新型炭材料
新型炭材料
신형탄재료
NEW CARBON MATERIALS
2013年
6期
454-460
,共7页
陈胜洲%杨旸%陈伟平%李良伟%邹汉波
陳勝洲%楊旸%陳偉平%李良偉%鄒漢波
진성주%양양%진위평%리량위%추한파
氮掺杂炭气凝胶%氧还原%非贵金属
氮摻雜炭氣凝膠%氧還原%非貴金屬
담참잡탄기응효%양환원%비귀금속
Nitrogen doped carbon aerogels%Oxygen reduction reaction%Non-noble metal
以三聚氰胺、间苯二酚、甲醛为原料,采用溶胶-凝胶法、冷冻干燥等步骤制备出三聚氰胺-间苯二酚-甲醛( MR)干凝胶;并以所制炭气凝胶为载体浸渍硝酸钴,经氮气中高温炭化,得到钴复合氮掺杂的炭气凝胶。考察间苯二酚和三聚氰胺比例、凝胶pH值及炭化条件等对气凝胶结构和催化氧还原活性的影响,采用XRD、XPS、低温氮气吸脱附等方法研究催化剂的结构。随pH值增加,MR气凝胶的介孔分布向小孔移动;当M/R物质的量比为6:1时,其介孔分布为3.0~4.0 nm。钴复合炭气凝胶多孔结构中存在均匀分布Co金属颗粒和管状炭,Co金属颗粒粒径随炭化温度升高而增加。采用旋转圆盘电极研究催化剂在0.5 mol/L H2 SO4溶液中的电化学性能,结果表明催化剂具有良好的氧还原活性。
以三聚氰胺、間苯二酚、甲醛為原料,採用溶膠-凝膠法、冷凍榦燥等步驟製備齣三聚氰胺-間苯二酚-甲醛( MR)榦凝膠;併以所製炭氣凝膠為載體浸漬硝痠鈷,經氮氣中高溫炭化,得到鈷複閤氮摻雜的炭氣凝膠。攷察間苯二酚和三聚氰胺比例、凝膠pH值及炭化條件等對氣凝膠結構和催化氧還原活性的影響,採用XRD、XPS、低溫氮氣吸脫附等方法研究催化劑的結構。隨pH值增加,MR氣凝膠的介孔分佈嚮小孔移動;噹M/R物質的量比為6:1時,其介孔分佈為3.0~4.0 nm。鈷複閤炭氣凝膠多孔結構中存在均勻分佈Co金屬顆粒和管狀炭,Co金屬顆粒粒徑隨炭化溫度升高而增加。採用鏇轉圓盤電極研究催化劑在0.5 mol/L H2 SO4溶液中的電化學性能,結果錶明催化劑具有良好的氧還原活性。
이삼취청알、간분이분、갑철위원료,채용용효-응효법、냉동간조등보취제비출삼취청알-간분이분-갑철( MR)간응효;병이소제탄기응효위재체침지초산고,경담기중고온탄화,득도고복합담참잡적탄기응효。고찰간분이분화삼취청알비례、응효pH치급탄화조건등대기응효결구화최화양환원활성적영향,채용XRD、XPS、저온담기흡탈부등방법연구최화제적결구。수pH치증가,MR기응효적개공분포향소공이동;당M/R물질적량비위6:1시,기개공분포위3.0~4.0 nm。고복합탄기응효다공결구중존재균균분포Co금속과립화관상탄,Co금속과립립경수탄화온도승고이증가。채용선전원반전겁연구최화제재0.5 mol/L H2 SO4용액중적전화학성능,결과표명최화제구유량호적양환원활성。
Melamine-resorcinol-formaldehyde ( MR) aerogels were prepared by the sol-gel polymerization of formaldehyde with melamine and resorcinol using NaOH as catalyst, followed by freeze-drying. Co-loaded carbon aerogels were obtained by impregna-ting the MR aerogels with Co( III) tert-butanol solution, followed by carbonization in N2 . The effects of the molar ratios of mela-mine to resorcinol ( M/R) , pH, Co content and carbonization temperature on the microstructure of the aerogels were investigated. It was found that the microstructure of the MR aerogels could be adjusted by the M/R ratio and pH. The mesopore size of the MR aer-ogels decreased with increasing pH and the mesopore size was in the range of 3-4nm when the M/R was 6:1. There were some gra-phitic nano-ribbons in Co-loaded carbon aerogels. The metal average particle size in the carbon aerogels increased from 5. 2 to 6. 2 nm when the carbonization temperature was increased from 700 to 900℃. The electrochemical properties of the Co-loaded car-bon aerogels as catalysts in the oxygen reduction reaction were evaluated by a rotating disc electrode technique in an O2-saturated 0. 5 mol/L H2 SO4 solution, and the catalysts showed a good electrocatalytic activity for the reaction.