CN106215954A - 一种碳纤维@二硒化钨纳米片核壳复合结构及其制备方法 - Google Patents
一种碳纤维@二硒化钨纳米片核壳复合结构及其制备方法 Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 52
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 52
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- SDDGNMXIOGQCCH-UHFFFAOYSA-N 3-fluoro-n,n-dimethylaniline Chemical compound CN(C)C1=CC=CC(F)=C1 SDDGNMXIOGQCCH-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000012159 carrier gas Substances 0.000 claims abstract description 24
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 21
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 3
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- 239000007772 electrode material Substances 0.000 abstract description 3
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
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- 230000001699 photocatalysis Effects 0.000 description 7
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- 150000003624 transition metals Chemical class 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- MEOSMFUUJVIIKB-UHFFFAOYSA-N [W].[C] Chemical compound [W].[C] MEOSMFUUJVIIKB-UHFFFAOYSA-N 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 238000005215 recombination Methods 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种碳纤维@二硒化钨纳米片核壳复合结构及其制备方法,属于材料制备技术领域。本发明提出的复合结构的内核是碳纤维、外壳是成阵列状的二硒化钨纳米片。本发明在真空管式炉中,用热蒸发技术直接蒸发硒粉作为硒源,在载气作用下,在高温下熏蒸浸泡过WO3悬浊液的预氧化聚丙烯腈纤维,实现碳纤维和二硒化钨纳米片的同时合成,能高产率地制备得到所述碳纤维@二硒化钨纳米片核壳复合结构。该方法的产品产量大、密度高、纯度高,形貌可控,无需后处理;且该方法具有设备和工艺简单、合成生长条件严格可控、产品收率高、成本低廉、生产过程清洁环保等优点。所获得材料是优异的可见光催化剂、电催化剂、钠/锂/镁离子电池电极材料等。
Description
技术领域
本发明涉及一种碳纤维@二硒化钨纳米片核壳复合结构及其制备方法,属于材料制备技术领域。
背景技术
二硒化钨作为一种典型的过渡金属二硫属化物,具有类石墨烯的层状结构。在二硒化钨材料中,由一层钨原子夹在两层硒原子之间构成三明治状的单层二硒化钨,其单层内原子间以强的共价键键合,各单层间以微弱的范德华力相连接。这种独特的层状结构使得二硒化钨具有独特的力学、热学、光学和电学性能,所以二硒化钨纳米材料不仅在润滑、磨损、隔热领域具有重要应用,而且在催化(如可见光降解有机污染物、电催化制氢)、钠(或锂)离子电池(如阳极材料)、镁离子电池(如阴极材料)、光电转化(如发光二极管、太阳能电池)、电子器件(如场效应晶体管)等领域也有着巨大的潜在应用前景,吸引了广泛关注。
虽然二硒化钨的带隙较小(约1.65eV),具有强的可见光吸收能力,理论上其在光电转化以及光催化领域会表现出非常优异的性能;但是实际上,相比于其他的过渡金属二硫属化物(如二硫化钨、二硫化钼等),关于二硒化钨材料在太阳能电池、光催化降解有机污染物以及可见光制氢等方面的应用报道却非常少。导致这种现象的主要原因有两个:一是二硒化钨材料、特别是其高性能纳米材料的合成相对较难,因为含硒前驱体的反应活性不如含硫前驱体;二是光催化过程中产生的电子和空穴非常容易复合,使得二硒化钨材料在光电转化以及光催化方面的性能表现较差。而二硒化钨的生产原料在自然界储量丰富,且价格低廉。因此,合成具有高光催化活性的二硒化钨及其复合纳米材料具有极大的实际应用价值。
提高二硒化钨材料的可见光催化能力的常用方法是,将二硒化钨和其他导电性较好的材料(如石墨烯等碳材料)复合,使得光生电子可以通过导电性好的材料快速传导出去,从而降低二硒化钨光生电子-空穴对的复合率,进而提高二硒化钨材料在光催化和光电转化等应用方面的性能。此外,与石墨复合还可以增强二硒化钨的导电性,从而使其在作为电催化剂或者电极材料等获得更好的应用。
目前,合成二硒化钨-碳复合材料的主要方法,一种是一步法,该方法将二硒化钨和碳的前驱体材料直接混合进行固相反应,但是这种方法所得到的二硒化钨-碳复合材料的形貌不可控,且反应副产物较多,后续提纯、除杂非常困难;另一种是两步法,先制备出钨-碳复合前驱体,再在高温下对其进行硒化,但是其制备过程复杂、冗长。因此,开发一种可以一步合成二硒化钨-碳复合材料,且产物形貌可控、操作简单的制备方法非常必要。
本发明直接采用市售的预氧化聚丙烯腈(PAN)纤维作碳源,利用其在高温下才热解成碳的特点,在真空管式炉中,用热蒸发技术直接蒸发硒粉末作为硒源,以惰性气体作为保护气体和载气,在高温下熏蒸浸泡过WO3悬浊液的预氧化聚丙烯腈纤维,实现了碳纤维和二硒化钨纳米片的同时合成,制备得到了一种特殊的碳纤维@二硒化钨纳米片核壳复合结构,其中的二硒化钨纳米片成阵列状生长在碳纤维表面。由于热蒸发沉积技术具有成本低、制备过程简单、工艺参数可控性强、可实现工业化大批量生产等特点,用本发明提出的这种碳纤维@二硒化钨纳米片核壳复合结构的制备方法,所得到的复合结构材料产量大、密度高、纯度高,形貌可控,无需后处理,且制备方法经济环保。
发明内容
本发明的目的之一在于提出一种碳纤维@二硒化钨纳米片核壳复合结构,这种复合结构的内核是碳纤维,外壳是成阵列状的二硒化钨纳米片。这种复合结构材料用于光催化时,既能充分利用二硒化钨纳米片带隙较小的特点,提高可见光的吸收率,还能利用碳纤维的良好的导电性能,促进光催化过程中产生的光生电子和空穴的分离,提高光催化效率;因此,这种复合结构材料能显著提高可见光对有害有机污染物的降解效率,提高可见光光解水制氢的效率,以及改善太阳能光电转化的效率等。由于这种复合结构材料中由阵列状的二硒化钨纳米片和高导电性的碳纤维构成,将其用于钠离子、锂电池和镁离子电极材料时有利于这些金属离子的嵌入和脱嵌,提高电池容量;用于电催化水解制氢时有利于电子的传导,提高制氢效率。此外,这种复合结构材料还可望在发光晶体管等领域有重要的应用。
本发明的目的之二在于提供这种碳纤维@二硒化钨纳米片核壳复合结构相应的制备方法。这种方法制备出的复合结构材料产量大、密度高、纯度高,形貌可控,无需后处理;而且该方法具有设备和工艺简单、合成生长条件严格可控、产品收率高、成本低廉、生产过程清洁环保等优点。
为了达成上述目标,本发明提出的碳纤维@二硒化钨纳米片核壳复合结构,其特征在于,所述复合结构的内核是碳纤维,外壳是成阵列状的二硒化钨纳米片。这种碳纤维@二硒化钨纳米片核壳复合结构,产物纯度高、密度大,碳纤维被二硒化钨纳米片充分包裹而呈现核壳结构,内核碳纤维直径4-10μm,外壳二硒化钨纳米片呈阵列排列,纳米片厚度30-110nm,纳米尺度有序。
本发明提供的碳纤维@二硒化钨纳米片核壳复合结构的制备方法,其特征在于,该方法利用预氧化聚丙烯腈纤维在高温下才热解成碳的特点,在真空管式炉中,用热蒸发技术直接蒸发硒粉末作为硒源,在载气作用下,在高温下熏蒸浸泡过WO3悬浊液的预氧化聚丙烯腈纤维,实现碳纤维和二硒化钨纳米片的同时合成,能高产率地制备得到所述碳纤维@二硒化钨纳米片核壳复合结构。
本发明提出的碳纤维@二硒化钨纳米片核壳复合结构的制备方法,包括以下步骤和内容:
(1)在真空管式炉中,将装有硒粉的氧化铝陶瓷坩埚放置在气流上方距离炉中央加热区域25-45cm处,将盛有浸泡过WO3悬浊液的预氧化聚丙烯腈纤维的石英基片放置在炉中央加热区域。
(2)在加热前,先用真空泵对整个系统抽真空至0.01Pa以下,然后向系统中通入高纯惰性载气,并重复多次,以排除系统中的空气。然后以10-20℃/min的速率升温到300-500℃,并保温5-20分钟,再以20-30℃/min的速率升温到1000-1150℃,并保温2-5小时。在加热过程中,在真空系统持续工作的前提下通入载气并保持载气流量为100-300标准立方厘米每分钟(sccm),且整个加热过程在惰性载气保护下完成,最后自然降温到室温,即可在基片上得到大量高纯度、高密度的碳纤维@二硒化钨纳米片核壳复合结构。
在上述制备方法中,所述步骤(1)中的蒸发源硒粉为市售分析纯试剂。
在上述制备方法中,所述步骤(1)中的WO3悬浊液为市售分析纯WO3粉在无水乙醇中分散而成,其中WO3粉与乙醇的配比为(10-80g):(50-100ml)。
在上述制备方法中,所述步骤(1)中的预氧化聚丙烯腈纤维为市售化学纯试剂。
在上述制备方法中,所述步骤(1)中的预氧化聚丙烯腈纤维在WO3悬浊液中浸泡10-60min,然后晾干待用。
在上述制备方法中,所述步骤(1)中的蒸发源硒粉与炉中央加热区域的距离为25-45cm。
在上述制备方法中,所述步骤(2)中高纯惰性载气为氩气、氮气之中的一种。
在上述制备方法中,所述步骤(2)中的惰性载气为高纯气体,纯度在99.99vol.%以上。
在上述制备方法中,所述步骤(2)中的惰性载气流量为100-300标准立方厘米每分钟(sccm)。
在上述制备方法中,所述步骤(2)中的加热过程为先以10-20℃/min的速率升温到300-500℃,并保温5-20分钟,再以20-30℃/min的速率升温到1000-1150℃,并保温2-5小时。
在上述制备方法中,所述步骤(2)中的降温过程为自然降温到室温。
采用本技术制备所述碳纤维@二硒化钨纳米片核壳复合结构,具有设备和工艺简单、合成生长条件严格可控、产品收率高、成本低廉、生产过程清洁环保等特点;所获得的碳纤维@二硒化钨纳米片核壳复合结构密度高、纯度高,纳米尺度有序、直径和厚度均匀、形貌可控,无需后处理。
附图说明
图1是本发明实施例1所制得的碳纤维@二硒化钨纳米片核壳复合结构的X-射线衍射花样及其解析结果
图2是本发明实施例1所制得的碳纤维@二硒化钨纳米片核壳复合结构的表面的扫描电镜照片
图3是本发明实施例1所制得的碳纤维@二硒化钨纳米片核壳复合结构的剖面处的扫描电镜表面照片
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明。
本发明提出一种碳纤维@二硒化钨纳米片核壳复合结构,其特征在于,所述复合结构的内核是碳纤维,外壳是成阵列状的二硒化钨纳米片。这种碳纤维@二硒化钨纳米片核壳复合结构,产物纯度高、密度大,碳纤维被二硒化钨纳米片充分包裹而呈现核壳结构,内核碳纤维直径4-10μm,外壳二硒化钨纳米片呈阵列排列,纳米片厚度30-110nm,纳米尺度有序。
本发明提供的碳纤维@二硒化钨纳米片核壳复合结构的制备方法,其特征在于,该方法利用预氧化聚丙烯腈纤维在高温下才热解成碳的特点,在真空管式炉中,用热蒸发技术直接蒸发硒粉末作为硒源,在载气作用下,在高温下熏蒸浸泡过WO3悬浊液的预氧化聚丙烯腈纤维,实现碳纤维和二硒化钨纳米片的同时合成,能高产率地制备得到所述碳纤维@二硒化钨纳米片核壳复合结构。
本发明提出的碳纤维@二硒化钨纳米片核壳复合结构的制备方法,包括以下步骤和内容:
(1)采用市售分析纯硒粉、WO3粉以及化学纯预氧化聚丙烯腈纤维为原料。
(2)将WO3粉与无水乙醇按照(10-80g):(50-100ml)的配比混合,充分搅拌制成均匀的悬浊液;然后将预氧化聚丙烯腈纤维放置在其中浸泡10-60min;然后晾干,待用。
(3)在真空管式炉中,将装有硒粉的氧化铝陶瓷坩埚放置在气流上方距离炉中央加热区域25-45cm处,将盛有浸泡过WO3悬浊液的预氧化聚丙烯腈纤维的石英基片放置在炉中央加热区域。
(4)在加热前,先用真空泵对整个系统抽真空至0.01Pa以下,然后向系统中通入高纯惰性载气,并重复多次,以排除系统中的空气。然后以10-20℃/min的速率升温到300-500℃,并保温5-20分钟,再以20-30℃/min的速率升温到1000-1150℃,并保温2-5小时。在加热过程中,在真空系统持续工作的前提下通入载气并保持载气流量为100-300标准立方厘米每分钟(sccm),且整个加热过程在惰性载气保护下完成,最后自然降温到室温,即可在基片上得到大量高纯度、高密度的碳纤维@二硒化钨纳米片核壳复合结构。
(5)所用的高纯惰性载气为氩气、氮气之中的一种,纯度在99.99vol.%以上,且整个实验加热过程在载气保护下完成。
所得到的碳纤维@二硒化钨纳米片核壳复合结构外观上为深灰色纤维状物质。
在扫描电子显微镜下,能观察到大量的纤维,且纤维呈现壳核结构,X-射线衍射分析表明,这种材料为高纯度的C/WSe2复合材料。其内核为直径4-10μm的碳纤维,外壳为大量的成阵列排列的二硒化钨纳米片,纳米片厚度30-110nm。
总之,用本技术能高产率获得高纯度、高密度的碳纤维@二硒化钨纳米片核壳复合结构。
实施例1:在真空管式炉中,将装有2g硒粉的氧化铝陶瓷坩埚放置在气流上方距离炉中央加热区域37cm处,将盛有浓度为2.5g WO3粉和5ml无水乙醇配制的悬浊液浸泡处理的并晾干的预氧化聚丙烯腈纤维的石英基片放置在炉中央加热区域。
在加热前,先用真空泵对整个系统抽真空至0.01Pa以下,然后向系统中通入99.99vol.%以上的高纯氩气,并重复3次,以排除系统中的空气。然后以20℃/min速率升温到400℃,保温10分钟,再以25℃/min速率升温到1100℃,并保温2小时。在加热过程中,在真空系统持续工作的前提下通入氩气并保持载气流量为200标准立方厘米每分钟(sccm),且整个加热过程在氩气保护下完成,最后自然降温到室温,即可在基片上得到大量高纯度、高密度的碳纤维@二硒化钨纳米片核壳复合结构。
所制得的深灰色纤维状物质为高纯度的C/WSe2复合材料(见图1),这种材料为碳纤维@二硒化钨纳米片核壳复合结构(见图2),其内核为碳纤维、外壳是成阵列状的高密度的二硒化钨纳米片(见图3),所得材料产量大,纳米片直径、厚度均匀(见图2)。
Claims (4)
1.一种碳纤维@二硒化钨纳米片核壳复合结构,其特征在于,所述复合结构的内核是碳纤维,外壳是成阵列状的二硒化钨纳米片;所述复合结构产物纯度高、密度大,碳纤维被高密度的二硒化钨纳米片充分包裹而呈现核壳结构。
2.按照权利要求1所述的碳纤维@二硒化钨纳米片核壳复合结构的制备方法,其特征在于,所述方法在真空管式炉中,用热蒸发技术直接蒸发硒粉末作为硒源,在载气作用下,在高温下熏蒸浸泡过WO3悬浊液的预氧化聚丙烯腈纤维,实现碳纤维和二硒化钨纳米片的同时合成,能高产率地制备得到所述碳纤维@二硒化钨纳米片核壳复合结构;包括以下步骤:
(1)在真空管式炉中,将装有硒粉的氧化铝陶瓷坩埚放置在气流上方距离炉中央加热区域25-45cm处,将盛有浸泡过WO3悬浊液的预氧化聚丙烯腈纤维的石英基片放置在炉中央加热区域;
(2)在加热前,先用真空泵对整个系统抽真空至0.01Pa以下,然后向系统中通入高纯惰性载气,并重复多次,以排除系统中的空气;然后以10-20℃/min的速率升温到300-500℃,并保温5-20分钟,再以20-30℃/min的速率升温到1000-1150℃,并保温2-5小时;在加热过程中,在真空系统持续工作的前提下通入载气并保持载气流量为100-300标准立方厘米每分钟(sccm),且整个加热过程在惰性载气保护下完成,最后自然降温到室温,即可在基片上得到大量高纯度、高密度的碳纤维@二硒化钨纳米片核壳复合结构。
3.按照权利要求2所述的制备方法,其特征在于,所述步骤(1)中的硒粉和WO3粉为市售分析纯试剂,预氧化聚丙烯腈纤维为市售化学纯试剂;所述WO3悬浊液为WO3粉在无水乙醇中分散而成,其中WO3粉与乙醇的配比为(10-80g):(50-100ml);所述预氧化聚丙烯腈纤维在WO3悬浊液中的浸泡时间为10-60min,然后晾干待用;所述蒸发源硒粉与炉中央加热区域的距离为25-45cm。
4.按照权利要求2所述的制备方法,其特征在于,所述步骤(2)中的高纯惰性载气为氩气、氮气之中的一种,纯度在99.99vol.%以上,流量为100-300标准立方厘米每分钟(sccm);所述加热过程为先以10-20℃/min的速率升温到300-500℃,并保温5-20分钟,再以20-30℃/min的速率升温到1000-1150℃,并保温2-5小时。
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CN113457714A (zh) * | 2021-07-15 | 2021-10-01 | 内蒙古工业大学 | 一种复合光催化材料及其制备方法和应用 |
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