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首页> 外文期刊>RSC Advances >Anaerobic vs. aerobic preparation of silicon nanoparticles by stirred media milling. The effects of dioxygen, milling solvent, and milling time on particle size, surface area, crystallinity, surface/near-surface composition, and reactivity
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Anaerobic vs. aerobic preparation of silicon nanoparticles by stirred media milling. The effects of dioxygen, milling solvent, and milling time on particle size, surface area, crystallinity, surface/near-surface composition, and reactivity

机译：搅拌介质研磨的厌氧对硅纳米粒子的有氧含量。二恶英，研磨溶剂和研磨时间对粒径，表面积，结晶度，表面/近表面组成和反应性的影响

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A stirred media mill was hermetically sealed in a high-purity dinitrogen atmosphere glovebox and used to prepare silicon nanoparticles (SiNPs) by milling a slurry of 45–90 μm pieces of metallurgical-grade silicon (MGS) suspended in anhydrous heptane (HEP), heptane containing a small amount of mesitylene (HEP/MES), or mesitylene containing 22 mM pyrene (MES/PYR) under anaerobic and anhydrous conditions (≤5 ppm dioxygen (O _(2) ) and water (H _(2) O) vapor). Excess solvent and other volatiles were removed using a rotary evaporator also housed in the glovebox. The SiNPs were further dried at 22 ± 1 °C under vacuum (≤1 × 10 ~(?5) Torr) for at least 15 h. The dark-brown or black pyrophoric nanoparticle powders were stored in a high-purity argon atmosphere glovebox. Samples were removed from the glovebox and analyzed by BET surface area (BET-SA) determination, tensimetric titrations with various pressures of O _(2) , PXRD, SEM, TEM, ATR-FTIR, and/or XPS. The effects of (i) anaerobic vs. aerobic milling, (ii) milling fluid, and (iii) milling time on BET-SA, degree of crystallinity, reactivity with O _(2) , and FTIR- or XPS-determined surface/near-surface composition of the SiNPs are discussed. The BET-SA of SiNPs milled anaerobically for 5 h in MES/PYR (258 m ~(2) g ~(?1) ) was ca. twice as large as the BET-SA for SiNPs milled aerobically in the same milling fluid. In contrast, the BET-SA of SiNPs milled anaerobically in HEP (40 m ~(2) g ~(?1) ) was four times smaller than for SiNPs milled aerobically in HEP. The PXRD-determined degree of crystallinity steadily decreased and the BET-SA steadily increased over time (1, 2, or 5 h) for SiNPs milled anaerobically in MES/PYR. The degree of crystallinity of SiNPs milled anaerobically in HEP also steadily decreased over time, but the BET-SAs for 1, 2, 3, 4, and 5 h milled samples were essentially the same. MES/PYR milled SiNPs reacted more slowly with O _(2) and irreversibly absorbed less O _(2) than HEP milled SiNPs.
机译：将搅拌的介质研磨机密封在高纯度的二氮气氛手套箱中并用来通过研磨45-90μm冶金级硅（Mgs）的浆料制备硅纳米颗粒（SINP），悬浮在无水庚烷（HEP）中，在厌氧和无水条件下含有少量乙烯（HEP / MES）或含有22mM芘（MES / PYR）的叶片（MES / PYR）（≤5ppm二氧（O _（2））和水（H _（2）o） ）蒸气）。使用旋转蒸发器除去过量的溶剂和其他挥发物，该旋转蒸发器也容纳在手套箱中。在真空（≤1×10〜（α5）托上的真空下，在22±1℃下进一步干燥SINPS至少15小时。深褐色或黑色荧光纳米粒子粉末储存在高纯度氩气氛手套箱中。从手套箱中除去样品并通过BET表面积（Bet-SA）测定，滴定滴定，具有O _（2），PXRD，SEM，TEM，ATR-FTIR和/或XPS的各种压力的滴定滴定分析。 （i）厌氧与有氧铣削，（ii）铣削液，（iii）铣削时间对Bet-sa，结晶度，与O _（2）的反应性的影响，以及FTIR-或XPS确定的表面的效果/讨论SINPS的近表面组成。 Sinps的Bet-Sa在MES / PYR中占据了5小时（258 m〜（2）g〜（？1））。在同一铣削液中磨削的SINPS磨削的两倍。相比之下，辛普斯的Bet-SA在HEP中突然碾碎（40m〜（2）g〜（α1））小于肝脏均匀磨削的SINPS的四倍。在MES / PYR中，PXRD确定的结晶度稳定地降低，并且稳定地增加了SINPS的时间（1,2，或5小时），以便在MES / PYR中研磨。随着时间的推移，SINPS的结晶度突出的SINPS的结晶度也稳定地降低，但是1,2,3,4和5h碾磨样品的BET-SAS基本相同。 MES / PYR MICRED SINPS与O _（2）更慢地反应，并且不可逆转地吸收较少的O _（2），而不是HEP磨削的SINPS。

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