北京化工大学 化学工程学院， 北京 100029
李彬彬， 曹峻豪， 陈孟达， 等. 复合法制备石墨烯纳米片［J］. 中国粉体技术， 2026， 32（1）： 1-13.
LI Binbin， CAO Junhao， CHEN Mengda， et al. Preparation of graphene nanosheets by composite method［J］. China Powder Science and Technology， 2026， 32（1）： 1−13.
DOI：10.13732/j.issn.1008-5548.2026.01.008
收稿日期：2025-04-18，修回日期：2025-05-30，上线日期：2025-07-12。
基金项目：国家自然科学基金项目，编号 ：22478026。
第一作者简介：李彬彬（2000—），男，硕士生，研究方向为石墨烯制备与石墨提纯技术开发。E-mail：libinbin3866@163. com。
通信作者简介：毋伟（1966—），男，教授，博士，博士生导师，研究方向为化工新型材料的制备及应用。E-mail：wuwei@mail. buct. edu. cn。
摘要：【目的】 针对石墨烯制备过程面临的污染多、成本高、工业化难度大等问题，寻找一种绿色节能、易工业化的高效
石墨烯制备方法。【方法】 采用球磨剥离的方式，在水相体系中制备石墨烯纳米片；采用单因素变量法探讨工艺条件对石
墨烯纳米片产量的影响，并以高温煅烧法研究此工艺中的表面活性剂去除方式。【结果】 在较优的工艺条件下，可生产固
含物质量浓度为2. 42 g/L的石墨烯纳米片分散液，约有数量分数为70%的石墨烯纳米片粒径为400~800 nm，较优工艺生
产的产品层数为 5~12，Raman光谱的 D峰强度（ID）与 G峰强度（IG）之比为 0.318，缺陷较少；在氮气氛围下 400 ℃煅烧 30
min可去除产品中的大部分表面活性剂，950 ℃时煅烧可更彻底地去除表面活性剂，此温度处理后的石墨烯纳米片电导
率可达1. 3×104 S/m。【结论】建立一种绿色环保、易工业化的高效石墨烯纳米片制备工艺，并提供一种表面活性剂的去除
方式，大幅提升工艺产品的电导率，拓宽应用领域。
关键词：液相剥离； 球磨法； 石墨烯纳米片； 表面活性剂
Objective Graphene， renowned for its excellent mechanical， thermal， and electrical properties， enables extensive applications
across various fields. However， its industrial-scale production remains constrained by significant challenges such as severe environmental pollution， substantial production costs， and limited scalability. To address these issues， the study develops a green， efficient， and scalable method for graphene nanosheet （GN） fabrication， while also providing an effective surfactant removal
strategy to enhance their applicability.
Methods GNs were synthesized through a combined ball milling pretreatment and surfactant-assisted aqueous-phase ball milling process. Key parameters， such as surfactant dosage， initial graphite concentration， ball milling time， and ball-to-material
ratio， were optimized through univariate analysis with the mass concentration of GNs as the evaluation metric. In addition， the
morphological and structural characterization of the resulting GNs were conducted， and the surfactant removal efficiency through
calcination was systematically investigated.
Results and Discussion Experimental studies showed that the optimal processing parameters were determined as follows： 3%
surfactant mass fraction， 120 mg/mL initial graphite mass concentration， 4 h ball milling time， and 12∶1 ball-to-material ratio.
Under these conditions， the resulting GNs were produced at a maximum solution concentration of 2. 42 mg/mL. Microscopic
characterization results， including scanning electron microscopy（ SEM）， transmission electron microscopy（ TEM）， and atomic
force microscopy（ AFM）， showed that about 70% of the GNs had lateral sizes between 400 nm and 800 nm and consisted of 5 to
12 layers. Raman spectroscopic analysis confirmed their high structural integrity， as evidenced by the low defect-related ID/IG ratio（ the ratio of peak intensity D to peak intensity G ） of 0. 318. In addition， calcination at 400 ℃ for 30 min under a nitrogen atmosphere effectively removed most of the surfactants， while moderately improving the conductivity of the resulting GNs. A
higher calcination temperature of 950 ℃ achieved complete surfactant removal， significantly enhancing conductivity of up to
1. 3×104 S/m.
Conclusion This study demonstrates a green， efficient， and scalable aqueous-phase exfoliation method for producing highquality
and low-defect GNs. The combined ball milling approach offers a novel idea for graphene production and holds promise
for large-scale graphene preparation. Additionally， the developed calcination-based surfactant removal method further enhances
conductivity， enabling flexible application-specific optimization. This work provides a promising pathway toward sustainable， large-scale graphene manufacturing.
Keywords：aqueous-phase exfoliation； ball milling method； graphene nanosheets； surfactant removal
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