CN103072986A - 一种梯度恒温活化法制备棉秆基活性炭电极材料的方法 - Google Patents
一种梯度恒温活化法制备棉秆基活性炭电极材料的方法 Download PDFInfo
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- 238000004140 cleaning Methods 0.000 claims description 13
- 230000001264 neutralization Effects 0.000 claims description 12
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- 238000007598 dipping method Methods 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000011363 dried mixture Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials data:image/svg+xml;base64,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 data:image/svg+xml;base64,PD94bWwgdmVyc2lvbj0nMS4wJyBlbmNvZGluZz0naXNvLTg4NTktMSc/Pgo8c3ZnIHZlcnNpb249JzEuMScgYmFzZVByb2ZpbGU9J2Z1bGwnCiAgICAgICAgICAgICAgeG1sbnM9J2h0dHA6Ly93d3cudzMub3JnLzIwMDAvc3ZnJwogICAgICAgICAgICAgICAgICAgICAgeG1sbnM6cmRraXQ9J2h0dHA6Ly93d3cucmRraXQub3JnL3htbCcKICAgICAgICAgICAgICAgICAgICAgIHhtbG5zOnhsaW5rPSdodHRwOi8vd3d3LnczLm9yZy8xOTk5L3hsaW5rJwogICAgICAgICAgICAgICAgICB4bWw6c3BhY2U9J3ByZXNlcnZlJwp3aWR0aD0nODVweCcgaGVpZ2h0PSc4NXB4JyB2aWV3Qm94PScwIDAgODUgODUnPgo8IS0tIEVORCBPRiBIRUFERVIgLS0+CjxyZWN0IHN0eWxlPSdvcGFjaXR5OjEuMDtmaWxsOiNGRkZGRkY7c3Ryb2tlOm5vbmUnIHdpZHRoPSc4NS4wJyBoZWlnaHQ9Jzg1LjAnIHg9JzAuMCcgeT0nMC4wJz4gPC9yZWN0Pgo8dGV4dCB4PSczLjQnIHk9JzUzLjYnIGNsYXNzPSdhdG9tLTAnIHN0eWxlPSdmb250LXNpemU6MjNweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiNFODQyMzUnID5IPC90ZXh0Pgo8dGV4dCB4PScxOC4yJyB5PSc1My42JyBjbGFzcz0nYXRvbS0wJyBzdHlsZT0nZm9udC1zaXplOjIzcHg7Zm9udC1zdHlsZTpub3JtYWw7Zm9udC13ZWlnaHQ6bm9ybWFsO2ZpbGwtb3BhY2l0eToxO3N0cm9rZTpub25lO2ZvbnQtZmFtaWx5OnNhbnMtc2VyaWY7dGV4dC1hbmNob3I6c3RhcnQ7ZmlsbDojRTg0MjM1JyA+TzwvdGV4dD4KPHRleHQgeD0nMzQuMScgeT0nNDQuMycgY2xhc3M9J2F0b20tMCcgc3R5bGU9J2ZvbnQtc2l6ZToxNXB4O2ZvbnQtc3R5bGU6bm9ybWFsO2ZvbnQtd2VpZ2h0Om5vcm1hbDtmaWxsLW9wYWNpdHk6MTtzdHJva2U6bm9uZTtmb250LWZhbWlseTpzYW5zLXNlcmlmO3RleHQtYW5jaG9yOnN0YXJ0O2ZpbGw6I0U4NDIzNScgPi08L3RleHQ+Cjx0ZXh0IHg9JzU2LjcnIHk9JzUzLjYnIGNsYXNzPSdhdG9tLTEnIHN0eWxlPSdmb250LXNpemU6MjNweDtmb250LXN0eWxlOm5vcm1hbDtmb250LXdlaWdodDpub3JtYWw7ZmlsbC1vcGFjaXR5OjE7c3Ryb2tlOm5vbmU7Zm9udC1mYW1pbHk6c2Fucy1zZXJpZjt0ZXh0LWFuY2hvcjpzdGFydDtmaWxsOiMzQjQxNDMnID5LPC90ZXh0Pgo8dGV4dCB4PSc3Mi42JyB5PSc0NC4zJyBjbGFzcz0nYXRvbS0xJyBzdHlsZT0nZm9udC1zaXplOjE1cHg7Zm9udC1zdHlsZTpub3JtYWw7Zm9udC13ZWlnaHQ6bm9ybWFsO2ZpbGwtb3BhY2l0eToxO3N0cm9rZTpub25lO2ZvbnQtZmFtaWx5OnNhbnMtc2VyaWY7dGV4dC1hbmNob3I6c3RhcnQ7ZmlsbDojM0I0MTQzJyA+KzwvdGV4dD4KPC9zdmc+Cg== [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M lithium hydroxide Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- -1 ZnCl 2 Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound 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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
本发明涉及一种梯度恒温活化法制备棉秆基活性炭电极材料的方法,该方法以棉秆为原料,将棉秆经清洗粉碎后进行炭化处理,然后与活化剂混合浸渍,通过梯度恒温活化法有效控制了大、中、微孔之间的比例,形成一种具有多孔结构的超级电容器用棉秆基活性炭电极材料。本发明所述方法通过对活化时间的梯度控制来调节棉杆基活性炭的孔径,具有较高的比表面积(1900m2/g)、较合理的孔径分布和较好的电容特性,其比容量超过180F/g,且循环500次后无容量衰减,表现出良好的电容特性,这对实现棉花产业的可持续发展,促进生物质资源的开发利用、深加工及超级电容器用多孔炭电极材料的研究具有重要现实意义。
Description
一种梯度恒温活化法制备棉秆基活性炭电极材料的方法
技术领域
[0001] 本发明涉及一种梯度恒温活化法制备棉杆基活性炭电极材料的方法,属于电化学领域。
背景技术
[0002] 能源是人类赖以生存和发展的基础,由于全球石油资源日趋短缺,燃烧石油的内燃机排放的尾气对环境的污染越来越严重,能源的供给和需求之间的矛盾日益突出。人们都在努力研究替代内燃机的新型能源装置。目前,人们已经对混合动力、燃料电池、化学电池等产品进行研究与开发,并且取得了一定的成效。但是它们使用寿命短、温度特性差、化学电池污染环境、系统复杂、造价昂贵等一些致命的弱点,一直没有得到很好的解决,限制了其实际应用。因此,寻找一种新型绿色能源迫在眉睫。
[0003] 超级电容器(supercapacitors) 又称电化学电容器(electrochemicalcapacitors, ECS),它是一种介于二次电池和传统电容器之间的新型储能元件。它由于具有功率密度高、循环寿命长、能瞬间大电流充放电、工作温度范围宽、安全、无污染等优点,填补了物理电容器与蓄电池这两类储能器件的空白。它独特的性质使得它发挥了无可替代的作用,尤其是在短时间大功率放电应用方面。广泛应用于移动通讯、工业领域、消费电子、电动汽车和国防科技等方面。同时还可作为辅助电源,与蓄电池联合作为飞机、坦克、火箭、导弹、人造卫星、宇宙飞船空间站和潜艇等的点火或启动电源。其巨大的应用潜力引起了越来越多的关注,成为当前化学电源领域的研究热点之一。
[0004] 可用作超级电容器电极材料的碳材料主要有:活性炭、炭气凝胶、活性炭纤维、碳纳米管。其按孔径大小分可以分为微孔(microporous)炭(<2nm)、介孔(mesoporous)炭(2-50nm)和大孔(macroporo us)炭(>50nm)。碳材料的研究主要集中在制备具有较大比表面积和较小电阻的多孔电极上,理想的碳电极材料,应该具有高比表面积、高中孔率、高电导率以及良好的电解液浸润性。
[0005] 活性炭材料的工业生产和应用历史悠久,具有比表面积大,导电性能优良、抗化学腐蚀性能好、热膨胀系数小,且低廉易得、易于实现工业化生产等特点。它是最早用于超级电容器的电极材料。制备活性炭的原料也比较丰富,煤、石油焦、木材、果壳、树脂、浙青等都是制备超级电容器用活性炭材料的优良原料。但由于资源的短缺,特别是煤和木屑的供应,给活性炭材料产业的发展带来了巨大压力。因此,寻找合适的新型原料成为活性炭行业持续发展的重要任务之一。
[0006] 随着中国农业的发展,棉花产量大幅上升,目前中国在世界上四大产棉国中位居第二。与此同时,棉花种植业还得到大量的副产物-棉杆。棉杆的利用技术单一,或直接堆怄还田,或烧火做饭取暖,导致其能量转化率和利用率都会很低。目前尚无用梯度恒温活化法制备超级电容器用棉杆基活性炭电极材料的报道。根据棉杆自身结构特点,因地制宜,通过将多种方法有机地组合起来,形成一种多层次、多途径综合利用的方式.从而提高棉杆利用率,促进其产业化。发明内容
[0007] 本发明的目的在于,提供一种梯度恒温活化法制备棉杆基活性炭电极材料的方法。该方法以棉杆为原料,将棉杆经清洗粉碎后进行炭化处理,然后与活化剂混合浸溃,通过梯度恒温活化法有效控制了大、中、微孔之间的比例,形成一种具有多孔结构的棉杆基活性炭电极材料。本发明所述方法通过梯度控制活化时间来调节棉杆基活性炭的孔径,制备的棉杆基活性炭电极材料具有较高的比表面积、较合理的孔径分布和较好的电容特性。其比表面积可达到1900m2/g,比容量超过200F/g。对实现棉花产业的可持续发展,以及提高超级电容器性能、降低电极材料生产成本具有重要意义。
[0008] 本发明所述的一种梯度恒温活化法制备棉杆基活性炭电极材料的方法,按下列步骤进行:
[0009] a、将棉杆清洗,粉碎成200 μ m-10mm颗粒,在温度70_120°C烘干;
[0010] b、将烘干后的棉杆颗粒在惰性气体保护或真空条件下,以温度2_50°C /min的升温速率升至400-90(TC,恒温l_20h进行炭化,得到炭化材料;
[0011] C、将炭化材料进行研磨后,与活化剂按固液比1:2-7混合,浸溃0.5-72h ;
[0012] d、将步骤c的混合物放入烘箱于温度70_120°C进行干燥处理;
[0013] e、在惰性气体保护或真空条件下,将干燥后的混合物以温度2_50°C /min升温,在温度400-900°C区间进行梯度恒温,在各个温度区间恒温0.25-10h,得到活性炭材料;
[0014] f、将步骤e得到的活性炭材料随炉降至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0015]步骤 c 中所述的活化剂为 KOH、NaOH, ZnCl2, NaCl、LiOH, CaCl2, H2O2, H3PO4 中的一种或两种或三种,其中活化剂浓度为20-70%。
[0016] 所述步骤b和e中的保护气体为氩气、氮气或氩气与氢气的混合气体,其中混合气体中氢气体积含量为40-60%。
[0017] 步骤b和e中所述的真空条件的真空度为133.322 X 1(Γ3_133.322 X l(T5Pa。
[0018] 本发明所述的一种梯度恒温活化法制备棉杆基活性炭电极材料的方法,通过该方法获得的棉杆基活性炭电极材料用于超级电容器,经采用全自动物理氮气吸附仪ASAP2020(美国Micromeritics公司产),以BET方法计算比表面积,采用SEM进行形貌分析,结果表明:制备的棉杆基活性炭电极材料拥有较高的比表面积和较好的电容特性。将制备的棉杆基活性炭电极材料研磨至0.3-40 μ m左右,采用涂抹法制备电极,以铝箔为集流体,聚丙烯(MPF35)为隔膜,以ImoVLEt4NBF4为电解液,组装成的钮扣超级电容器具有较好的电化学特性,即具有较高的比电容、 较小的等效串联电阻和稳定的循环特性,可见棉杆基活性炭可以作为制备超级电容器的电极材料。
附图说明
[0019] 图1为本发明的恒流充放电图;
[0020] 图2为本发明的循环伏安图;
[0021] 图3为本发明的不同活化时间下的交流阻抗图;
[0022] 图4为本发明的在2A/g电流密度下循环稳定性图。具体实施方式
[0023] 实施例1:
[0024] a、将棉杆清洗,粉碎成200 μ m颗粒,在温度80°C烘干;
[0025] b、将烘干后的棉杆颗粒在惰性气体氩气保护下,以温度2V Mn的升温速率升至温度900°C,恒温Ih进行炭化,得到炭化材料;
[0026] C、将步骤b中的炭化材料进行研磨后,与活化剂浓度为20%的KOH按固液比1: 2进行混合,浸溃0.5h ;
[0027] d、将浸溃混合物放入烘箱于温度80°C烘干;
[0028] e、在惰性气体氩气保护条件下,将步骤d得到的干燥后的混合物以温度2V /min升温,按照梯度恒温活化,首先在温度400°C恒温Ih后,然后升温至500°C恒温lh,最后升温至800°C恒温2h,得到活性炭材料;
[0029] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0030] 实施例2:
[0031] a、将棉杆清洗,粉碎成Imm颗粒,在温度100°C烘干;
[0032] b、将烘干后的棉杆颗粒在惰性气体氮气保护下,以温度5°C /min的升温速率升至500°C,恒温IOh进行炭化,得到炭化材料;
[0033] c、将步骤b中的炭化材料进行研磨,与活化剂浓度为40%的ZnCl2按固液比1:3混合,浸溃12h ;
[0034] d、将浸溃后的混合物放置烘箱于温度100°C进行干燥处理;
[0035] e、在惰性气体氮气保护条件下,将步骤d得到的干燥混合物以温度5°C/min升温,按梯度升温活化,首先在温度600°C恒温5h,然后升温至700°C恒温10h,最后升温至800°C恒温lh,得到活性炭材料;
[0036] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0037] 实施例3
[0038] a、将棉杆清洗,粉碎成800/ μ m颗粒,在温度70°C烘干;
[0039] b、将烘干后的棉杆颗粒在惰性气体氮气与氢气混合气体的保护下,其中氢气体积含量为40%,以温度30°C /min的升温速率升至800°C,恒温IOh进行炭化,得到炭化材料;
[0040] c、将步骤b中的炭化材料进行研磨后,与活化剂浓度为50%的NaOH按固液比1:5混合,浸溃24h ;
[0041] d、将浸溃后的混合物放入烘箱于温度80°C进行干燥处理;
[0042] e、在惰性气体氮气与氢气混合气体的保护下,其中氢气体积含量为40%,将步骤d得到的混合物以温度10°C /min升温,按梯度恒温活化,首先在温度500°C恒温5h,温度600°C恒温Ih后,然后升温至700°C恒温10h,最后升温至800°C恒温lh,得到活性炭材料;
[0043] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0044] 实施例4[0045] a、将棉杆清洗、粉碎成500 μ m颗粒,在温度80°C烘干;
[0046] b、将烘干后的棉杆颗粒在惰性气体氩气与氢气的混合气体保护下的气氛炉里(氢气体积含量为50%)烧结,以温度40°C /min的升温速率升至400°C,恒温20h进行炭化,得到炭化材料;
[0047] C、配制活化剂浓度为35%的CaCl、浓度为40%的ZnCl2和浓度为60%的H2O2的按质量比5:2: 3,将步骤b中的炭化材料研磨后,与配制好的活化剂按固液比1:4混合,进行混合浸溃12h ;
[0048] d、将浸溃后的混合物放入烘箱于温度80°C进行干燥处理;
[0049] e、在惰性气体氩气与氢气的混合气体保护下的气氛炉里(氢气体积含量为50%),将干燥后的混合物以温度40° C /min升温,按梯度恒温活化,首先在温度400°C恒温Ih后,然后分别在温度500°C恒温lh、温度600°C恒温2h、温度700°C恒温3h、温度800°C恒温4h,最后温度900°C恒温lh,得到活性炭材料;
[0050] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C下进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0051] 实施例5
[0052] a、将棉杆清洗,粉碎成Icm颗粒,在温度120°C烘干;
[0053] b、将烘干后的棉杆颗粒在真空条件下的气氛炉里(真空度为133.322X 10_3Pa)烧结,以温度50°C /min的升温速率升至800°C,恒温3h进行炭化,得到炭化材料;
[0054] c、将步骤b中的炭化材料进行研磨,与活化剂浓度为55%的H3PO4按固液比1:5混合,浸溃24h ;
[0055] d、将浸溃后的混合物放入烘箱于温度120°C进行干燥处理;
[0056] e、在真空条件下(真空度为133.322 X 10_3Pa),将干燥后的混合物以温度50°C /min升温,按照梯度恒温活化,首先在温度60(TC恒温5h后,然后升温70(TC恒温2h,最后800°C恒温5h,得到活性炭材料;
[0057] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C下进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0058] 实施例6
[0059] a、将棉杆清洗、粉碎成2mm颗粒,在温度11 (TC烘干;
[0060] b、将烘干后的棉杆颗粒在真空条件下的气氛炉里(真空度为133.322X 10_5Pa)烧结,以温度5°C /min的升温速率升至750°C,恒温IOh进行炭化,得到炭化材料;
[0061] C、将炭化材料进行研磨后,与活化剂浓度为60%的LiOH按固液比1:7进行混合,浸溃72h ;
[0062] d、将浸溃后的混合物放入烘箱于温度110°C进行干燥处理;
[0063] e、在真空条件下(真空度为133.322X 10_5Pa),将干燥后的混合物以温度5°C /min升温,按照梯度恒温活化,首先在温度60(TC恒温0.25h后,然后升温至70(TC恒温10h,最后温度800°C恒温lh,得到活性炭材料;
[0064] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C下进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0065] 实施例7[0066] a、将棉杆清洗,粉碎成5mm颗粒,在温度120°C烘干;
[0067] b、将烘干后的棉杆颗粒在真空条件下的气氛炉里(真空度为133.322X 10_5Pa)烧结,以温度15°C /min的升温速率升至850°C,恒温20h,进行炭化,得到炭化材料;
[0068] C、将步骤b的炭化材料进行研磨后,与活化剂浓度为70%的H2O2按固液比1:7进行混合,浸溃72h ;
[0069] d、将浸溃后的混合物放入烘箱于温度120°C进行干燥处理;
[0070] e、在真空条件下(真空度为133.322 X 10_5Pa),将干燥后的混合物以温度15°C /min升温,按照梯度恒温活化,首先在温度600°C恒温Ih后,然后在温度700°C恒温lh,温度800°C恒温2h,得到活性炭材料;
[0071] f、将步骤e得到的活性炭材料随炉降至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0072] 实施例8
[0073] a、将棉杆清洗,粉碎成5mm颗粒,在温度80°C烘干;
[0074] b、将烘干后的棉杆颗粒在惰性气体氮气保护下烧结,以5°C /min的升温速率升至6000C,恒温2h,进行炭化,得到炭化材料;
[0075] C、配制活化剂浓度为40%的ZnCl2和浓度为30%的NaCl按质量比7:3配制成50%混合液,将步骤b得到的炭化材料研磨后,与配制好的活化剂混合液按固液比1:6混合,将其浸溃72h ;
[0076] d、将浸溃后的混合物于 温度80°C烘干;
[0077] e、在惰性气体氮气保护下,将干燥后的混合物以温度5°C /min升温,按照梯度恒温活化,首先在温度60(TC恒温Ih后;然后在温度70(TC恒温lh,在温度80(TC恒温2h,得到活性炭材料;
[0078] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C下进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0079] 实施例9
[0080] a、将棉杆清洗,粉碎成3mm颗粒,在温度105°C烘干;
[0081] b、将烘干后的棉杆颗粒在惰性气体氩气保护下,以温度25°C /min的升温速率升至600°C,恒温3h进行炭化,得到炭化材料;
[0082] C、将炭化材料进行研磨后,与活化剂浓度为65%的H2SO4按固液比1:2进行混合,浸溃12h ;
[0083] d、将浸溃后的混合物放入烘箱于温度90°C进行干燥处理;
[0084] e、在惰性气体氩气保护下,将干燥后的混合物以温度25°C /min升温,按照梯度恒温活化,首先在温度600°C恒温3h,然后升温至700°C恒温lh,最后温度800°C恒温lh,得到活性炭材料;
[0085] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C下进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0086] 实施例10
[0087] a、将棉杆清洗,粉碎成IOmm颗粒,在温度120°C烘干;
[0088] b、将烘干后的棉杆颗粒在惰性气体氮气的保护下,以温度30°C /min的升温速率升至800°C,恒温3h进行炭化,得到炭化材料;
[0089] C、配制活化剂浓度为30%的NaOH和浓度为30%的KOH按质量比1:1配制成40%的混合液,将炭化材料进行研磨后,与配制好的活化剂混合液按固液比1:7进行混合,浸溃24h ;
[0090] d、将浸溃后的混合物放入烘箱于温度90°C进行干燥处理;
[0091] e、在惰性气体氮气的保护下,将干燥后的混合物以温度10°C /min升温,按梯度恒温活化,首先在温度500°C恒温5h,温度600°C恒温Ih后,然后升温至700°C恒温10h,最后升温至800°C恒温lh,得到活性炭材料;
[0092] f、将步骤e中得到的活性炭材料随炉降温至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
[0093] 实施例11
[0094] 将实施例1-10任意获得的用于超级电容器的棉杆基活性炭电极材料进行研磨至0.3-40 μ m,然后将其和粘结剂乳液按质量比8:2的比例称取,加入0.1ml去离子水进行混合,将混合物均匀涂覆在集流体铝箔上,在10MPa的压力下压制成片,待自然晾干后,用(Φ 12mm)铳子裁片,放入真空烘箱中,在温度120°C干燥8h,取出后称取其质量,其中活性物质的质量可通过电极片质量减去招箔的质量后得到;将质量相近(精确到0.1mg)的电极片组装成模拟纽扣式超级电容器;
[0095] 以实施例1为例,将制备的活性炭浓度在3mol/L的KOH为电解液进行电化学性能测试,电压区间为0-1V,测得制备的棉杆基活性炭电极材料的比电容为208F/g,等效串联电阻为2.98 Ω,能量密度为22.0ThKg^1,功率密度为800.2ffhKg^ ;
[0096] 以实施例4为例,将制备的活性炭浓度在浓度为lmol/L Et4NBF4为电解液进行电化学性能测试,电压区间为0-3.5V,测得制备的棉杆基活性炭电极材料的比电容为190F/g,等效串联电阻为10.5Ω,能量密度为85.eWhKg—1,功率密度为787.AWhKg-1
Claims (4)
1.一种梯度恒温活化法制备棉杆基活性炭电极材料的方法,其特征在于按下列步骤进行: a、将棉杆清洗,粉碎成200 μ 颗粒,在温度70-120°C烘干; b、将烘干后的棉杆颗粒在惰性气体保护或真空条件下,以温度2-50°C /min的升温速率升至400-90(TC,恒温l_20h进行炭化,得到炭化材料; C、将炭化材料进行研磨后,与活化剂按固液比1:2-7混合,浸溃0.5-72h ; d、将步骤c的混合物放入烘箱于温度70-120°C进行干燥处理; e、在惰性气体保护或真空条件下,将干燥后的混合物以温度2-50°C /min升温,在温度400-900°C区间进行梯度恒温,在各个温度区间恒温0.25-10h,得到活性炭材料; f、将步骤e得到的活性炭材料随炉降至室温,经洗涤至中性,然后于温度80°C进行干燥处理,即可得到用于超级电容器的棉杆基活性炭电极材料。
2.根据权利要求1所述的方法,其特征在于步骤c中所述的活化剂为KOH、NaOH、ZnCl2、NaCl.LiOH, CaCl2, H2O2> H3PO4中的一种或两种或三种,其中活化剂浓度为20_70%。
3.根据权利要求1所述的方法,其特征在于所述步骤b和e中的保护气体为氩气、氮气或氩气与氢气的混合气体,其中混合气体中氢气体积含量为40-60%。
4.根据权利要求1所述的方法,其特征在于步骤b和e中所述的真空条件的真空度为133.322X 1(Γ3- 13 3.322Χ l(T5Pa。
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