CN114256463A - 一种基底有序介孔石墨烯的包覆方法 - Google Patents
一种基底有序介孔石墨烯的包覆方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 51
- 239000000758 substrate Substances 0.000 title claims abstract description 42
- 238000000576 coating method Methods 0.000 title claims abstract description 19
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 229940096992 potassium oleate Drugs 0.000 claims abstract description 14
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 12
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- 239000002244 precipitate Substances 0.000 claims abstract description 10
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- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 7
- 238000005087 graphitization Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052582 BN Inorganic materials 0.000 claims description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
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- 238000010000 carbonizing Methods 0.000 claims description 8
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- 238000000197 pyrolysis Methods 0.000 claims description 3
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- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 abstract description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 abstract description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 abstract description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 abstract description 11
- 239000005642 Oleic acid Substances 0.000 abstract description 11
- HOIQWTMREPWSJY-GNOQXXQHSA-K iron(3+);(z)-octadec-9-enoate Chemical compound [Fe+3].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O HOIQWTMREPWSJY-GNOQXXQHSA-K 0.000 abstract description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- -1 iron ions Chemical class 0.000 abstract description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 6
- 238000005341 cation exchange Methods 0.000 abstract description 3
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 16
- 238000001000 micrograph Methods 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 10
- 239000002356 single layer Substances 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007429 general method Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229940049964 oleate Drugs 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
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- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
本发明提出了一种基底有序介孔石墨烯的包覆方法,包括以下步骤:将基底分散于油酸钾或油酸钠溶液中,超声、搅拌使其均匀分散;缓慢加入硝酸铁溶液,发生阳离子交换,铁离子取代掉油酸钾中的钾离子,摇晃使其沉淀,然后水洗;所得沉淀经过冻干、氮气氛围热解,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳、再经过酸刻蚀、氩气氛围下石墨化即可实现基底上介孔石墨烯的包覆。本发明可以在多种基底包覆一层有序介孔石墨烯,方法简单且石墨化可调。
Description
技术领域
本发明属于材料和无机化学领域,具体来说是一种基底有序介孔石墨烯的包覆方法,尤其是一种利用表面化学修饰在多种基底上包覆介孔石墨烯的方法。
背景技术
随着“碳达峰、碳中和”目标的提出,纳米材料迎来了全新的发展契机,其中碳材料可作为催化剂载体、导电剂等多重身份应用于各种能量存储和转化领域,大大促进了新能源领域的发展。目前商业上已经开发出多种碳材料,包括石墨烯、碳纳米管、碳纤维、科琴黑、Super P、炭黑等等。每款商品都有自己独特的结构特点和物化性质,在商品价格、应用价值上各有优劣,但上述碳产品却不能适用于各种领域。
基底碳包覆是一种新型碳材料修饰方法,它旨在对现有碳材料或其他基底进行碳包覆从而赋予新的物化性质而大大扩宽应用领域。但现有的碳包覆技术的方法是单一的,只能在一种或很少的基底上负载。而且包覆上的碳结构无序、石墨化程度低。因此,开发一种能够在各种基底上包覆有序介孔石墨烯的通用方法很有必要。
发明内容
本发明的目的在于提出一种基底有序介孔石墨烯的包覆方法,通过表面化学修饰,可以在多种基底上包覆一层有序介孔石墨烯。
本发明提出的一种基底包覆有序介孔石墨烯的通用方法,包括以下步骤:
(1)将基底分散于油酸钾或油酸钠溶液中,超声搅拌;
(2)向步骤(1)所得的溶液中加入硝酸铁溶液,沉淀后水洗;
步骤(2)中加入硝酸铁发生阳离子交换反应,铁离子交换掉油酸钾中的钾离子得到油酸铁和硝酸钾,而油酸铁不溶于水,带着基底一起水中沉淀,而硝酸钾极易溶于水,从而实现前驱体与副产物的分离,避免副产物对后续反应的影响;
(3)将步骤(2)所得沉淀冻干,然后高温热解、刻蚀、石墨化;
其中,步骤(1)中所述的基底为石墨烯、二氧化硅微球、碳管、氮化硼、碳纤维或硅片中的一种;
步骤(3)中高温热解条件为N2氛围下,400-500℃碳化2-4小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳;刻蚀剂为3-6 mol/L 的盐酸溶液;步骤(3)中石墨化条件为Ar氛围,800-1600 oC石墨化3-6小时。
本发明中,步骤(1)中基底为石墨烯,层数1-2层,直径1-5微米。
本发明中,步骤(1)中基底为直径10-60 nm的碳纳米管。
本发明中,步骤(1)中基底为直径厚度5-10nm,直径2-6的微米的氮化硼二维片。
本发明中,步骤(1)中基底为直径400-800 nm的二氧化硅微球。
本发明中,步骤(1)中基底为直径5-15μm的碳纤维。
本发明中,步骤(1)中基底为直径5-30 mm的硅片。
本发明中,步骤(1)中油酸钾或油酸钠与步骤(2)中的硝酸铁的摩尔比为3:1。
本发明得到的基底包覆的石墨烯为单层、有序、具有15 nm左右的介孔。
本发明将油酸钾修饰在各种基底表面,然后加入硝酸铁,通过阳离子交换在基底表面原位生成油酸铁前驱体,然后洗涤冻干、原位热解、刻蚀,最后石墨化即在基底上包覆一层有序介孔石墨烯。
本发明的有益效果在于可以在多种基底组包覆一层有序介孔石墨烯,方法简单,且石墨化程度可调、包覆高效。而现有方法只能在单种基底上包覆,且包覆的碳大多无序、石墨化程度低,应用价值有限。因此本发明开发了在基底上包覆有序介孔石墨烯的方法。
附图说明
图1是实施例1制得的石墨烯包覆有序介孔石墨烯的透射电镜图;
图2是实施例2制得的碳纳米管包覆有序介孔石墨烯的透射电镜图;
图3是实施例3制得的氮化硼包覆有序介孔石墨烯的透射电镜图;
图4是实施例4制得的碳纤维包覆有序介孔石墨烯的扫描电镜图;
图5是实施例5制得的二氧化硅包覆有序介孔石墨烯的透射电镜图;
图6是实施例6制得的硅片包覆的有序介孔石墨烯扫描电镜图。
具体实施方式
实施例1
(1)将20 mg石墨烯分散于20 ml 0.25 mol/L 的油酸钾溶液中,超声30分钟、搅拌两小时使其均匀分散。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下, 500 oC碳化2小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用6 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围, 1600 oC石墨化3小时。
图1是实施例1制得的石墨烯包覆有序介孔石墨烯的透射电镜图,可以看出石墨烯表面包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在石墨烯上表面包覆一层有序介孔石墨烯。
实施例2
(1)将50 mg碳纳米管分散于20 ml 0.25 mol/L 的油酸钾溶液中,超声30分钟、搅拌两小时使其均匀分散。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下,400 oC碳化4小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用3 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围,800 oC石墨化6小时。
图2是实施例2制得的碳纳米管包覆有序介孔石墨烯的透射电镜图,可以看出碳纳米管表面包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在碳纳米管表面包覆一层有序介孔石墨烯。
实施例3
(1)将40 mg氮化硼二维片分散于20 ml 0.25 mol/L 的油酸钾溶液中,超声30分钟、搅拌两小时使其均匀分散。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下,500 oC碳化3小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用5 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围,1600 oC石墨化5小时。
图3是实施例3制得的氮化硼包覆有序介孔石墨烯的透射电镜图,可以看出氮化硼表面包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在氮化硼表面包覆一层有序介孔石墨烯。
实施例4
(1)将100 mg 商业碳纤维 (公司:金博股份,型号:T300)浸润于10 ml 0.25 mol/L 的水溶性油酸钾溶液中。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下,400 oC碳化4小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用6 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围,1600 oC石墨化5小时。
图4是实施例4制得的碳纤维包覆有序介孔石墨烯的透射电镜图,可以看出碳纤维包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在碳纤维表面包覆一层有序介孔石墨烯。
实施例5
(1)将50 mg二氧化硅微球分散于20 ml 0.25 mol/L 的油酸钾溶液中,超声30分钟、搅拌两小时使其均匀分散。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下,500 oC碳化2小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用6 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围, 1600 oC石墨化3小时。
图5是实施例5制得的二氧化硅包覆有序介孔石墨烯的透射电镜图,可以看出二氧化硅表面包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在二氧化硅表面包覆一层有序介孔石墨烯。
实施例6
(1)将1块直径20mm商用硅片(公司:北京特博,型号:普通硅片)浸润于3 ml 0.25mol/L 的水溶性油酸钠溶液中,超声30分钟使其均匀分散。
(2)向步骤(1)所得的溶液中缓慢加入2.5 ml 1 mol/L 的硝酸铁溶液,摇晃使其沉淀,然后水洗三次。
(3)将步骤(2)所得沉淀冻干保持形貌,然后N2氛围下,400 oC碳化2小时,此时油酸铁中的铁离子转变为四氧化三铁纳米颗粒,而油酸根均匀包覆在纳米颗粒上并热解为碳,再用5 mol/L 的盐酸溶液刻蚀三次,最后Ar氛围, 1000 oC石墨化4小时。
图6是实施例6制得的硅片包覆有序介孔石墨烯的透射电镜图,可以看出硅片表面包覆一层有序介孔石墨烯,且单层、有序、具有15 nm左右的介孔。表明此方法能够在硅片表面包覆一层有序介孔石墨烯。
Claims (8)
1.一种基底有序介孔石墨烯的包覆方法,其特征在于,包括以下步骤:
(1)将基底分散于油酸钾或油酸钠溶液中,超声搅拌;
(2)向步骤(1)所得的溶液中加入硝酸铁溶液,沉淀后水洗;
(3)将步骤(2)所得沉淀冻干,然后高温热解、刻蚀、石墨化;
其中,步骤(1)中所述的基底为石墨烯、二氧化硅微球、碳管、氮化硼、碳纤维或硅片中的一种;
步骤(3)中高温热解条件为N2氛围下,400-500℃碳化2-4小时;刻蚀剂为3-6 mol/L 的盐酸溶液;步骤(3)中石墨化条件为Ar氛围,800-1600 oC石墨化3-6小时。
2.根据权利要求1所述的方法,其特征在于步骤(1)中基底为石墨烯,层数1-2层,直径1-5微米。
3.根据权利要求1所述的方法,其特征在于步骤(1)中基底为直径10-60 nm的碳纳米管。
4.根据权利要求1所述的方法,其特征在于步骤(1)中基底为直径厚度5-10nm,直径2-6的微米的氮化硼二维片。
5.根据权利要求1所述的方法,其特征在于步骤(1)中基底为直径400-800 nm的二氧化硅微球。
6.根据权利要求1所述的方法,其特征在于步骤(1)中基底为直径5-15μm的碳纤维。
7.根据权利要求1所述的方法,其特征在于步骤(1)中基底为直径5-30 mm的硅片。
8.根据权利要求1所述的方法,其特征在于步骤(1)中油酸钾或油酸钠与步骤(2)中的硝酸铁的摩尔比为3:1。
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