲激光加工技术主要基于皮秒激光和飞秒激光。激光加工技术具有高分辨、低成本的优势,成为构筑3D无机微结构的重要途径。近年来,激光加工制备的各种3D无机微结构已经广泛应用于**建设和生命健康等领域。
2.1 连续激光加工3D无机微纳结构
连续激光加工3D无机微结构是无机材料通过吸收激光能量,发生各种物理化学效应,从而形成所需的3D无机微结构。Hu等[3]发现在473 nm半导体激光照射下,稀土离子掺杂的磷酸钨玻璃产生可逆的发光调制,颜色由浅黄色变为蓝色,实现了信息数据在透明玻璃内的任意写入与擦除[
图 1. 连续激光加工3D无机微纳结构。(a)473 nm连续激光在玻璃内写入图案信息[3];(b)CO2激光加工的105层3D玻璃结构的实物照片(左)和侧壁截面的光学显微镜图像(右)[39];(c)CO2激光加工的玻璃微透镜阵列,右图是单个微透镜成像效果图[40];(d)442 nm连续激光加工的3D透明玻璃微结构[41];(e)980 nm 连续激光打印的3D无支撑陶瓷微结构[42]
Fig. 1. Continuous wave (CW) laser fabrication of 3D inorganic micro and nanostructures. (a) 473 nm CW laser writes patterning information in glass [3]; (b) photograph of 105 layers glass structure processed by CO2 laser (left), optical microscope image of sidewall section (right) [39]; (c) glass microlens array processed by CO2 laser, the image on the right is the image effect of a single microlen[40]; (d) 3D transparent glass microstructures processed by 442 nm CW laser[41]; (e) unsupported ceramic microstructures fabricated by 980 nm CW laser [42]
2.2 皮秒激光加工3D无机微纳结构
皮秒激光加工技术由于高峰值功率密度能够实现3D微纳结构的加工。皮秒脉冲激光与材料作用时间短,有效地降低了连续激光加工中的热效应,能够以较低的热影响实现复杂3D微纳结构的加工。皮秒激光加工技术在无机微纳结构加工中具有独特的优势和应用潜力,可以实现高断裂强度的区域焊接[43]。Penilla等[44]利用皮秒激光脉冲照射,在室温条件下将具有复杂形状的陶瓷微结构进行焊接,有望应用于温度敏感的微机械系统等领域[
图 2. 皮秒激光加工3D无机微纳结构。(a)皮秒激光焊接陶瓷组件[44];(b)损伤通道端面图[46];(c)皮秒激光在透明玻璃内嵌入3D结构[47];(d)皮秒激光加工HSQ得到玻璃3D微结构[51]
Fig. 2. Picosecond laser fabricating 3D inorganic micro and nanostructures. (a) Picosecond laser welding ceramic components[44]; (b) end face of damaged channel[46]; (c) picosecond laser embedded 3D structure in transparent glass[47]; (d) 3D microstructure of glass fabricated by picosecond laser fabricating HSQ[51]
2.3 飞秒激光加工3D无机微纳结构
飞秒激光作为一种“冷加工”技术[52-53],已经成为精密加工领域的重要手段,可以制备出高精度、复杂3D微结构。飞秒激光加工3D无机微纳结构按照所使用材料的不同,大致可以分成三类。第一类是使用飞秒激光直接加工纯无机材料如玻璃、光学晶体、陶瓷和量子点等形成3D无机微纳结构。第二类是利用飞秒激光加工有机-无机杂化材料先形成复杂3D微纳结构,然后经过热处理去除有机成分,形成致密的、光学性质和机械性能优良的3D无机微纳结构。有机-无机杂化材料又分为可转化为无机材料的光刻胶前驱体,以及无机纳米颗粒掺杂有机光刻胶两种材料体系。第三类是通过聚合物模板法辅助制备3D无机微纳结构,即通过飞秒激光加工先制备出聚合物模板,再利用沉积、溅射等手段将无机材料涂覆在表面,最后经过热处理、等离子体刻蚀、特定溶液降解等去除聚合物得到3D无机微纳结构。
2.3.1 飞秒激光加工纯无机材料制备3D无机微纳结构
玻璃具有优良的透光性、化学稳定性、生物相容性、机械强度等,玻璃微纳结构在集成光子学和量子芯片等领域中具有极大的应用价值。1996年,Davis等[54]首次利用810 nm飞秒激光在块体玻璃内部留下微纳线条结构,证明飞秒激光可在玻璃内部书写光波导结构[
图 3. 飞秒激光加工玻璃基质的3D无机微纳结构。(a)飞秒激光在玻璃内写入永久痕迹[54];(b)飞秒激光在玻璃内写入低损耗的弯曲波导[56];(c)飞秒激光在掺Au玻璃内部的图案化[62];(d)飞秒激光在玻璃内写入包含深度信息的图像[64];(e)飞秒激光在玻璃中制备3D CsPbBr3纳米晶体结构[65];(f)飞秒激光在HSQ上加工3D无机微结构[69]
Fig. 3. Femtosecond laser fabrication of 3D inorganic micro and nanostructures in glass. (a) Permanent trace in glass[54]; (b) femtosecond laser writes low loss curved waveguide in glass[56]; (c) patterning of femtosecond laser inside Au doped glass[62]; (d) femtosecond laser writing of depth information in glass[64]; (e) CsPbBr3 nanocrystalline structures prepared by femtosecond laser[65]; (f) femtosecond laser writing 3D inorganic microstructure based on HSQ[69]
光学晶体具有较大的非线性光学系数、稳定的理化性质和良好的机械强度,被用于制备光波导、光调制器等光子学器件。研究人员利用飞秒激光加工技术在钇铝石榴石(YAG∶Nd3+)晶体[70]、硫化锌(ZnS)晶体[71]、掺铥氟化钇锂(Tm∶YLF)晶体[72]、三硼酸锂(LBO)晶体[73]、铌酸锂晶体(LiNbO3)[74]、钛蓝宝石(Ti∶ sapphire)晶体[75]和蓝宝石(sapphire)晶体[76]中制备了预定形状的波导结构[
图 4. 飞秒激光在光学晶体中加工3D无机微纳结构。(a)YAG∶Nd3+中刻写的凹陷包层波导的端视图[70];(b)LiNbO3晶体中写入波导端面图[74];(c)ZnS晶体中波导的截面[71];(d)LBO晶体中产生的双线(No.1)和凹陷包层(No.2)波导[73];(e)飞秒激光在LiNbO3晶体中的纳米级调控[78];(f)飞秒激光在LiNbO3晶体中写入特定图案的全息图像[80]
Fig. 4. Femtosecond laser fabricating 3D inorganic micro and nanostructures in optical crystal. (a) End view of concave cladding waveguide written in YAG∶Nd3+ [70]; (b) waveguide end face written in LiNbO3 crystal[74]; (c) cross section of waveguide in ZnS crystal[71]; (d) double line (No.1) and concave cladding (No.2) waveguides generated in LBO crystal[73]; (e) nanoscale regulation of femtosecond laser in LiNbO3 crystal[78]; (f) femtosecond laser writes holograms of specific patterns in LiNbO3 crystal[80]
量子点因其优异的光学性能和尺寸调控特性,而被广泛应用于微纳发光器件和显示等领域。Liu等[32]提出光激发诱导化学键合,利用飞秒激光照射半导体量子点激发出的空穴转移到纳米晶体表面,从而诱导粒子间的化学键合,打印出高精细3D量子点结构[
图 5. 飞秒激光加工3D量子点、陶瓷微结构。(a)飞秒激光诱导量子点化学键合形成3D无机微纳结构[32];(b)飞秒激光打印混合量子点形成3D纳米柱阵列[81];(c)飞秒激光在陶瓷中以螺旋式运动加工圆形波导[84]
Fig. 5. Femtosecond laser fabrication of 3D inorganic micro and nanostructures based on ceramics and quantum dots. (a) Femtosecond laser-induced chemical bonding of quantum dots to form 3D inorganic micro and nanostructures[32]; (b) femtosecond laser printing of mixed quantum dots to form a 3D nanopillar array[81]; (c) femtosecond laser fabricating circular waveguides in ceramics with spiral motion[84]
陶瓷材料因其硬度大、脆性大、耐高温、耐磨损、耐腐蚀的优势,广泛用于航空航天、电子器件、生物医药等领域。但其较大的刚硬度和较差的透明度,导致传统加工方式难以制造出3D异形结构。而利用飞秒激光加工技术,无需掩模版就能够高精度地加工复杂陶瓷微结构。Castillo-Vega等[83]对光学透明氧化钇稳定氧化锆(YSZ)陶瓷进行激光加工,辐照区域光学性质发生永久性变化。随后沿螺旋轨迹写入激光,成功制备出圆形波导[84][
2.3.2 飞秒激光加工有机-无机前驱体光刻胶制备3D无机微纳结构
飞秒激光加工有机-无机前驱体光刻胶能够制备出3D无机微结构。首先,利用飞秒激光加工出前驱体光刻胶微纳结构,再经过高温处理等去除有机成分,得到3D无机微纳结构[85][
图 6. 飞秒激光在含无机组分的前驱体光刻胶中加工3D无机微纳结构。(a)自支撑非球面微透镜[85];(b)十四面体晶胞[86];(c)自由形态雕塑[87];(d)微米十字扭转结构[88];(e)干燥收缩过程引起3D结构裂纹[89];(f)多孔微通道结构[90];(g)印刷在支撑柱上的微透镜[91];(h)150 μm高的多透镜衍射微物镜[33]
Fig. 6. Femtosecond laser fabricating of 3D inorganic micro and nanostructures in precursor photoresist containing inorganic components. (a) Self supporting aspheric microlens [85]; (b) tetrahedral cell [86]; (c) free form sculpture [87]; (d) micron cross torsion structure [88]; (e) drying shrinkage process causes 3D structural cracks [89]; (f) porous microchannel structure [90]; (g) microlens printed on support column [91]; (h) 150 μm-high diffractive micro objective lens[33]
2.3.3 飞秒激光加工无机纳米颗粒掺杂光刻胶体系制备3D无机微纳结构
通过将无机纳米颗粒掺杂到有机光刻胶中,利用飞秒激光加工结合高温烧结,即“掺杂-加工-烧结”工序,可实现3D无机微纳结构的制备。Kotz等[92]利用飞秒激光直写含SiO2纳米颗粒的光刻胶,制备了具有几十微米分辨率和表面粗糙度约为6 nm的3D熔融石英玻璃,该结构在780 nm波长处显现出91.6%的高透明度[
图 7. 飞秒激光加工无机纳米粒子掺杂的光刻胶制备3D无机微纳结构。(a)透明玻璃微结构[92];(b)悬垂线[93];(c)玻璃圆盘桁架结构(左)和八面体桁架结构(右)[94];(d)陶瓷点阵立方体[95]
Fig. 7. Femtosecond laser fabrication of 3D inorganic micro and nanostructures based on inorganic nanoparticles doped photoresists. (a) Transparent glass microstructure[92]; (b) pendant [93]; (c) disk truss structure (left) and octahedral truss structure (right)[94]; (d) ceramic lattice cube [95]
2.3.4 聚合物模板法辅助制备3D无机微纳结构
飞秒激光加工技术还可以通过聚合物模板法辅助加工3D无机微纳结构。首先,利用飞秒激光加工出3D聚合物微结构作为模板,随后通过沉积、溅射等将无机材料涂覆在聚合物模板表面,经热处理、等离子体刻蚀、特定溶液降解等去除模板获得3D无机微纳结构。Meza等[96-97]采用飞秒激光加工3D支架结构,通过原子层沉积在支架上沉积一层氧化铝薄膜,利用聚焦离子束打磨最外层和氧等离子体刻蚀技术制备了空心管状氧化铝纳米点阵[
图 8. 聚合物模板法辅助飞秒激光加工制备3D无机微纳结构。(a)氧化铝八面体桁架纳米晶格[97];(b)DNA双螺旋中空玻璃微结构[10];(c)3D硅纳米结构[98];(d)双壁陶瓷纳米晶格[99];(e)3D中空螺旋微管结构[100]
Fig. 8. 3D inorganic micro and nanostructures prepared by the polymer template assisted femtosecond laser fabrication method. (a) Alumina octahedral truss nanolattice[97]; (b) microstructure of DNA double helix hollow glass[10]; (c) 3D silicon nanostructure[98]; (d) double-well ceramic nanolattice[99]; (e) 3D hollow spiral microtubule structure[100]
3 应用
激光加工技术无接触、无污染、加工速度快、精度高,是制备3D无机微纳结构的重要手段。与传统加工技术相比,激光加工技术更能满足新型功能器件微型化、集成化的发展需求,制备出形状尺寸可控的复杂3D无机微纳结构,在微型光子学器件、量子技术、信息存储与加密、航空航天以及仿生结构等领域有着广泛的应用。
3.1 光学器件
激光加工技术制备的3D无机微纳结构广泛应用于构筑微型光学器件,如集成光子学的基本元件回音壁微谐振腔、自由曲面透镜等。Fang等[101]利用飞秒激光在LiNbO3中制备了品质因子高达107的回音壁微谐振腔。Wen等[94]基于SiO2纳米复合材料打印出高品质因子的微环回音壁谐振腔[
图 9. 3D无机微结构在光学微器件中的应用。(a)微环光学谐振腔[94];(b)玻璃微透镜[92];(c)Alvarez透镜[2];(d)菲涅耳透镜[69];(e)光子微型环芯谐振器[51];(f)非球面轮廓的平凸微透镜[33]
Fig. 9. Application of 3D inorganic microstructure as optical micro devices. (a) Microring optical resonator[94]; (b) glass microlens[92]; (c) Alvarez lens[2]; (d) Fresnel lens[69]; (e) photonic micro ring resonator[51]; (f) plano convex microlens with aspheric profile[33]
3.2 量子芯片
量子芯片作为量子计算机的核心,是目前各国竞相追逐的科学前沿。利用飞秒激光在玻璃、铌酸锂等无机材料中加工微型波导等结构,是构筑量子芯片的重要途径。Flamini等[102]利用飞秒激光在玻璃中写入动态可重构的集成光子电路,实现了对单光子态和双光子态的调控,条纹可见度大于95%,为可重构光量子电路开辟了道路[
图 10. 激光加工3D无机微纳结构应用于量子芯片。(a)飞秒激光图案化加工电阻器[102];(b)飞秒激光在玻璃内部直写光波导(左)和波导定向耦合器(右)[104];(c)飞秒激光直写3D波导阵列(左上),光子晶格截面图(左下),3D波导阵列中一个波导耦合到其他波导的示意图(右上),单光子在晶格中量子行走后输出的演化图案(右下)[106];(d)飞秒激光直写路径编码三量子比特Toffoli门[107]
Fig. 10. Laser fabrication of 3D inorganic micro and nanostructures for quantum chips. (a) Femtosecond laser patterns resistors[102]; (b) femtosecond laser directly writing optical waveguide (left) and waveguide directional coupler (right)inside the glass[104]; (c) femtosecond laser direct writing 3D waveguide array (top left), photonic lattice section (bottom left), schematic diagram of coupling one waveguide to other waveguides in a 3D waveguide array (upper right), and evolution pattern of single photon output after quantum walk in the lattice (lower right)[106]; (d) 3D layout of three qubit Toffoli gate encoded by femtosecond laser direct writing path[107]
3.3 信息存储与加密
3D无机微纳结构存储信息具有长期稳定性和多样性,通过设计和组装能够大大提高存储容量和存储稳定性。1996年,Glezer等[109]利用飞秒激光脉冲聚焦在透明材料内部,产生较大折射率的亚微米比特,可用于永久性的3D光学数据存储。Smetanina等[110]利用飞秒激光脉冲在掺银磷酸盐玻璃中诱导形成局域二次和三次谐波,实现非线性光数据存储。在3D无机微纳结构中结合量子点的荧光特性,通过光学防伪进一步保障信息存储的安全性。2020年,Huang等[66]利用飞秒激光在玻璃中形成蓝光钙钛矿纳米晶,可以在玻璃中写入3D图案,该荧光图案在激光的照射下,可以局部擦除后恢复,为信息存储安全、防伪编码提供了应用价值[67][
图 11. 激光加工3D无机微纳结构的应用。(a)飞秒激光擦除/恢复过程[66];(b)QR码加密演示[67];(c)Cl-Br-—I-共掺杂玻璃图案化[65];(d)激光焊接侧面图[112];(e)激光焊接成功的装配图[44];(f)传感器内的垂直波导[7];(g)储仓微结构[115];(h)圆偏振激光脉冲加工熔融石英[117];(i)裸石英玻璃和带有抗反射结构的石英玻璃效果对比[118];(j)截锥阵列[119]
Fig. 11. Application of laser fabricated 3D inorganic micro and nanostructures. (a) Femtosecond laser erasure/recovery[66]; (b) QR code encryption demonstration[67]; (c) patterning of Cl-Br-—I- codoped glass[65]; (d) side view of laser welding[112]; (e) assembly drawing of successful laser welding[44]; (f) vertical waveguide in the sensor[7]; (g) microstructure of storage bin[115]; (h) fabrication of fused quartz by circularly polarized laser pulses[117]; (i) effect comparison between bare quartz glass and quartz glass with anti-reflective structure[118]; (j) truncated cone array [119]
3.4 航空航天
航空航天领域的零部件需要耐高温、优良机械性能、高精度等性质来应对极端的外界环境。陶瓷因其低导热系数、低密度等优良性质,成为航空航天零部件的重要材料。激光加工可以实现陶瓷等材料的焊接及其他加工技术,在航空航天器的组装、修复与维护中发挥着重要作用。Tamaki等[111]利用飞秒激光在不使用胶水等中间层的情况下实现透明玻璃材料间缝隙小于λ/4的焊接。Richter等[112]则实现3 μm的均匀间隙焊接,且成功焊接的熔融石英稳定性达原始材料85%[
3.5 仿生学
激光加工技术能够制备出多种仿生无机微结构,造福人类。Lee等[114]根据梯度硅基膜模拟原始人类毛细胞频率的选择功能,结合激光剥离制备出柔性无机压电纳米声传感器。Liang等[115]利用飞秒激光在石英玻璃上刻写新型3D仿生光滑表面,该结构将润滑剂储存在内部,在毛细管力的作用下运输到表面,具有良好的表面耐久性和光学透光率[
4 结束语
激光加工技术无论是在精度还是图案设计自由度上,都呈现出优异的加工能力,广泛应用于科学研究、**民生等领域[120-121]。近年来,激光加工3D无机微纳结构分辨率达到纳米量级,突破光学衍射极限,实现了复杂微纳结构的3D制备,为微纳尺度下多种材料高精度的加工提供了基础,也为微纳电子器件、光学微器件、超表面、量子芯片等领域的发展提供了重要支撑。目前,飞秒激光加工3D无机微纳结构多采用逐点扫描的方式,加工效率较低,不适合批量化生产。飞秒激光与数字微镜(DMD)结合能很好地解决该问题,通过DMD面投影,能够快速地加工出大面积、复杂微结构,大大提高了加工效率[122-124]。Saha等[125]基于投影逐层打印出宽度小于175 nm的纳米线,完成亚微米分辨率的任意复杂3D结构。Liu等[126]提出使用高效跨尺度图案化的无掩模光学投影纳米光刻技术,单次曝光实现最小特征尺寸32 nm,突破了光学衍射极限,进一步实现了尺寸超数百微米、精度达数十纳米的微结构的快速制备。Wang等[127]利用无掩模光学投影技术制备Ag/聚苯胺壳-核结构的纳米复合材料,在多种基底上制备出微纳尺度下的纳米复合图案,且具有一定的导电性和表面增强拉曼特性,为传感器和探测器等微纳器件的制备开辟了新的途径。然而,目前基于DMD的飞秒激光加工技术主要针对有机材料,将其与无机微纳结构的加工相结合,必将大大提高3D无机微纳结构的加工效率。随着新材料和新技术的不断发展,激光加工制备3D无机微纳结构必将在光学、信息、能源、生物工程等领域展示出更为广阔的应用前景。
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Article Outline
章剑苗, 金峰, 董贤子, 郑美玲. 中国光学十大进展:三维无机微纳结构的激光加工与应用(特邀)‡[J]. 激光与光电子学进展, 2024, 61(19): 1900001. Jianmiao Zhang, Feng Jin, Xianzi Dong, Meiling Zheng. China