Reproducibility in the synthesis of nanomaterials is a crucial aspect for their real-life applications. It is particularly pertinent in the context of gold nanoparticles, where a plethora of seeded-growth methods are being developed to control particle morphology and size. The translation of such methods to manufacturing can be hindered by poor reproducibility of the seed production step. This study focuses on the development of a highly reproducible platform for the synthesis of gold nanoparticles, as potential substrates for glucose sensing. A flow reactor was designed, starting from a detailed study of the synthesis in batch. The well-established Turkevich synthesis was investigated via in situ time-resolved UV-vis spectroscopy. In order to enhance the reproducibility of the synthesis the effect of passivating the gold precursor stock before its use in the synthesis was investigated. It is shown that starting from a pre-passivated precursor provided improved control over the initial reaction stage, at the expense of a small increase in the reaction time. At the optimal reaction conditions, the proposed modified Turkevich method allowed for the synthesis in batch of ∼12 nm monodisperse (RSD ∼10%) particles, with a variability from batch to batch of only ∼5%. The information gathered from the batch study, in particular the reaction time, was used to translate the synthesis from batch to flow. The system utilized for the flow synthesis consisted of a segmented flow reactor, where an organic stream was employed to segment the reactive aqueous stream to avoid reactor fouling and improve monodispersity. The use of segmented flow enables treating each droplet as a “travelling batch”, hence allowing the direct use of the kinetic data obtained in batch to design the flow reactor, leading to the rapid identification of the minimum residence time to allow for reaction completion. The flow reactor enabled the synthesis of ∼11 nm monodisperse (RSD ∼10%) particles, with full precursor conversion and reproducibility between reactor runs higher than that obtained in batch (variability of ∼2%). The flow-produced gold nanoparticles were tested for glucose sensing, exploiting their glucose oxidase-mimicking behaviour and demonstrated satisfactory glucose detection in the range of 1–10 mM.

中文翻译：

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基于合理的反应器设计，利用还原的钝化Au（III）进行还原，可高产量，高产率地合成金纳米颗粒

纳米材料合成中的可再现性是其实际应用的关键方面。这在金纳米颗粒的情况下特别相关，在金纳米颗粒中，正在开发大量的种子生长方法来控制颗粒的形态和大小。种子生产步骤的可重复性差可能会阻碍这种方法向生产的转化。这项研究专注于开发高度可复制的平台，用于合成金纳米颗粒，作为葡萄糖传感的潜在底物。从分批合成的详细研究开始，设计了流动反应器。通过原位研究完善的Turkevich合成时间分辨紫外可见光谱。为了提高合成的可重复性，研究了在将金前体原料用于合成之前对其进行钝化的效果。已经表明，从预钝化的前体开始提供了对初始反应阶段的改进控制，但以反应时间的少量增加为代价。在最佳反应条件下，所提出的改进的Turkevich方法允许分批合成约12 nm单分散（RSD约10％）的颗粒，批次之间的变异性仅为约5％。从批次研究中收集的信息，特别是反应时间，被用于将合成过程从批次转化为流动。用于流动合成的系统由分段流动反应器组成，其中使用有机物流将反应性水性物流分段以避免反应器结垢并改善单分散性。分段流动的使用能够将每个液滴视为“移动批料”，因此可以直接使用分批获得的动力学数据来设计流动反应器，从而快速确定最小停留时间以允许反应完成。流动反应器能够合成约11 nm单分散（RSD约10％）的颗粒，反应器之间的完全前驱物转化率和重现性高于批量生产（约2％的变异性）。对流动产生的金纳米颗粒进行了葡萄糖感测测试，利用了它们的葡萄糖氧化酶模拟行为，并证明了其在1–10 mM范围内的令人满意的葡萄糖检测能力。