目的 为解决传统陶瓷砂轮活性金属氧化失效问题,旨在开发一种兼具防氧化与界面强化功能的金刚石衬底机械化学抛光陶瓷砂轮。方法 研究采用硅包铁粉末,利用外层硅隔绝氧气保护内层Fe活性,在常压烧结条件下同步实现砂轮基体防氧化及磨粒与基体界面强化;通过扫描电镜观察微观结构、抗弯实验测试强度,并借助磨削实验结合表面粗糙度、材料去除率、拉曼表征优化配方,探究不同加工转速和进给下的最佳参数,利用TEM观测亚表面损伤、结合XPS分析材料去除机制。结果 实验结果显示,该方法制备的砂轮可有效防氧化并提升结构强度,优化后单晶金刚石(100)面材料去除率达10.69 μm/h,表面粗糙度Sa=0.82 nm,亚表面非晶碳层仅1.913 nm,拉曼及XPS光谱证实材料去除源于砂轮中铁活性组分催化金刚石表面非晶碳化形成Fe3C层,结合硬质磨料机械磨削实现。结论 硅包铁梯度氧化结构陶瓷砂轮成功实现常压烧结下的界面强化与氧化防护,其机械-化学协同去除机制显著提升了单晶金刚石加工效率与表面质量,为金刚石衬底高效低损伤加工提供了新方案,在金刚石基电子器件制造领域具有良好的产业化应用前景。
Abstract
Ceramic grinding wheels containing transition metals exhibit significant advantages over traditional wheels when processing diamonds. However, during sintering and processing, transition metals are prone to oxidation, particularly in high-temperature and high-humidity environments. To address the issue of oxidation-induced failure in ceramic grinding wheels containing transition metals, the work aims to develop a diamond ceramic grinding wheel that integrates both antioxidant and interface reinforcement functions. By coating iron with silicon, the wheel effectively isolates oxygen, protecting the active iron layer and achieving oxidation protection for the wheel matrix and interface reinforcement between the abrasive grains and matrix under conventional sintering conditions (air, ambient pressure). In the study, scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to analyze the microstructure and composition of the silicon-coated iron powder. The results showed that after high-temperature sintering, the composition of the silicon-coated iron powder remained unchanged, confirming its excellent anti-oxidation properties. Subsequently, N68 vitrified binder powder, PMMA pore-forming agents, 2000# diamond abrasives, and silicon-coated iron powder were mixed in different ratios (silicon-coated iron powder: diamond powder = 1∶2, 1∶1, 2∶1), along with dextrin solution, sieved, cold-pressed, and sintered to produce wheel blocks. Comparative experiments were conducted to test the bending strength and block composition of traditional ceramic wheels containing transition metals and silicon-coated iron wheels with different powder ratios. The results showed that, under the same ratio, the silicon-coated iron ceramic wheel had higher strength and did not undergo oxidation after sintering, proving that the silicon-coated iron powder not only had strong anti-oxidation ability but also significantly enhanced the structural strength of the wheel. To further validate the effectiveness of the grinding wheel, grinding experiments were conducted with single-crystal diamond (7 mm×7 mm×0.3 mm) as the workpiece. The spindle speed was initially set to 1 250 r/min, and the feed rate was 0.2 μm/s for diamond processing. Surface roughness, material removal rate, and Raman spectral characteristics were used to screen and optimize the wheel formula. Based on this optimized formula, the effect of different spindle speeds (1 000, 1 250, 1 500, 1 750 r/min) and feed rates (0.1, 0.2, 0.3, 0.4 μm/s) on single-crystal diamond processing was investigated. The best processing conditions were determined through surface roughness, material removal rate, and Raman spectra, and the subsurface damage of the processed diamond was analyzed through X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM), revealing the material removal mechanisms. Experimental results indicated that the fabricated wheel not only demonstrated excellent anti-oxidation performance but also significantly improved structural strength. Under the optimized formula, the material removal rate for single-crystal diamond (100) reached 10.69 μm/h, the surface roughness (Sa) was 0.82 nm, and the thickness of the subsurface amorphous carbon layer was only 1.913 nm. Raman and XPS spectra confirmed that material removal occurred due to the catalytic effect of the iron active component in the grinding wheel, leading to the formation of Fe3C layer on the diamond surface. This process, combined with mechanical grinding by hard abrasives, effectively improved the surface quality of the material. The study demonstrates that, under normal sintering conditions, the silicon-coated iron gradient oxidation structure ceramic grinding wheel successfully achieves interface reinforcement and oxidation protection. The mechanical-chemical synergistic removal mechanism significantly improves the processing efficiency and surface quality of single-crystal diamonds, providing a new solution for efficient, low-damage processing of diamond substrates. This method shows great industrial application potential in the manufacturing of diamond-based electronic devices.
关键词
陶瓷砂轮 /
机械化学抛光 /
单晶金刚石 /
自旋转磨削
Key words
ceramic grinding wheel /
mechanical-chemical polishing /
single-crystal diamond /
self-rotating grinding
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参考文献
[1] 安康, 张永康, 刘鹏, 等. 预制应力提高大尺寸金刚石抛光成功率[J]. 表面技术, 2025, 54(6): 143-151.
AN K, ZHANG Y K, LIU P, et al.Prefabricated Stress for Improving Success Rate of Large-Size Diamond Polishing[J]. Surface Technology, 2025, 54(6): 143-151.
[2] XIN Y K, LU J, LI C, et al.Effects of Processing Parameters and Grinding Direction on the Material Removal Mechanism of (100) Surface Single Crystal Diamond in Self-Rotating Mechanical Grinding[J]. Diamond and Related Materials, 2024, 141: 110685.
[3] YUAN S, GUO X G, WANG H, et al.Atomistic Understanding of Rough Surface on the Interfacial Friction Behavior during the Chemical Mechanical Polishing Process of Diamond[J]. Friction, 2024, 12(6): 1119-1132.
[4] YUAN S, GUO X G, HUANG J X, et al.Insight into the Mechanism of Low Friction and Wear during the Chemical Mechanical Polishing Process of Diamond: A Reactive Molecular Dynamics Simulation[J]. Tribology International, 2020, 148: 106308.
[5] REN J, ZHANG K L, WANG F, et al.Investigation of Diamond Films Polished by Thermal Chemical Mechanical Polishing[J]. ECS Transactions, 2013, 52(1): 517-522.
[6] KATAMUNE Y, MURASAWA K, YOSHITAKE T, et al.Low-Volume-Loss Surface Polishing with a Krypton Fluoride Excimer Laser for Polycrystalline Diamond Films[J]. Applied Physics Letters, 2023, 123(3): 031604.
[7] LIU H G, XIE L R, LIN W X, et al.Optical Quality Laser Polishing of CVD Diamond by UV Pulsed Laser Irradiation[J]. Advanced Optical Materials, 2021, 9(21): 2100537.
[8] YU J R, LIU X Y, XU R B, et al.Single Crystal Diamond Polishing Assisted by Inductively Coupled Plasma Etching[J]. Diamond and Related Materials, 2025, 152: 111978.
[9] 焦硕沛, 张旭芳, 李明坤, 等. 金刚石等离子体刻蚀技术研究进展[J]. 表面技术, 2025, 54(7): 34-49.
JIAO S P, ZHANG X F, LI M K, et al.Research Progress on Diamond Plasma Etching Technique[J]. Surface Technology, 2025, 54(7): 34-49.
[10] LIU N, SUGAWARA K, YOSHITAKA N, et al.Damage-Free Highly Efficient Plasma-Assisted Polishing of a 20-mm Square Large Mosaic Single Crystal Diamond Substrate[J]. Scientific Reports, 2020, 10: 19432.
[11] SCHUELKE T, GROTJOHN T A.Diamond Polishing[J]. Diamond and Related Materials, 2013, 32: 17-26.
[12] XU H Q, ZANG J B, TIAN P F, et al.Rapid Grinding CVD Diamond Films Using Corundum Grinding Wheels Containing Iron[J]. International Journal of Refractory Metals and Hard Materials, 2018, 71: 147-152.
[13] XU H Q, ZANG J B, YANG G P, et al.An Efficient Titanium-Containing Corundum Wheel for Grinding CVD Diamond Films[J]. Diamond and Related Materials, 2018, 84: 119-126.
[14] ZENKIN S, GAYDAYCHUK A, OKHOTNIKOV V, et al.CVD Diamond Interaction with Fe at Elevated Temperatures[J]. Materials, 2018, 11(12): 2505.
[15] KU Y L, XU K, YAN L B, et al.Revealing the Atomic Mechanism of Diamond-Iron Interfacial Reaction[J]. Carbon Energy, 2024, 6(3): e440.
[16] 周仁宸, 王哲, 杨远航, 等. 超精密晶圆减薄砂轮及减薄磨削装备研究进展[J]. 表面技术, 2024, 53(3): 1-21.
ZHOU R C, WANG Z, YANG Y H, et al.Research Progress on Grinding Wheels and Equipment for Ultra Precision Wafer Thinning[J]. Surface Technology, 2024, 53(3): 1-21.
[17] AIDA H, OSHIMA R, MINAMIGATA H, et al.Mirror-Grinding of Single-Crystal Diamond Substrates with a Rotary Grinder[J]. Diamond and Related Materials, 2022, 121: 108733.
[18] DAHAL N, CHIKAN V.Phase-Controlled Synthesis of Iron Silicide (Fe3Si and FeSi2) Nanoparticles in Solution[J]. Chemistry of Materials, 2010, 22(9): 2892-2897.
[19] CHEUNG S H, SCHMIDT K, BARIBEAU J M, et al.A Re-Examination of Thin-Film Silicon’s Raman Spectrum[J]. Journal of Materials Science: Materials in Electronics, 2024, 35(13): 911.
[20] ZHENG Y T, YE H T, THORNTON R, et al.Subsurface Cleavage of Diamond after High-Speed Three-Dimensional Dynamic Friction Polishing[J]. Diamond and Related Materials, 2020, 101: 107600.
[21] YE S, ZHENG Y T, ZHAO S M, et al.Evolutionary Features of Subsurface Defects of Single Crystal Diamond after Dynamic Friction Polishing[J]. Functional Diamond, 2024, 4(1): 2316147.
[22] WANG X B, ZHANG P, GAO J J, et al.Facile Synthesis and Magnetic Properties of Fe3C/C Nanoparticles via a Sol-Gel Process[J]. Dyes and Pigments, 2015, 112: 305-310.
[23] 龚晓晔, 尤静林, 王建, 等. 几种铁氧化合物微观结构及其拉曼光谱研究[J]. 光谱学与光谱分析, 2018(S1): 241-242.
GONG X Y, YOU J L, WANG J, et al.Study on Microstructure and Raman Spectra of Several Iron Oxides[J]. Spectroscopy and Spectral Analysis, 2018(S1): 241-242.
[24] PAPROCKI K, DITTMAR-WITUSKI A, TRZCIŃSKI M, et al. The Comparative Studies of HF CVD Diamond Films by Raman and XPS Spectroscopies[J]. Optical Materials, 2019, 95: 109251.
[25] ZHIGACH A N, LEIPUNSKY I O, KUSKOV M L, et al.On the Production of Dispersive Single-Crystal Iron Carbide (Fe3C) Nanoparticulate[J]. Bulletin of Materials Science, 2022, 45(1): 38.
基金
厦门市重大科技专项(3502Z20231047); 华侨大学先进碳转化技术研究院开放研究基金