CN114228182A - 一种快速制备石墨烯三明治型光热转换地膜的方法 - Google Patents

一种快速制备石墨烯三明治型光热转换地膜的方法 Download PDF

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CN114228182A
CN114228182A CN202111614968.XA CN202111614968A CN114228182A CN 114228182 A CN114228182 A CN 114228182A CN 202111614968 A CN202111614968 A CN 202111614968A CN 114228182 A CN114228182 A CN 114228182A
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graphene
mulching film
sandwich type
photothermal conversion
polyimide
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CN114228182B (zh
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王振洋
张淑东
李年
宋彦平
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Hefei Intelligent Agriculture Collaborative Innovation Research Institute Of China Science And Technology
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Abstract

本发明公开了一种快速制备石墨烯三明治型光热转换地膜的方法，属于农业地膜新材料技术领域。本发明采用高能束流制备石墨烯技术实现高质量、3D多孔石墨烯，并利用热压技术实现聚合物‑石墨烯‑聚合物三明治型地膜的成膜，真正将高光热转换效率的石墨烯材料制备和复合材料膜生产集成到一个步骤中。其中，石墨烯高的光吸收性能赋予了地膜全光谱吸收能力，可以实现高效的光热转换；主要的成膜材料使用热塑性的聚合物，通过热辊压实现复合材料的成膜。本发明中的石墨烯制备方法速度快、成本低，所得石墨烯质量高光热转换效率高，并且易于实现工业化的卷对卷生产，在光热转换薄膜制备等领域有很大的应用前景。

Description

一种快速制备石墨烯三明治型光热转换地膜的方法
技术领域
本发明涉及一种快速制备石墨烯三明治型光热转换地膜的方法，属于农业地膜新材料技术领域。
背景技术
太阳能作为一种绿色能源，具有以下优点：(1)分布广泛。太阳光几乎可以照射到地球的每个角落，可以直接采集和利用，节省了大量人力和物力。(2)清洁、无消耗。太阳能的开发和利用不会带来任何环境污染和其它能源消耗，也不会带来任何社会压力。(3)能量丰富且持久。据科学报道，太阳每小时向地球辐射的能量远远超过人类生存一年所需全部能量的总和，太阳辐射到地球表面一年的能量相当于大约24000亿吨煤炭的能量。
太阳光与物质的相互作用可以归纳为光吸收和能量转化两个阶段。整个过程由物质本身的性质和光的波长决定的，只有在特定波长光的作用下物质内部的电子才能够发生跃迁，光才能够被吸收，其它波长范围内的太阳光则不会被吸收。太阳光的能量被物质吸收后，电子由基态跃迁至激发态，当电子再次回到基态时，会将多余的能量以特定的形式转化或释放。太阳光的光谱范围主要分布在200-2500nm之间，当物质内电子或分子的能级分布越多对于太阳光的吸收范围就越大(宽谱带吸收)，能级之间连续性越强就越容易发生非辐射跃迁，光热转化效果越明显。太阳能的光电转化只能利用太阳能的短波部分，而太阳能的光热转化几乎能够利用全波谱范围的太阳光，是太阳能转化效率最髙的一种能源转化方式。相对于复杂、昂贵而低效的光电转换系统，太阳能的光热应用无疑是人类利用太阳能最简单、最直接、最有效的途径之一。如何将低品位、分散不连续的太阳能转换成高品位的热能，以便最大限度地利用太阳能，成为突破太阳能光热应用的关键瓶颈。要实现这种太阳能光热应用的关键就是研制高效稳定的光热转换材料。
石墨烯具有优异的宽频吸收能力，成为了一个具有应用前景的太阳能光热转换应用的材料。碳基体材料因其价格低廉，制备工艺简单，引起人们广泛关注。石墨烯作为一种新型碳家族层状结构材料，层与层之间靠相对较弱的范德华力连接，单层之间化学键连接，本身具有一定的强度，又有一定的柔性，通常复合一些高聚物，形成石墨烯纳米复合材料。石墨烯由于其具有连续的能级，带隙宽度为零，同时石墨烯内有大量的自由载流子，理论上能够对太阳光实现全谱范围的吸收。石墨烯由于具有良好的红外光吸收、导热性和结构稳定性等优点，在光热转化材料的研究中显示出极大的优势。
但石墨烯由于对光的反射比较强，需要构建具有一定层次的纳米结构，如阵列多孔或分级多孔结构使光在材料内多次反射，增强对光的吸收。制备3D多孔石墨烯材料可实现太阳光在石墨烯孔内的多次反射，但目前常见的3D石墨烯生产方法存在许多不足之处，还不能实现大规模应用。如已经报道的有，三维的多孔石墨烯片通过化学气相沉积法应用在制备太阳能蒸汽，但是，制备过程比较复杂，这可能会限制材料在实际生活中的应用。其他制备三维石墨烯的方法如水热法，这种方法通常由于反应容器的限制，制备出来的气凝胶面积比较小。所以急需一种低成本、高吸收太阳光以及多孔的3D石墨烯被制备出来并用于太阳能高效的光热转换。
地膜覆盖技术是用塑料薄膜把适播农田从地面上封盖起来，造成不同于露地栽培的农田土壤环境，通过增温、保墒、蓄水、防旱及保持土壤疏松，在一定程度上抑制杂草生长、压碱、促进作物根系发育，从而促进作物增产和改善作物品质，进而提高种植效益。
发明内容
本发明的目的在于提供一种快速制备石墨烯三明治型光热转换地膜的方法，其是先使用高能束流照射聚酰亚胺得到多孔石墨烯材料，紧接着采用热辊压方式制备热塑性聚合物-石墨烯-热塑性聚合物的石墨烯三明治型光热转换地膜。
在本发明中，聚酰亚胺在激光的瞬时高温中快速碳化并结晶生长获得高质量的石墨烯，石墨烯为少数片层结构的堆叠，结晶性好，导电性高，有利于在太阳光照时更高效地发挥光热转换作用。
在本发明中，激光的瞬时高温作用使得聚酰亚胺材料中大量气体快速的释放，因此获得的石墨烯具有丰富的3D多孔结构，所以能够实现太阳光在石墨烯多孔结构中能够多次反射、多次吸收，克服石墨烯的光吸收能力。高能束流为激光束、电子束、离子束中的一种或多种的组合照射；优选红外激光束；更优选择以CO2红外激光为例的高能束流，激光波长10.6μm，功率4-10W，脉冲频率5-20kHz，激光扫描速度200-400mm/s；优选的，激光功率为5W，脉冲频率20kHz，激光扫描速度200mm/s。光斑大小80-200μm。
在本发明中，聚合物-石墨烯-聚合物三明治型的光热转换地膜可以有效避免石墨烯粉末材料在聚合物中难以均匀分散的问题，这种结构也能有效增加石墨烯在聚合物中的负载量，可以更进一步提高表面系统的温度。
本发明提出的3D多孔石墨烯地膜，将石墨烯制备和复合材料成膜集成到一个步骤中，制备速度快、成本低，得益于石墨烯的多孔结构，能在现有的地膜技术上进一步提高温度，将会进一步推动地膜的实际应用。
该石墨烯基复合地膜使用近年来最新发展的高能束流高效制备石墨烯技术实现高质量、3D多孔石墨烯的制备，并利用热压技术实现聚合物-石墨烯-聚合物三明治型地膜的成膜，真正将高光热转换效率的石墨烯材料制备和复合材料膜生产集成到一个步骤中(如图1所示)。其中，石墨烯高的光吸收性能赋予了地膜全光谱吸收能力，可以实现高效的光热转换；主要的成膜材料使用热塑性的聚合物，通过热辊压实现复合材料的成膜。本发明中的石墨烯制备方法速度快、成本低，所得石墨烯质量高光热转换效率高，并且易于实现工业化的卷对卷生产，在光热转换薄膜制备等领域有很大的应用前景。
附图说明
图1是聚合物-石墨烯-聚合物三明治型的光热转换地膜的制备工艺过程示意图。
图2是所制备的石墨烯的扫描电镜图。
图3是所制备的石墨烯的透射电镜图。
图4是所制备的石墨烯的拉曼谱图。
具体实施方式
为了使本发明的技术方案及技术优势更加清晰，以下对本发明内容进行进一步的详细说明。需要说明的是，下述实施例是对于本发明内容的进一步说明以作为对本发明技术内容的阐释，但本发明的实质内容并不仅限于下述实施例所述，本领域的普通技术人员可以且应当知晓任何基于本发明实质精神的简单变化或替换均应属于本发明所要求的保护范围。
实施例1
如图1所示，一种快速制备石墨烯三明治型光热转换地膜的方法，步骤如下；a.高能束流照射聚酰亚胺聚合物实现3D多孔石墨烯材料的快速制备
将聚酰亚胺薄膜暴露于二氧化碳激光的照射下，高能束流在聚合表面非常聚集的局部点上瞬时高温会使得聚酰亚胺迅速碳化，并且同时发生碳原子的重排和气体快速释放，最终便能在聚酰亚胺表面生成一层数十微米厚的3D多孔石墨烯；
b.热辊压技术实现聚合物-石墨烯-聚合物三明治型地膜的成膜制备
在获得的聚酰亚胺支撑的石墨烯膜上覆盖一层聚乙烯薄膜，在热辊压的作用下实现石墨烯从聚酰亚胺上的剥离，实现石墨烯到聚乙烯薄膜上的转移，接着在卷对卷的过程中，下一步的热辊压过程实现聚乙烯-石墨烯-聚乙烯复合材料的成膜。所制得的石墨烯复合地膜，其中石墨烯的厚度约为30μm；单层聚乙烯的厚度为100μm；石墨烯三明治型光热转换地膜厚度约为200μm。石墨烯复合材料地膜宽幅为0.5m-5m均可，长度任意。
在步骤a中，CO2激光为例的高能束流，激光波长10.6μm，激光使用功率为5W，脉冲频率20kHz，激光扫描速度200mm/s。光斑大小约为100μm。
如图2所示，获得的石墨烯材料为蜂窝多孔的结构，石墨烯的孔径约为1μm-3μm，这种多孔石墨烯结构的形成有利于太阳光在石墨烯孔内的多次反射，使得石墨烯孔壁多次对红外光进行吸收，可有效提高光热转换效率。
如图3所示，此图为激光诱导石墨烯的透射电子显微镜图像，可以看出石墨烯的为很薄的碳层结构，是少数石墨烯片层的堆叠，具有较好的结晶质量。
如图4所示，此图为激光照射聚酰亚胺获得的石墨烯拉曼谱图，在拉曼位移分别为1350cm-1，1580cm-1和2700cm-1分别出现了石墨烯特征的D、G和2D峰。单独而尖锐的2D洛伦兹峰，可以明显区别于无定型碳等结晶质量地的碳材料。
在步骤b中，选择聚乙烯(PE)作为热塑性聚合物用以制备地膜较佳，热辊压时选择160℃的温度更佳，为防止热塑性塑料熔化到滚轮上，可使用热固性PET套管包裹金属滚轮。
实施例2
一种快速制备石墨烯三明治型光热转换地膜的方法，步骤如下；
a.高能束流照射聚酰亚胺聚合物实现3D多孔石墨烯材料的快速制备
将聚酰亚胺薄膜暴露于二氧化碳激光的照射下，高能束流在聚合表面非常聚集的局部点上瞬时高温会使得聚酰亚胺迅速碳化，并且同时发生碳原子的重排和气体快速释放，最终便能在聚酰亚胺表面生成一层数十微米厚的3D多孔石墨烯；CO2激光为例的高能束流，激光波长10.6μm，激光使用功率为8W，脉冲频率15kHz，激光扫描速度300mm/s。光斑大小约为100μm。
b.热辊压技术实现聚合物-石墨烯-聚合物三明治型地膜的成膜制备
在获得的聚酰亚胺支撑的石墨烯膜上覆盖一层聚乙烯薄膜，在160℃热辊压下实现石墨烯从聚酰亚胺上的剥离以及石墨烯到聚乙烯薄膜上的转移，接着在卷对卷的过程中，下一步的热辊压过程实现聚乙烯-石墨烯-聚乙烯复合材料的成膜。所制得的石墨烯复合地膜，其中石墨烯的厚度约为32μm；单层聚乙烯的厚度为80μm；石墨烯三明治型光热转换地膜厚度约为250μm。石墨烯复合材料地膜宽幅为0.5m-5m均可，长度任意。
实施例3
一种快速制备石墨烯三明治型光热转换地膜的方法，步骤如下；
a.高能束流照射聚酰亚胺聚合物实现3D多孔石墨烯材料的快速制备
将聚酰亚胺薄膜暴露于二氧化碳激光的照射下，高能束流在聚合表面非常聚集的局部点上瞬时高温会使得聚酰亚胺迅速碳化，并且同时发生碳原子的重排和气体快速释放，最终便能在聚酰亚胺表面生成一层数十微米厚的3D多孔石墨烯；CO2激光为例的高能束流，激光波长10.6μm，激光使用功率为6W，脉冲频率10kHz，激光扫描速度200mm/s。光斑大小约为100μm。
b.热辊压技术实现聚合物-石墨烯-聚合物三明治型地膜的成膜制备
在获得的聚酰亚胺支撑的石墨烯膜上覆盖一层聚乙烯薄膜，在160℃热辊压下实现石墨烯从聚酰亚胺上的剥离以及石墨烯到聚乙烯薄膜上的转移，接着在卷对卷的过程中，下一步的热辊压过程实现聚乙烯-石墨烯-聚乙烯复合材料的成膜。所制得的石墨烯复合地膜，其中石墨烯的厚度约为35μm；单层聚乙烯的厚度为100μm；石墨烯三明治型光热转换地膜厚度约为280μm。石墨烯复合材料地膜宽幅为0.5m-5m均可，长度任意。
应当说明的是，本发明的上述所述之技术内容仅为使本领域技术人员能够获知本发明技术实质而进行的解释与阐明，故所述之技术内容并非用以限制本发明的实质保护范围。本发明的实质保护范围应以权利要求书所述之为准。本领域技术人员应当知晓，凡基于本发明的实质精神所作出的任何修改、等同替换和改进等，均应在本发明的实质保护范围之内。

Claims (8)

1.一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，先使用高能束流照射聚酰亚胺得到多孔石墨烯材料，紧接着采用热辊压方式制备热塑性聚合物-石墨烯-热塑性聚合物的石墨烯三明治型光热转换地膜。
2.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，所述高能束流为激光束、电子束、离子束中的一种或多种的组合照射；优选红外激光束。
3.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，选择以CO2红外激光为例的高能束流，激光波长10.6μm，功率4-10W，脉冲频率5-20kHz，激光扫描速度200-400mm/s；优选的，激光功率为5W，脉冲频率20kHz，激光扫描速度200mm/s。
4.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，所述多孔石墨烯中石墨烯的孔径为10nm至10μm。
5.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，所述热辊压温度在100-180℃范围内。
6.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，所述多孔石墨烯的厚度为20-50μm；所述热塑性聚合物的厚度为50-150μm；石墨烯三明治型光热转换地膜厚度为100-400μm。
7.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，所述热塑性聚合物为聚乙烯、聚氯乙烯、聚苯乙烯、聚丙烯中的一种或几种的组合。
8.如权利要求1所述的一种快速制备石墨烯三明治型光热转换地膜的方法，其特征在于，包括下述步骤：
a.高能束流照射聚酰亚胺制备多孔石墨烯材料
将聚酰亚胺薄膜暴露于CO2激光的高能束流照射下，聚酰亚胺在高能束流的瞬时高温下迅速碳化，从而在聚酰亚胺表面生成聚酰亚胺支撑的多孔石墨烯；激光波长10.6μm，激光功率为5W，脉冲频率20kHz，激光扫描速度200mm/s；
b.热辊压制备聚乙烯-石墨烯-聚乙烯三明治型地膜
在获得的聚酰亚胺支撑的石墨烯膜上覆盖一层热塑性聚合物薄膜，在热辊压的作用下石墨烯从聚酰亚胺上的剥离并转移到热塑性聚合物薄膜上，接着在卷对卷的过程中，进一步的热辊压得到热塑性聚合物-石墨烯-热塑性聚合物三明治型地膜；热辊压温度在100-180℃。
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CN107739027A (zh) * 2017-10-27 2018-02-27 清华大学深圳研究生院 一种连续制备多孔石墨烯薄膜的方法及装置
CN109712742A (zh) * 2018-12-17 2019-05-03 中国科学院合肥物质科学研究院 一种具有高导电能力的石墨烯晶体薄膜及其制备方法
CN109440145A (zh) * 2018-12-30 2019-03-08 苏州碳素集电新材料有限公司 一种石墨烯/铜复合导电材料及其制备方法
CN109686501A (zh) * 2018-12-30 2019-04-26 苏州碳素集电新材料有限公司 一种石墨烯/铝复合导电材料及其制备方法
CN110253988A (zh) * 2019-06-04 2019-09-20 深圳先进技术研究院 一种具有电磁屏蔽功能的聚合物膜及其制备方法
CN112964380A (zh) * 2021-03-22 2021-06-15 浙江大学 一种基于激光加工法的柔性温度传感器的制备方法

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CN115819824A (zh) * 2022-12-27 2023-03-21 中科合肥智慧农业协同创新研究院 一种石墨烯/聚酰亚胺渗水地膜及其制备方法
CN115819824B (zh) * 2022-12-27 2024-05-28 中科合肥智慧农业协同创新研究院 一种石墨烯/聚酰亚胺渗水地膜及其制备方法

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