介孔碳的制備及其用于超級(jí)電容器電極材料的研究
發(fā)布時(shí)間：2019-02-20 21:20
【摘要】：超級(jí)電容器是一種介于傳統(tǒng)電容器和電池之間的一種新型儲(chǔ)能元件。它具有功率密度高、充放電速率快、超高的電容量、超長(zhǎng)的壽命、價(jià)格較低、免維護(hù)、對(duì)環(huán)境比較友善、安全性高等優(yōu)點(diǎn)，因此受到了國(guó)內(nèi)外科學(xué)家的廣泛關(guān)注，可以用于信息技術(shù)、交通、國(guó)防科技和航空航天等領(lǐng)域，具有相當(dāng)大的市場(chǎng)和使用前景。 本論文使用無(wú)模板高溫碳化法，以葡萄糖和葡萄糖與三聚氰胺混合物為前驅(qū)體，通過(guò)調(diào)節(jié)碳化過(guò)程中氮?dú)鈮毫?lái)控制孔的尺寸進(jìn)而制備介孔碳材料（Mesoporouscarbon—MCs）和氮摻雜介孔碳（Nitrogen-doped mesoporous carbon—NMCs）材料，實(shí)現(xiàn)了雙電層電容和法拉第贗電容的良好結(jié)合。同時(shí)利用氮?dú)馕矫摳椒治觯˙ET）、高分辨透射電子顯微鏡分析（HRTEM）、X射線光電子能譜（XPS）和循環(huán)伏安（CV）、交流阻抗（EIS）、恒流充放電等測(cè)試手段對(duì)材料的結(jié)構(gòu)、形貌、電化學(xué)性能進(jìn)行表征與分析。 實(shí)驗(yàn)結(jié)果表明，在真空和不同的氮?dú)鈮毫ο隆囟葹?20°C保溫4h制備的多孔碳材料具備一定的混亂度。在0MPa和0.02MPa氮?dú)鈮毫l件下，制備的多孔碳材料為微孔材料；在0.05MPa和0.1MPa氮?dú)鈮毫l件下，制備的多孔碳材料的孔徑由微孔變?yōu)榻榭�，孔徑分布范圍分別為2～4nm和2～3.5nm。隨著氮?dú)鈮毫Φ脑黾�，孔徑分布范圍變窄，主要是由于高壓�?huì)壓縮孔體積和阻礙前驅(qū)體的分解。 采用不同質(zhì)量比的三聚氰胺和葡萄糖制備的NMCs材料中N1s的類型分別為吡啶型N即N-6（398.7eV）、吡啶/吡咯型N即N-5（399.8eV）和石墨型N即N-Q（401eV），原子含量分別為0.46%、1.04%和0.78%。 通過(guò)電化學(xué)測(cè)試結(jié)果可知，制備的MCs材料經(jīng)KOH活化后具有更好的電化學(xué)穩(wěn)定性和可逆性；在氮?dú)鈮毫?.05MPa下制備的MCs材料具有更高的比電容，達(dá)到250F·g-1。在電流密度為2A·g-1時(shí)，循環(huán)掃描1000圈后，，比電容衰減4%。以質(zhì)量比分別為1、2、6的三聚氰胺和葡萄糖為前驅(qū)體制備NMCs，在質(zhì)量比為2時(shí)，獲得的NMCs材料具有更高的電容，達(dá)到442.5F·g-1。在電流密度為2A·g-1時(shí)，制備的MCs和NMCs的比電容分別為250F·g-1和442.5F·g-1。
[Abstract]:Supercapacitor is a new energy storage element between conventional capacitor and battery. It has the advantages of high power density, high charge / discharge rate, super high capacitance, long life, low price, no maintenance, friendly to the environment, high safety and so on, so it has attracted wide attention from scientists at home and abroad. Can be used in information technology, transportation, defense science and technology, aerospace and other fields, with considerable market and application prospects. In this paper, a template free high-temperature carbonization method was used. Glucose and glucose mixtures with melamine were used as precursors. The mesoporous carbon materials (Mesoporouscarbon-MCs) and nitrogen-doped mesoporous carbon (Nitrogen-doped mesoporous carbon-NMCs) materials were prepared by controlling the pore size by adjusting the nitrogen pressure during carbonation. The combination of double layer capacitance and Faraday pseudo-capacitance was achieved. At the same time, (BET), high resolution transmission electron microscopy (TEM) was used to analyze the structure of (HRTEM), X ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV),) (CV), impedance constant current charge / discharge (EIS),) measurements. The morphology and electrochemical properties were characterized and analyzed. The experimental results show that the porous carbon materials prepared at 620 擄C for 4 h under vacuum and different nitrogen pressure have a certain degree of confusion. Under the nitrogen pressure of 0MPa and 0.02MPa, the porous carbon materials are microporous materials. Under the nitrogen pressure of 0.05MPa and 0.1MPa, the pore size of the prepared porous carbon materials changed from micropore to mesoporous, and the pore size distribution ranges from 2~4nm and 2C3.5 nm, respectively. With the increase of nitrogen pressure, the pore size distribution becomes narrower, mainly because the high pressure will compress the pore volume and hinder the decomposition of the precursor. The types of N1s in NMCs materials with different mass ratios of melamine and glucose are pyridine N-6 (398.7eV), pyridine / pyrrole N-5 (399.8eV) and graphite-type N-Q (401eV), respectively. The atomic content was 0.46% and 0.78%, respectively. The electrochemical test results show that the prepared MCs material has better electrochemical stability and reversibility after KOH activation, and the MCs material prepared under the nitrogen pressure of 0.05MPa has a higher specific capacitance up to 250F g-1. When the current density is 2A g ~ (-1), after 1000 cycles of cyclic scanning, the capacitance is attenuated 4 times. NMCs, was prepared by using melamine and glucose as precursors. When the mass ratio was 2, the obtained NMCs material had a higher capacitance, reaching 442.5 F g-1. When the current density is 2A g ~ (-1), the specific capacitance of MCs and NMCs are 250F g ~ (-1) and 442.5 F g ~ (-1), respectively.
【學(xué)位授予單位】：燕山大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：TM53
本文編號(hào)：2427287
[Abstract]:Supercapacitor is a new energy storage element between conventional capacitor and battery. It has the advantages of high power density, high charge / discharge rate, super high capacitance, long life, low price, no maintenance, friendly to the environment, high safety and so on, so it has attracted wide attention from scientists at home and abroad. Can be used in information technology, transportation, defense science and technology, aerospace and other fields, with considerable market and application prospects. In this paper, a template free high-temperature carbonization method was used. Glucose and glucose mixtures with melamine were used as precursors. The mesoporous carbon materials (Mesoporouscarbon-MCs) and nitrogen-doped mesoporous carbon (Nitrogen-doped mesoporous carbon-NMCs) materials were prepared by controlling the pore size by adjusting the nitrogen pressure during carbonation. The combination of double layer capacitance and Faraday pseudo-capacitance was achieved. At the same time, (BET), high resolution transmission electron microscopy (TEM) was used to analyze the structure of (HRTEM), X ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV),) (CV), impedance constant current charge / discharge (EIS),) measurements. The morphology and electrochemical properties were characterized and analyzed. The experimental results show that the porous carbon materials prepared at 620 擄C for 4 h under vacuum and different nitrogen pressure have a certain degree of confusion. Under the nitrogen pressure of 0MPa and 0.02MPa, the porous carbon materials are microporous materials. Under the nitrogen pressure of 0.05MPa and 0.1MPa, the pore size of the prepared porous carbon materials changed from micropore to mesoporous, and the pore size distribution ranges from 2~4nm and 2C3.5 nm, respectively. With the increase of nitrogen pressure, the pore size distribution becomes narrower, mainly because the high pressure will compress the pore volume and hinder the decomposition of the precursor. The types of N1s in NMCs materials with different mass ratios of melamine and glucose are pyridine N-6 (398.7eV), pyridine / pyrrole N-5 (399.8eV) and graphite-type N-Q (401eV), respectively. The atomic content was 0.46% and 0.78%, respectively. The electrochemical test results show that the prepared MCs material has better electrochemical stability and reversibility after KOH activation, and the MCs material prepared under the nitrogen pressure of 0.05MPa has a higher specific capacitance up to 250F g-1. When the current density is 2A g ~ (-1), after 1000 cycles of cyclic scanning, the capacitance is attenuated 4 times. NMCs, was prepared by using melamine and glucose as precursors. When the mass ratio was 2, the obtained NMCs material had a higher capacitance, reaching 442.5 F g-1. When the current density is 2A g ~ (-1), the specific capacitance of MCs and NMCs are 250F g ~ (-1) and 442.5 F g ~ (-1), respectively.
【學(xué)位授予單位】：燕山大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：TM53
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