铌酸锂晶体超精密加工技术研究进展

田业冰; 魏成伟; 宋晓梅; 钱乘

doi:10.13394/j.cnki.jgszz.2024.0011

铌酸锂晶体超精密加工技术研究进展

doi: 10.13394/j.cnki.jgszz.2024.0011

田业冰^1, ,,
魏成伟^1,,
宋晓梅^{1, 2, ,},
钱乘^1,

1.
山东理工大学机械工程学院, 山东淄博 255000
2.
山东理工大学计划财务处, 山东淄博 255000

基金项目: 国家自然科学基金(51875329)；山东省泰山学者工程专项(tsqn201812064)；山东省自然科学基金(ZR2023ME112, ZR2017MEE050)。

详细信息

通讯作者:
田业冰，男，1979年生，博士、教授、博士研究生导师。主要研究方向：精密/超精密加工技术与装备。E-mail：tianyb@sdut.edu.cn ; tyb79@sina.com

宋晓梅，女，1980年生，硕士。主要研究方向：精密与特种加工、数字化设计与制造。E-mail：songxm@sdut.edu.cn

中图分类号: TH706
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- HTML全文浏览量: 22
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- 被引次数: 0
出版历程
- 收稿日期: 2024-01-12
- 修回日期: 2024-07-09
- 录用日期: 2024-07-19
- 网络出版日期: 2025-01-11
- 刊出日期: 2024-12-06

Recent advances in ultra-precision machining of lithium niobate crystals

TIAN Yebing^{1
, ,},
WEI Chengwei^1
,,
SONG Xiaomei^{1, 2
, ,},
QIAN Cheng^1
,

1.
School of Mechanical Engineering, Shandong University of Technology, Zibo 255000, Shandong, China
2.
Financial Affairs Office, Shandong University of Technology, Zibo 255000, Shandong, China

摘要

摘要: 铌酸锂（LiNbO₃）晶体光电特性优异，是制造光学调制器、频率倍增器、滤波器等光电子器件的首选材料，在5G无线通信、微纳/集成光子学和人工智能等前沿领域具有巨大应用价值。然而，铌酸锂晶体硬度低、脆性大、各向异性强，大尺寸高品质晶体的制备方法及其高效高质低/无损伤的超精密加工技术是实现铌酸锂晶体器件广泛应用的重要瓶颈。本文主要介绍超精密加工铌酸锂晶体过程中表面/亚表面损伤的产生机理与演变规律，以及减薄、研磨、抛光、超构表面制备等方面的研究进展。分析铌酸锂加工过程中易出现划痕、裂纹和磨料嵌入的原因，以及目前常用铌酸锂晶体超精密加工方法的特点及局限性，提出未来实现大尺寸铌酸锂高效率高表面质量加工的新技术。研究表明：离子切片和磨削能有效实现铌酸锂晶体减薄，研磨和化学机械抛光是常用的铌酸锂晶体表面超精密加工技术，刻蚀、激光烧蚀、聚焦离子束等技术是制备高质量铌酸锂超构表面的微纳加工技术。同时，高剪低压磨削、磁性剪切增稠抛光等新技术在实现铌酸锂晶体表面高效高质加工方面具有极大潜力，但铌酸锂晶体材料去除机理、弹-塑-脆加工临界条件和表面质量控制等问题还亟待系统研究。
- 铌酸锂 /
- 超精密加工 /
- 表面/亚表面损伤 /
- 高剪低压磨削 /
- 化学机械抛光 /
- 磁性剪切增稠抛光
Abstract: Significance: The fabrication of high-performance optoelectronic devices requires substrate materials with exceptional optoelectronic properties, robust mechanical stability, and broad application versatility. These substrates are crucial for advancing the information technology sector and driving economic growth. Lithium niobate (LiNbO₃) crystal has the advantages in piezoelectric, electro-optic, nonlinear optical, and photorefractive effects, and exhibits superior thermal stability, chemical resilience, and tenability, making it an ideal substrate for the development of optoelectronic components such as optical modulators, frequency doublers, and optical filters. The LiNbO₃ crystal is quite promising for application in cutting-edge technologies, such as 5G communication systems, micro/nano-integrated photonics, and artificial intelligence. Achieving an ultra-smooth, low/no-damage crystal surface is paramount for LiNbO₃-based optoelectronic devices. Any imperfections, such as scratches, cracks, or embedded abrasives, can lead to scattering, absorption, or diffraction of optical signals, adversely affecting device performance. However, the challenges posed by LiNbO₃’s intrinsic properties—namely, its relatively low hardness, high brittleness, and significant anisotropy—complicate the precise surface processing. High-efficiency, high-quality, and low/no-damage ultra-precision machining technology for large-sized high-quality crystals is a critical bottleneck in enabling the widespread application of LiNbO₃ crystal devices. Progress: Thinning, lapping, and polishing are essential for LiNbO₃ crystals to meet industrial application requirements for high-performance optoelectronic devices. The stability and reliability of optoelectronic devices are significantly influenced by the generation and evolution of surface and subsurface damages. The hardness, fracture toughness, Young's modulus, and other material properties of LiNbO₃ along different crystallographic orientations are investigated using methods such as nanoindentation and scratch tests. The surface damage patterns of various planes are analyzed. The material removal behaviors under different parameters are revealed. Ion slicing and grinding are two critical processes for thinning LiNbO₃ crystals. Ion slicing, which relies on ion implantation and wafer bonding, enables the precise thinning of crystals. Currently, it is possible to produce high-quality LiNbO₃ films with thicknesses varying from several hundred nanometers to a few micrometers. Grinding utilizes the mechanical behavior of abrasives to rapidly remove material from the LiNbO₃ crystal. A crystal substrate with a thickness of 80 μm is prepared effectively by optimizing the grinding parameters. Free-abrasive lapping has a wide range of applicability. However, lapping for LiNbO₃can easily lead to surface damage and abrasive embedding. During fixed abrasive lapping, abrasive embedding is effectively prevented, and surface and subsurface damage are reduced. It also exhibits notable advantages for continuous batch grinding. Chemical mechanical polishing is a widely adopted final polishing method that effectively reduces damage from previous processes, achieving a surface roughness (R_a) of less than 1 nm. With advancements in grinding and chemical mechanical polishing, techniques such as photolithography, etching, and femtosecond laser ablation have been employed to fabricate LiNbO₃ crystal metasurfaces, facilitating the development and application of multifunctional and ultra-compact integrated optoelectronic devices. Additionally, innovative methods, such as optimizing polishing slurry compositions with nanomaterial additives and adaptive shearing-gradient thickening polishing, have enabled ultra-precision processing, achieving ultra-smooth and low/no-damage results. High-shear and low-pressure grinding and magnetorheological shear thickening polishing under the coupling of magnetic, stress, and flow fields hold significant promise for the ultra-precision polishing of LiNbO₃ crystals. Conclusions and Prospects: As critical functional materials in advanced applications, such as 5G wireless communication, integrated/micro-nanophotonics, and big-data processing, LiNbO₃ crystals have garnered significant attention for their potential in ultra-precision machining technologies. Research shows that the development and evolution of surface/subsurface damage have been examined using methods such as nano-indentation and scratch testing. Ion slicing and grinding are effective techniques for thinning lithium niobate crystals. Lapping and chemical mechanical polishing are commonly used techniques to achieve ultra-precision machining. Furthermore, high-quality LiNbO₃ metasurfaces can be generated using micro-nano manufacturing methods such as femtosecond laser ablation, etching, and photolithography. New technologies, such as high-shear and low-pressure grinding and magnetorheological shear thickening polishing, are the most promising methods for achieving ultra-precision machining of LiNbO₃ crystals. Considering the complex interplay between material properties, processing parameters, and underlying mechanisms, the ongoing exploration of new ultra-precision machining techniques and process optimizations for LiNbO₃ crystals is critical. Such advancements are essential for enhancing machining efficiency, improving surface quality, and minimizing damage. However, future work, including the material removal mechanism of LiNbO₃ crystals, the critical machining conditions of elastic-plastic-brittle transition, and surface/subsurface quality control, needs to be systematically studied to provide theoretical and technical guidance for the ultra-precision machining of LiNbO₃ crystals. Given the fundamental challenges and technological implications, the ultra-precision machining of LiNbO₃ crystals is expected to remain a focal point of research for the foreseeable future, warranting continued investigation and development in this field.
- lithium niobate /
- ultra-precision machining /
- surface/subsurface damage /
- high-shear and low-pressure grinding /
- chemical mechanical polishing /
- magnetorheological shear thickening polishing

HTML全文

图 1 铌酸锂晶体的应用^[1-3]

Figure 1. Applications of lithium niobate crystals^[1-3]

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图 2 铌酸锂晶体结构示意图^[6]

Figure 2. Schematic diagram of lithium niobate crystal structure^[6]

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图 3 铌酸锂晶体中铌和锂的位置^[10]

Figure 3. Location of niobium and lithium in lithium niobate crystal^[10]

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图 4 铌酸锂晶体在8000 μN载荷下形成的压痕^[12]

Figure 4. Indentation of lithium niobate under a load of 8000 μN^[12]

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图 5 铌酸锂晶体不同切向的载荷-位移数据及残余压痕^[13]

Figure 5. Load-displacement data and residual impression after unloading^[13]

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图 6 球形压痕工具(R=4.5 μm)下压痕深度为2 μm时铌酸锂表面代表性SEM图^[15]

Figure 6. Representative SEM images after spherical indentation(R = 4.5 μm) on lithium niobate with a depth of 2 μm^[15]

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图 7 LN128和LN0的代表性断裂模式^[16]

Figure 7. Representative fracture patterns of LN128和LN0^[16]

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图 8 高载荷作用下铌酸锂表面^[17]

Figure 8. Lithium niobate surfaces under high loads^[17]

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图 9 铌酸锂表面划痕图^[18]

Figure 9. Surface scratches of lithium niobate^[18]

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图 10 断裂后铌酸锂样品示意图^[19]

Figure 10. Schematic diagram of fractured lithium niobate sample^[19]

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图 11 铌酸锂晶体截面扫描电镜图^[19]

Figure 11. Cross-section SEM image of lithium niobate crystal^[19]

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图 12 3.3 J/cm²、512脉冲烧蚀后X切铌酸锂的表面形貌^[22]

Figure 12. X-cut lithium niobate surface after ablation of 3.3 J/cm², 512 pulses^[22]

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图 13 不同离子速度和电子能量下30 MeV 氯离子和氩离子辐照试样透射电镜图^[24]

Figure 13. TEM images of lithium niobate samples irradiated with 30 MeV Cl ion and Ar ion with different ion velocities and electronic energy losses^[24]

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图 14 不同切削方向的凹槽^[26]

Figure 14. Notch images for different cutting directions^[26]

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图 15 塑性和脆性加工铌酸锂表面形貌图^[25]

Figure 15. Topography of ductile and brittle mode machined lithium niobate surface^[25]

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图 16 铌酸锂离子切片典型流程^[28]

Figure 16. Typical process for lithium niobate ion-cut^[28]

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图 17 铌酸锂薄膜制备工艺^[29]

Figure 17. Fabrication process of lithium niobate thin film^[29]

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图 18 铌酸锂键合界面透射电镜图^[29]

Figure 18. TEM images of LiNbO₃ bonding interface^[29]

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图 19 铌酸锂/硅杂化晶圆的制备工艺流程^[30]

Figure 19. Fabrication processes of LiNbO₃/Si hybrid wafers^[30]

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图 20 原子力显微镜图^[32]

Figure 20. AFM images^[32]

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图 21 截面扫描电镜图^[32]

Figure 21. Cross-section SEM images^[32]

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图 22 集成在Si上的铌酸锂薄膜扫描电镜图^[33]

Figure 22. SEM image of LiNbO₃ single-crystal thin film integrated on Si^[33]

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图 23 卧式减薄磨削示意图^[34]

Figure 23. Schematic diagram of horizontal thinning via grinding^[34]

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图 24 #1000杯型砂轮磨削后铌酸锂晶片不同位置的表面形貌^[34]

Figure 24. Surface morphology of lithium niobate wafers at different locations after grinding with #1000 cup wheel^[34]

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图 25 不同温度磨削后的铌酸锂晶体表面形貌图^[35]

Figure 25. Surface morphology of lithium niobate crystals after grinding at different temperatures^[35]

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图 26 外置正电场的铌酸锂晶体表面形貌图^[35]

Figure 26. Surface morphology of lithium niobate crystals with applied positive electric field^[35]

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图 27 外置负电场的铌酸锂晶体表面形貌图^[35]

Figure 27. Surface morphology of lithium niobate crystals with applied negative electric field^[35]

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图 28 不同磨削温度磨削后的铌酸锂晶片表面形貌图^[37]

Figure 28. Surface morphology of lithium niobate crystals after grinding at different temperatures^[37]

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图 29 不同电场强度磨削后的铌酸锂晶片表面形貌图^[37]

Figure 29. Surface morphology of lithium niobate crystals after grinding at different electric field strengths^[37]

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图 30 不同载荷研磨后的铌酸锂表面形貌^[17]

Figure 30. Surface morphology of lithium niobate after lapping under different loads^[17]

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图 31 不同粒径磨料研磨后铌酸锂的损伤层^[39]

Figure 31. Deformed layer of lithium niobate after lapping at different abrasive grain sizes^[39]

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图 32 游离磨料和固结磨料研磨后铌酸锂表面形貌(W28)^[40]

Figure 32. Surface morphology of lithium niobate after lapping with loose and fixed abrasives (W28)^[40]

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图 33 部分试样表面微观结构^[41]

Figure 33. Surface morphology of some lapped samples^[41]

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图 34 游离磨料和固结磨料研磨后铌酸锂晶体的表面形貌^[42]

Figure 34. Surface morphology of lithium niobate after lapping with fixed and loose abrasives^[42]

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图 35 不同基体研磨后铌酸锂的表面形貌^[43]

Figure 35. Surface morphology of lithium niobate after lapping using different matrices^[43]

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图 36 2种不同磨料形式研磨后铌酸锂的表面形貌^[43]

Figure 36. Surface morphology of lithium niobate after lapping with two types of abrasives^[43]

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图 37 X切和Z切铌酸锂研磨后的表面粗糙度和表面形貌^[19]

Figure 37. Surface roughness and surface morphology of X-cut and Z-cut lithium niobate after grinding^[19]

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图 38 不同pH值抛光后铌酸锂晶体的表面形貌^[55]

Figure 38. Surface morphology of lithium niobate crystals after polishing at different pH values^[55]

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图 39 化学机械抛光过程中的铌酸锂表面形貌^[56]

Figure 39. Surface morphology of lithium niobate during chemical mechanical polishing^[56]

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图 40 化学机械抛光前后铌酸锂晶体的表面形貌图^[57]

Figure 40. Surface morphology of lithium niobate crystals before and after chemical mechanical polishing^[57]

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图 41 超声波精细雾化化学机械抛光工作原理图^[58]

Figure 41. Operating principle of ultrasonic fine atomization chemical mechanical polishing^[58]

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图 42 刻蚀结构的扫描电镜图^[64]

Figure 42. SEM images of etched microstructures^[64]

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图 43 不同剂量离子束刻蚀后的铌酸锂表面^[66]

Figure 43. Lithium niobate surface after ion beam etching with different doses^[66]

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图 44 无磨料抛光装置示意图^[68]

Figure 44. Device schematic diagram of non-abrasive polishing ^[68]

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图 45 抛光前后铌酸锂表面形貌图^[68]

Figure 45. Surface morphology of lithium niobate before and after polishing^[68]

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图 46 抛光后铌酸锂的表面形貌^[69]

Figure 46. Surface morphology of polished lithium niobate^[69]

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图 47 新型抛光液性能验证的案例设计与实验结果^[69]

Figure 47. Case design and experimental results of performance verification of new polishing solution^69]

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图 48 选定参数加工后的工件形貌^[70]

Figure 48. Morphology of the workpiece with selected polishing parameters^[70]

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图 49 表面形貌的扫描电镜图以及对应位置的截面透射电镜图^[71]

Figure 49. SEM images of surface topography and cross-sectional TEM images of corresponding positions^[71]

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图 50 自适应剪切梯度增稠抛光前后的表面完整性^[71]

Figure 50. Surface integrity before and after adaptive shearing-gradient thickening polishing^[71]

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图 51 剪切增稠化学抛光过程中铌酸锂表面形貌和表面粗糙度变化^[72]

Figure 51. Evolution of surface topography and surface roughness before and after shear thickening-chemical polishing^[72]

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图 52 剪切增稠化学抛光过程中铌酸锂表面完整性分析^[72]

Figure 52. Surface integrity analyzed during shear thickening-chemical polishing^[72]

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图 53 高剪低压磨削原理图^[74]

Figure 53. Microscopic diagram of high-shear and low-pressure grinding principle^[74]

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图 54 高剪低压磨削前后铌酸锂晶体的宏观对比图

Figure 54. Macroscopic comparison of lithium niobate crystals before and after high-shear and low-pressure grinding

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图 55 磁性剪切增稠抛光原理^[79]

Figure 55. Magnetorheological shear thickening polishing^[79]

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图 56 磁性剪切增稠抛光前后铌酸锂表面三维形貌图

Figure 56. Three-dimensional morphology of lithium niobate surface before and after magnetorheological shear thickening polishing

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表 1 铌酸锂晶体的基本物理化学参数(20 ℃)^[11]

Table 1. Basic physical and chemical properties of lithium niobate crystals (20 °C) ^[11]

基本性质	实验数值
晶体密度 ρ / (g·cm⁻³）	4.612
莫氏硬度 H_m	5
熔点 T_m / ℃	1260
居里温度 T_c / ℃	1210
菱形晶胞参数 a_l / Å	5.4920
菱形晶胞参数 α₁	55°53′
六角晶胞参数 a₂ / Å	5.14829 ± 0.00002
六角晶胞参数 c₂ / Å	13.86310 ± 0.00004
菱形晶胞分子数 N_l	2
六角晶胞分子数 N₂	6
a轴热膨胀系数 λ_a / ℃^－1	16.7 × 10⁻⁶
c轴热膨胀系数 λ_c / ℃^－1	2.0 × 10⁻⁶
介电常数	ε^s₁₁=44, ε^t₁₁=84, ε^s₃₃=29, ε^t₃₃=30
折射率 n (632.8 nm)	n_o=2.286, n_e=2.202
25 ℃水溶解度 S / (mol·L⁻¹)	2.8 × 10⁻⁴
分解热 ΔH / ( J·mol⁻¹)	25941.42

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表 2 铌酸锂晶体的系列化学机械抛光实验

Table 2. A series of chemical mechanical polishing experiments on lithium niobate crystals

序号	磨料	粒径 d / nm	pH	载荷 F / kPa	转速 v / (r·min⁻¹)	流量 q / (mL·min⁻¹)	时间 t / min	效果
1^[46]	SiO₂	25	9.5	6.5	100	200	—	无划痕和缺陷
2^[47]	SiO₂	20～40	9.5～10	—	15	10	360	R_a 0.387 nm 面型误差<4 μm
3^[48]	SiO₂	50	9.5～10	170	40	3	60	R_a0.32 nm，表面平整光滑
4^[49]	SiO₂	—	11.26	140	60	120	—	R_a 0.21 nm
5^[50]	SiO₂	—	—	140	60	120	—	300 nm/min R_a 0.21 nm
6^[51]	SiO₂	50	9.5～10	17	40	3	60	R_a 0.20 nm
7^[52]	—	—	10.8	90	50	—	180	R_a 1.0 nm
8^[53]	SiO₂	20	11	140	60	180	—	350 nm/min
9^[54]	SiO₂	40	9.0～11.5	60	60	50	5	R_a 0.38 nm
10^[55]	—	—	10	160	60	3000	—	R_a 0.196 nm

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