High efficient oxygen reduction performance of Fe/Fe3C nanoparticles in situ encapsulated in nitrogen-doped carbon via a novel microwave-assisted carbon bath method

Fe-based carbon materials are widely considered promising to replace Pt/C as next-generation electrocatalysts towards oxygen reduction reaction (ORR). However, the preparation of Fe-based carbon materials is still carried out by conventional heating method (CHM). Herein, a novel microwave-assisted carbon bath method (MW-CBM) was proposed, which only took 35 min to synthesize Fe/Fe3C nanoparticles encapsulated in N-doped carbon layers derived from Prussian blue (PB). The catalyst contained large specific surface area and mesoporous structure, abundant Fe-Nx and C–N active sites, unique core-shell structure. Due to the synergistic effects of these features, the as-prepared Fe/Fe3C@NC-2 displayed outstanding ORR activity with onset potential of 0.98 VRHE and halfwave potential of 0.87 VRHE, which were more positive than 20 wt.% Pt/C (0.93 VRHE and 0.82 VRHE). Besides, Fe/Fe3C@NC-2 gave a better stability and methanol tolerance than Pt/C towards ORR in alkaline media, too.

Overwhelming electrochemical oxygen reduction reaction of zinc-nitrogen-carbon from biomass resource chitosan via a facile carbon bath method

Developing high efficiency and low cost electrocatalysts is critical for the enhancement of oxygen reduction reaction(ORR),which is the fundamental for the development and commercialization of renewable energy conversion technology.Herein,zinc-nitrogen-carbon(Zn-N-C)was prepared by using biomass resource chitosan via a facile carbon bath method.The obtained Zn-N-C delivered a high specific surface area(794.7 cm^2/g)together with pore volume(0.49 cm^3/g).During the electrochemical evaluation of oxygen reduction reaction(ORR),Zn-N-C displayed high activity for ORR with an onset pote ntial E0=0.96 VRHE and a half wave potential E1/2=0.86 VRHE,which were more positive than those of the comme rcial 20 wt%Pt/C benchmark catalyst(E0=0.96 VRHE and E1/2=0.81 VRHE).In addition,the ZnN-C catalyst also had a better stability and methanol tolerance than those of the Pt/C catalyst.

蒸汽浴-流动分析仪法测定土壤有机碳含量的方法

为了准确高效批量测定土壤有机碳含量,采用比色管代替消煮管,蒸汽加热消煮土壤,利用流动分析仪法测定有机碳。并将此方法与重铬酸钾氧化-外加热法(常规通用)进行了比较,探讨方法的可行性。结果表明,蒸汽浴-流动分析仪法测定土壤有机碳含量重复性试验的相对标准偏差为3.19%~9.41%,回收率为92.21%~97.63%。方法精密度及准确性良好。所测结果与重铬酸钾氧化-外加热法无显著性差异(P>0.05),两种方法拟合的回归方程:y(蒸汽浴-流动分析仪法)=0.947x(重铬酸钾氧化-外加热法)+1.621(r^(2)=0.933),两者呈良好的相关性。用两种方法测定200个土壤有机碳,蒸汽浴-流动分析仪法的检测用时是重铬酸钾氧化-外加热法用时的68%,人工操作用时是重铬酸钾氧化-外加热法用时的44%,蒸汽浴-流动分析仪法无需使用硫酸亚铁,重铬酸钾、硫酸和水用量为重铬酸钾氧化-外加热法的40%。蒸汽浴-流动分析仪法省工省时,人员工作强度低,试剂用量少,环境危害降低,检测准确高效,经济安全,可推荐为大批量土壤有机碳含量测定的方法。

简便的碳浴法制备N,S共掺杂类石墨烯炭提高氧还原反应性能

合理设计和优化氧还原反应(ORR)非金属电催化剂对于燃料电池和金属空气电池非常重要。然而,这现在仍然是一个巨大的挑战。本工作通过简单的碳浴法成功制备了N,S共掺杂的类石墨烯炭材料(GLC),并将其用于电催化氧还原反应。经高温热解和模板分解后,得到的GLC-11具有较高的比表面积(583.68 cm^2/g)和孔体积(0.63 cm^3/g)。其中,微孔表面积占总表面积的29.39%,微孔体积占总孔体积的12.70%。同时,通过XPS结果计算得到,GLC-11的吡啶氮和石墨氮含量总和高达92.2%。因此,GLC-11在碱性电解液中显示出了高电催化ORR性能,其中波电位(E1/2)为0.82 VRHE,优于Pt/C(E 1/2=0.80 VRHE)。此外,GLC-11催化剂与商业Pt/C(20 wt%)催化剂相比表现出更好的稳定性和优异的甲醇耐受性。

氮掺杂碳原位锚定铜纳米颗粒用于高效氧还原反应催化剂

与贵金属铂基电化学氧还原反应(ORR)催化剂相比,廉价的非贵金属催化剂引起了广泛的关注。本文以壳聚糖作为一种富含氮和碳元素的生物质资源,利用碳浴法成功制备了氮掺杂碳原位负载铜纳米颗粒(Cu/N-C)催化剂。纯壳聚糖碳化得到的样品N-C的比表面积为67.5 m^(2)·g^(-1)、平均孔径0.14 nm、平均孔体积8.00 m^(2)·g^(-1),与之相比,Cu/N-C比表面积可达607.3 m^(2)·g^(-1)、平均孔径为2.5 nm、平均孔体积为0.40 cm^(3)·g^(-1)。通过密度泛函理论(DFT)进行计算表明,Cu(111)/N-C的自由能值低于N-C,更有利于氧还原催化进行。在0.1 mol·L^(-1) KOH的介质中,Cu/N-C不仅表现出优异的起始和半波电势(分别为0.96 V和0.84 V),而且还表现出了优异的抗甲醇性能和稳定性,并且Cu元素掺杂量达到1.67wt.%。

重铬酸钾-烘箱加热法测定土壤有机碳研究

重铬酸钾氧化法测定土壤有机质含量(HJ615—2011)时利用油浴加热消解有机物,本文针对油浴加热具有易发生溢油以及附着在消解管壁上的油污难以清洗等缺点,研究了在烘箱常用温度下用烘箱加热代替油浴加热的可能性。研究结果表明,135℃下(该温度在烘箱常用温度范围内,且与HJ615—2011中的油浴加热温度一致)利用烘箱加热时重铬酸钾氧化法的相对标准偏差为0.294%～1.593%,加标回收率为99%～103%,而用油浴加热时的相对标准偏差为0.386%～1.945%,加标回收率为96%～105%,使用烘箱加热提高了重铬酸钾氧化法的精确度和准确度,在HJ615—2011土壤有机碳测定方法中,采用烘箱加热较传统的油浴加热测定有机碳更适宜。

沙浴消解法测定水中总铬

对高锰酸钾氧化—二苯碳酰二肼分光光度法测定总铬中的氧化过程进行改进,采用沙浴加热氧化,即于50mL比色管中取样加入0.5mL(1+1)硫酸、0.5mL(1+1)磷酸、2滴4%高锰酸钾氧化剂,于沙浴中加热氧化、冷却、定容、显色、比色测定。结果表明,此方法操作简便,耗时较短,测定结果准确度、精密度高,有一定可行性。