高密度间苯二酚-甲醛碳气凝胶ICF靶的制备与吸附性能研究

 以间苯二酚和甲醛为前驱体，通过改进传统制备技术解决了高密度间苯二酚-甲醛(CRF)碳气凝胶制备过程中的龟裂问题，制备出了符合ICF实验需要的高密度CRF碳气凝胶材料。分别对CRF碳气凝胶的元素组成和物相组成进行了鉴定，采用自动吸附仪考察了CRF碳气凝胶对N₂和H₂的吸附性能。结果表明：该碳气凝胶是一种由C元素组成的类似石墨结构的非晶固态材料，结构均匀性好，具有良好的机械加工性能，比表面积达676 m²·g^-1，平均孔径为7.16 nm；氢吸附质量分数达2.28%，相应体积密度为17.83 kg·m^-3。     

CO2活化温度对碳气凝胶结构及氢吸附性能影响

 以间苯二酚(R)和甲醛(F)为前驱体制备出RF碳气凝胶,并利用CO₂气体对其进行活化,通过热重分析(TG)、X射线衍射(XRD)、氢吸附等表征手段研究了活化过程中温度对碳气凝胶微结构及氢吸附性能的影响。结果表明：CO₂活化可使碳气凝胶比表面积大幅提高,且不会影响其微孔网络结构。随着活化温度的升高,碳气凝胶非晶性变得更加明显,失重率显著增加,微孔体积、比表面积及氢吸附量先增后减,有望通过改变CO₂活化温度增加碳气凝胶微孔数量来提高其氢吸附性能。     

种子法制备金掺杂二氧化硅气凝胶

 采用羟胺种子法合成了金掺杂二氧化硅气凝胶。采用紫外 可见光分光光度计研究了还原过程中体系的变化情况。使用透射电镜（TEM）研究了气凝胶的微观结构，气凝胶的比表面积和孔径分布由BET-BJH方法测试。结果表明通过种子法可以制备金掺杂质量分数0.01%~1.00%，密度25～50 mg／cm³，比表面积达800 m²/g以上的SiO₂气凝胶样品。     

对苯二酚-甲醛碳气凝胶的制备

 溶胶-凝胶法制备了高HC比（10~40，对苯二酚与催化剂(Na₂CO_{3/sub>)的物质的量之比）的对苯二酚-甲醛有机气凝胶，并经高温碳化处理得到其碳气凝胶。借助有机气凝胶的红外光谱研究了其化学结构，说明其网孔结构形成的可能性；研究了有机气凝胶的扫描电镜图像、比表面积及孔径分布等，并得到碳化前后的一些对比数据：有机气凝胶颗粒大小30~50 nm，碳化后约为10 nm，比表面积从341.77 m²/g增大到452.75 m²/g，密度从0.170 8 g/cm^{3/sup>增大到0.335 6 g/cm3/sup>。}}     

MF气凝胶的制备和结构表征

 以三聚氰胺(M)和甲醛(F)为原料，经溶胶-凝胶和超临界干燥工艺制备出密度156.82 mg/cm³的MF气凝胶。通过X射线衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)及比表面测定仪(BET)等测试手段研究了其结构和性能。XRD结果表明MF气凝胶是一种非晶材料；TEM和SEM结果表明MF气凝胶所有孔孔径均在10 nm左右；孔径分布及比表面积测试仪测得该气凝胶具有很高的比表面积（1 015.98 m²/g），孔径大小主要为5~30 nm。所得MF气凝胶是一种具有nm量级3维网络结构的轻质多孔材料，有望在ICF实验靶中得到应用。     

碳气凝胶及活化碳气凝胶电极材料制备与性能

 以间苯二酚(R)-甲醛(F)为原料,制备了有机气凝胶和碳气凝胶,并对其进行二氧化碳活化。X射线衍射(XRD)测试表明,二氧化碳渗入到碳气凝胶网络结构发生反应,造成(002)峰和(100)峰减弱;扫描电子显微镜(SEM)测试表明,活化没有破坏碳气凝胶的骨架结构,而是增加了大量的nm尺度微孔,从而大大提高了碳气凝胶的比表面积和微孔比例。在1 mol/L KOH电解液中进行了循环伏安和计时电位扫描测试,电极材料电化学性能稳定,具有较好的可逆性,在1 mA/s电流密度下进行充放电测试,得到活化前电极比电容为103 F/g,活化后由于比表面积的增加,比电容达到371 F/g,是一种理想的电化学电极材料。     

密度渐变多层碳气凝胶靶型的制备

 以间苯二酚-甲醛为原料,结合自制活动式微模具成型工艺制备不同厚度和密度的碳气凝胶薄片,采用密度为10 mg·cm^-3的SiO₂溶胶为“粘合剂”,获得单元薄片厚度在100～580 μm,密度在50～400 mg·cm^-3范围内变化的5层密度渐变碳气凝胶靶型。重点研究了该特殊靶型内部C/SiO₂气凝胶层间界面情况。采用场发射扫描电镜（FESEM）,X射线相衬成像仪等对靶型整体结构及碳气凝胶单元薄片表面和内部微观结构进行了表征。结果表明：胶粘层SiO₂气凝胶厚度约为15 μm,厚度一致,远小于碳气凝胶层厚度且与碳气凝胶薄片的胶粘程度较好,界面平整,靶结构均匀。     

氮掺杂碳气凝胶电极材料的制备及性能

以三聚氰胺（M）、间苯二酚（R）和甲醛（F）为原料,经溶胶-凝胶法、超临界干燥和高温碳化制备了系列的氮掺杂碳气凝胶（NCAs）。X射线光电子能谱(XPS)分析表明,氮元素成功地引入到碳气凝胶中,并且可以通过调节三聚氰胺掺杂量来控制氮掺杂量;扫描电子显微镜（SEM）和N2吸附测试显示出不同氮掺杂量的碳气凝胶的微观结构差异较大,随着氮含量的增加,比表面积有先减后增的趋势;在6 mol/L KOH溶液中进行的恒流充放电和循环伏安测试表明,引入氮元素能够极大地改善碳气凝胶的电化学性能,最高比电容量达176 Fg-1,并且凝胶具有良好的电容特性和可逆性。     

间苯三酚-乙醛有机气凝胶的制备与表征

 以碳酸钠为催化剂,乙醇为溶剂,间苯三酚 乙醛为反应前躯体,经溶胶 凝胶、交联老化、二氧化碳超临界干燥制备出间苯三酚-乙醛(PA)有机气凝胶。扫描电镜观察和N2吸附测试结果表明：气凝胶具有较高的比表面积,是一种连续nm级３维网络结构的多孔材料,其比表面积为1 210 m²/g,平均孔径为11 nm,与传统有机气凝胶相比,提高了比表面积,一定程度上实现有机气凝胶的扩孔。     

常压干燥法制备碳气凝胶及其电极性能研究北大核心CSCD

以间苯二酚-甲醛为前驱体,通过加入P123以增强有机气骨架的方法,采用常压干燥技术制备碳气凝胶电极材料,有机凝胶在干燥过程中收缩率极大降低。通过二氧化碳活化法对常压干燥获得的碳气凝胶孔结构进行了调控。研究了不同温度对其结构的影响,获得了最高比表面积达3544m2/g的碳气凝胶。6mol/L的KOH电解液中测试表明,常压干燥碳气凝胶具有稳定的充放电性能,随着活化温度的升高,比容量逐渐增加,最高比电容可达261F/g。常压干燥技术制备的碳气凝胶电极材料在降低生产成本的同时,仍具有理想的电化学性能。     

Preparation and characterization of metal-doped carbon aerogel for supercapacitor

Carbon aerogel was prepared by polycondensation of resorcinol and formaldehyde using sodium carbonate as a catalyst with a resorcinol to catalyst ratio of 500. Co-doped carbon aerogels were then prepared by an impregnation method with a variation of cobalt content (1, 3, 5, 7, 10, and 15 wt.%), and their performance for supercapacitor electrode was investigated by measurement of specific capacitance in 1 M H₂SO₄ electrolyte at a scan rate of 10 mV/s. Among the samples prepared, 7 wt.% Co-doped carbon aerogel showed the highest capacitance (100 F/g) and stable cyclability. The enhanced capacitance of Co-doped carbon aerogel was attributed to the faradaic redox reactions of cobalt oxide. On the basis of this result, 7 wt.% Cu-, Fe-, Mn-, and Zn-doped carbon aerogels were also prepared by an impregnation method for use as a supercapacitor electrode. Among the metal-doped carbon aerogels, Mn-doped carbon aerogel showed the highest capacitance (107 F/g) while Cu- and Fe-doped carbon aerogels exhibited the most stable cyclability.     

超高比表面积氮掺杂碳气凝胶的制备及其电化学性能

以间苯二酚和甲醛为反应前驱体, 三聚氰胺为氮源, 通过溶胶-凝胶法制备出氮掺杂碳气凝胶(N-CA), 并对其进行CO2活化后得到活化氮掺杂碳气凝胶(N-ACA), 分别通过扫描电子显微镜、氮吸附、X-光电子能谱和元素分析研究样品的表面形态、孔结构以及含氮官能团的存在形态, 并利用恒流充放电(GV)、循环伏安(CV)、电化学阻抗谱等检测技术评价了其在6 molL-1 KOH电解液中的电化学性能。 实验结果表明: 丰富的孔隙结构和含氮官能团的存在形态是影响碳基电容器性能的决定性因素。 经CO2活化后的N-CA富含较多的的微孔和介孔, 比表面积高达4082 m2g-1, 供电子能力较强的吡咯氮含量有所增加, 在1 mA电流密度下测试的比电容值高达211.9 Fg-1, 经1200次充放电后比电容值保持在98%以上。     

Preparation of carbon aerogel in ambient conditions for electrical double-layer capacitor

Carbon aerogels were prepared by polycondensation of resorcinol with formaldehyde using sodium carbonate as a catalyst in ambient conditions, and they were used as an electrode of electrical double-layer capacitor. The effect of resorcinol to catalyst ratio (R/C ratio) on volume shrinkage, BET surface area, and electrochemical property of carbon aerogels was investigated by changing R/C ratio from 50 to 2000. In order to minimize volume shrinkage, solvent exchange was performed with acetone at 50 °C for 1 day. Volume shrinkage was <2% after 2-day gelation in the absence of CO₂ supercritical drying. BET surface area was strongly dependent on R/C ratio. Carbon aerogel prepared at R/C ratio of 500 showed the highest BET surface area (706 m²/g) with average pore diameter of 10.9 nm. Electrochemical property of carbon aerogels as an electrode of electrical double-layer capacitor was investigated by cyclic voltammetry measurement. Specific capacitance of carbon aerogel prepared at R/C ratio of 500 was found to be 81 F/g in 1 M H₂SO₄ electrolyte at the scan rate of 10 mV/s.     

Mn-doped activated carbon aerogel as electrode material for pseudo-capacitive supercapacitor: Effect of activation agent

Carbon aerogel (CA) was prepared by a sol-gel polymerization of resorcinol and formaldehyde, and a series of activated carbon aerogels (ACA-X, X = H₃PO₄, K₂CO₃, KOH, and ZnCl₂) were then prepared by a chemical activation using different activation agent (X represented an activation agent). Specific capacitances of activated carbon aerogels were measured by cyclic voltammetry and galvanostatic charge/discharge methods in 6 M KOH electrolyte. Among the samples prepared, ACA-K₂CO₃ showed the highest specific capacitance (152 F/g). In order to combine excellent electrochemical performance of activated carbon aerogel with pseudo-capacitive property of manganese oxide, 7 wt% manganese oxide was doped on activated carbon aerogels (Mn/ACA-X) by an incipient wetness impregnation method. Capacitance measurements revealed that Mn/ACA-K₂CO₃ showed the highest specific capacitance (189 F/g). The enhanced capacitance of Mn/ACA-K₂CO₃ was attributed to the fine pore structure and outstanding electric properties of activated carbon aerogel as well as the faradaic redox reactions of manganese oxide.     

低密度Cu掺杂SiO_2复合气凝胶的制备及表征

分别以正硅酸甲酯、醋酸铜为硅源和铜源,通过溶胶凝胶法及CO2超临界干燥技术制备了一系列Cu掺杂SiO2复合气凝胶。采用红外谱仪(FTIR)、扫描电镜(SEM)、X射线能谱仪(EDS)、比表面积和孔隙度分析仪(BET)、动态热机械分析仪(DMA)对样品进行了表征。结果表明随着铜含量的增加,复合气凝胶密度增加,比表面积降低,平均孔径增加,实际掺杂比与理论掺杂比对应增加。该复合气凝胶具有三维网状结构,密度低(40mg/cm3),比表面积高(390m2/g),成型性较好,有望应用于惯性约束聚变(ICF)实验。     

Activated carbon aerogel as electrode material for coin-type EDLC cell in organic electrolyte

Carbon aerogel (CA) was prepared by a carbonization of resorcinol–formaldehyde (RF) polymer gels, and it was chemically activated with KOH to obtain activated carbon aerogel (ACA) for electrode material for EDLC in organic electrolyte. Coin-type EDLC cells with two symmetrical carbon electrode were assembled using the prepared carbon materials. Electrochemical performance of the carbon electrodes was measured by galvanostatic charge/discharge and cyclic voltammetry methods. Activated carbon aerogel (20.9 F/g) showed much higher specific capacitance than carbon aerogel (7.9 F/g) and commercial activated carbon (8.5 F/g) at a scan rate of 100 mV/s. This indicates that chemical activation with KOH served as an efficient method to improve electrochemical performance of carbon aerogel for EDLC electrode in organic electrolyte. The enhanced electrochemical performance of activated carbon aerogel was attributed to the high effective surface area and the well-developed pore structure with appropriate pore size obtained from activation with KOH.