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摘要:
激光化学气相沉积技术(LCVD)相较于传统化学气相沉积技术具有低沉积温度、高膜层纯度、高沉积效率等特点，在各类功能薄膜材料制备上有着巨大的应用前景。围绕激光化学气相沉积技术，本文详细阐述了激光热解离、激光光解离与激光共振激发解离作用机制，同时介绍了各类LCVD的常用设备，着重总结了LCVD在金属材料、碳基材料、氧化物材料以及半导体材料等各类材料制备应用上的最新研究进展，特别介绍了LCVD制备过程中常用的检测与分析方法，最后讨论了激光化学气相沉积技术目前所面临的挑战与机遇，并展望了该技术的发展前景。
Abstract:Laser chemical vapor deposition (LCVD) technology has its unique advantages in reducing deposition temperatures, enhancing film purity and directly writing complex thin film patterns compared with conventional chemical vapor deposition (CVD). This technology has been widely applied in thin film deposition and attracted growing attention from both research and industries. This review categorizes the LCVD technology into three types according to the laser-matter interaction mechanisms, including laser pyrolysis, laser photolysis, and laser resonance excitation sensitization. We illustrate the deposition principles governed by the three different mechanisms in detail, and briefly introduce the commonly used equipment, and summarize the latest research progress of LCVD technology in synthesis and applications of metals, carbon-based materials, oxides and semiconductors. The detection and analysis methods used in LCVD are specially introduced, and the challenges and prospects of LCVD in material synthesis are discussed.
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Overview: Laser chemical vapor deposition (LCVD) is a promising method for selective deposition of solid materials via localized chemical vapor reaction driven by a laser beam. It has several advantages over traditional CVD processes including decreased deposition temperature, increased deposition rate, higher crystallization quality, superior spatial resolution, site-selective deposition characteristics and the ability to produce a wide range of complex 3D micro- and nanostructures. In this review, LCVD is divided into three types based on the interaction mechanisms of laser and gaseous precursor, i.e., pyrolytic LCVD, photolytic LCVD and vibrational excitation LCVD. In pyrolytic LCVD processes, a focused laser beam triggered by a continues CO2 laser or Nd:YAG laser is used to locally heat the surface of the substrate and material deposition occurs when the temperature near the irradiated area reaches the decomposition threshold of the gaseous precursor. This approach is often used to deposit small regions of 2D films with complex and fine patterns. Photolytic LCVD processes use photons from focused laser beams (typically generated by short-wavelength ultraviolet laser light source, such as excimer laser and high frequency output of Nd:YAG laser) to reactant gases, resulting in precise deposition of solid material in either 2D films or 3D structures. Photolytic LCVD processes rely on the photochemical action of the laser beam and the chemical reactants. The precursor gas molecules are directly dissociated by the high-energy photons and subsequently form a solid deposit on the surface of the substrate through recombination/re-decomposition. Photolytic LCVD typically utilizes pulsed lasers as their high peak power levels more effectively to drive the chemical reactions. This method is suitable for large-area film formation. Vibrational excitation LCVD often uses laser sources with adjustable wavelengths, such as infrared CO2 lasers and OPO lasers. By precisely modulating the laser wavelength, the laser energy is directionally coupled to selected gas molecules to induce efficient dissociation of key reaction molecules, resulting in deposition of solid material in a low ambient temperature. Vibrational excitation LCVD typically offers a higher deposition rate and a better film quality compared to the photolysis of the precursors with a UV laser. In this article, we first introduce the deposition principles and commonly used equipment of the three LCVD processes, and then a comprehensive survey of recent material deposition applications using this three LCVD approaches is presented. Finally, the challenges and opportunities in the application of LCVD for material preparation are summarized, and the development prospects of this technology are prospected.
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图 3 (a) 2.44 W沉积的W膜孕育、成核和聚结三阶段图；(b) 沉积时间对W膜沉积厚度的影响；(c) 激光功率对W薄膜表面形貌的影响[81]
Figure 3. (a) Plot of three regimes for incubation, nucleation and coalescence of W deposited at 2.44 W; (b) Thickness of W films deposited on glass substrates plotted as a function of deposition time; (c) Surface morphology of deposited W films deposited at different laser power[81]
图 5 (a) 在不同激光功率、沉积压力和沉积温度下制备的β-SiC薄膜XRD图；(b) 激光功率和沉积压力对 β-SiC 薄膜择优取向的影响[97]
Figure 5. (a) XRD patterns of the β-SiC films prepared at different laser power, deposition pressure and deposition temperature; (b) Effects of laser power and deposition pressure on preferred crystalline orientations of β-SiC films[97]
图 6 使用传统CVD于1173 K制备的HfO2薄膜(a)表面和(b)横截面扫描电镜图像，使用热解LCVD于1203 K和1383 K制备的HfO2薄膜(c), (e)表面和(d), (f)横截面扫描电镜图像，(c), (e) 沉积温度对(g)常规CVD和(h)热解CVD制备的HfO2薄膜沉积速率、微晶尺寸、以及形态演化的影响[71]
Figure 6. (a) Surface and (b) cross-sectional SEM images of HfO2 films prepared using conventional CVD at 1173 K, (c), (e) surface and the corresponding (d), (f) cross-sectional SEM images of (c), (d) HfO2 films prepared at 1203 K and (e), (f) HfO2 films prepared at 1383 K by pyrolysis CVD, effect of deposition temperature on deposition rate, crystallite size, and morphological evolution in HfO2 films prepared using (g) conventional CVD and (h) pyrolysis CVD[71]
图 7 激光功率150 W，沉积温度分别在760 K (a, b)、957 K (c, d)和1104 K (e, f)时在石英玻璃上制备的SrTiO3薄膜表面和横截面SEM图像；(g) 沉积温度对SrTiO3薄膜厚度、晶粒尺寸、晶粒形状和择优取向的影响[128]
Figure 7. Surface and cross‐sectional SEM images of the SrTiO3 films prepared at 760 K (a, b) , 957 K (c, d) and 1104 K (e, f) with a laser power of 150 W, respectively; (g) Influences of the deposition temperature on thickness, grains size, grains shape, and preferred orientation of the SrTiO3 films[128]
图 8 在1523 K和400 Pa下沉积的具有类纳米森林结构的3C-SiC/石墨烯复合薄膜的(a)，(b)TEM形貌(c)原子构型，具有稳定框架和连续电子路径的3C-SiC/石墨烯复合薄膜的(d)示意图与(e)循环性能测试图[136]
Figure 8. (a), (b) TEM observations and (c) atomic configuration of the nanoforest-like 3C-SiC/graphene composite films deposited at 1523 K and 400 Pa, (d) schematic illustration and (e) cycling performance of 3C-SiC/graphene nanoforest composite films with stable framework and continuous electron pathways[136]
图 9 光解LCVD常用实验装置以及光解机制示意图
Figure 9. Commonly used experimental setup and principle of photolysis LCVD
图 10 不同激光功率下沉积的W图案SEM 照片和相应的 3D 图像。
Figure 10. SEM photographs and corresponding 3D images of the deposited tungsten patterns for various laser power.
图 12 在衬底预热温度423 K时不同激光功率制备的TiNx薄膜表面和横截面图。
Figure 12. Surface image surface and cross-sectional SEM images of TiNx films prepared at Tpre = 423 K with varied laser power.
图 14 激光共振激发LCVD常用实验装置
Figure 14. Commonly used experimental setup for laser resonant excitation LCVD
图 15 激光共振激发对CVD制备碳纳米洋葱的影响。
Figure 15. The influence of laser resonant excitation on CVD of carbon nano-onions.
图 16 LCVD制备的掺硼金刚石以及其电极的血糖传感器性能表征。
Figure 16. BDD prepared using resonant excitation LCVD method and their electrochemical performance in glucose tests.
图 18 (a) CO2激光辅助燃烧化学气相沉积实验装置与不同激光激励下NH3/C2H2/O2火焰的(b)发射光谱和(c)质谱分析所得到的火焰中离化基团的相对摩尔分数[181]；(d) C2H4/C2H2/O2火焰的光学图像[184]
Figure 18. (a) Experimental setup for the CO2 laser-assisted CCVD and (b) optical emission spectra and (c) mole fractions of the species of NH3/C2H2/O2 flames under different laser excitations measured using mass spectrometer[181]; (d) Optical images of C2H4/C2H2/O2 flames[184]
表 1 各类化学气相沉积技术对比
Table 1. Comparison of various CVD techniques
技术类别 优点 缺点 MOCVD 大面积制备，高沉积精度 设备成本高，材料要求苛刻，沉积速度慢 PCVD 较低沉积温度，较快沉积速度，设备维护简单 反应过程复杂难以控制 HFCVD 大面积制备，适用于复杂形貌，操作系统简单 沉积速度慢 CCVD 大气环境下制备 沉积速度慢 LCVD 可局部制备，高沉积精度/效率/质量，成膜材料种类广泛 设备成本高，操作略复杂 
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表 3 最近热解LCVD薄膜制备研究工作
Table 3. Recent reports of thin film deposition using pyrolysis LCVD
年 材料 基体 光源 沉积参数 温度/(°C) 速率/(μm/h) 2021[28] SmBa2Cu3O7-δ LaAlO3 波长808 nm半导体连续激光器 780 8.76 2020[71] HfO2 AlN 波长976 nm半导体连续激光器 600~1300 67 2020[72] BCN SiO2 波长1064 nm Nd:YAG连续激光器 1100 18.4 2020[73] ZrCN C Nd:YAG连续激光器 1100~1180 40 2020[74] SrTiO3 MgAl2O4 波长1064 nm Nd:YAG连续激光器 900 20 2020[75] Y-doped BaZrO3 AlN 波长1064 nm Nd:YAG连续激光器 645.1~656.3 2.67 2020[76] β-Yb2Si2O7, X1/X2-Yb2SiO5 AlN 波长808 nm半导体连续激光器 750~1100 114~423、353~943 2019[77] LaPO4 Al2O3 波长1064 nm Nd:YAG连续激光器 802~847 58.6 2019[78] SiBCN Graphite 波长1064 nm Nd:YAG连续激光器 1210~1410 1620
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表 4 最近光解LCVD制备薄膜的工作总结
Table 4. Reports of thin film deposition using photolysis LCVD recently
年 材料 基体 光源 沉积参数 温度/(°C) 速率/(μm/h) 2020[141] 金刚石 Si 波长532 nm超高斯分布连续激光器 700~900 0.38 2019[47] W TFT-LCD 波长351 nm脉宽45 ns Nd:YAG脉冲激光器 > 450 - 2018[59] 金刚石 WC 波长193 nm脉宽15 ns ArF、波长248 nm脉宽20 ns KrF准分子激光器 2177 11、10.3 2018[142] β-SiC β-SiC 波长808 nm InGaAlAs半导体激光器 1067~1257 50 2018[143] Si3N4 Si/PET 波长193 nm ArF
准分子激光器100 0.93 2017[144] Ni U 波长248 nm KrF
准分子激光器165~200 - 2011[145] Cr2O3 Al2O3 波长248 nm脉宽30 ns KrF准分子激光器 室温 360
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