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CN102391618A - Preparation method of alignment carbon nano tube/polymer composite membrane - Google Patents

Preparation method of alignment carbon nano tube/polymer composite membrane Download PDF

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CN102391618A
CN102391618A CN201110229604XA CN201110229604A CN102391618A CN 102391618 A CN102391618 A CN 102391618A CN 201110229604X A CN201110229604X A CN 201110229604XA CN 201110229604 A CN201110229604 A CN 201110229604A CN 102391618 A CN102391618 A CN 102391618A
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carbon nanotube
density
preparation
composite film
film
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彭慧胜
黄三庆
仰志斌
李立
张玲莉
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Fudan University
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Abstract

本发明属于碳纳米管薄膜制备技术领域，具体为一种取向碳纳米管/聚合物复合膜的制备方法。本发明采用切片法，制备得取向良好的碳纳米管/聚合物复合膜，该薄膜中碳纳米管平行于薄膜表面，均匀分布，使薄膜表面具有极佳的导电性能。同时，该复合膜的厚度和密度均可控：采用切片机对薄膜厚度在较宽范围内进行精确控制；复合膜中碳纳米管的密度可通过改变碳纳米管阵列的合成条件或压缩碳纳米阵列的体积来实现。所制备的复合膜具有较高的透光率、优异的柔韧性和变形能力。本发明操作简单、可控性好，所制备的复合膜可作为优良的透明、柔性电极取代传统导电玻璃用于多个领域。

Figure 201110229604

The invention belongs to the technical field of carbon nanotube film preparation, in particular to a preparation method of an aligned carbon nanotube/polymer composite film. The invention adopts a slicing method to prepare a well-oriented carbon nanotube/polymer composite film. In the film, the carbon nanotubes are parallel to the surface of the film and uniformly distributed, so that the surface of the film has excellent electrical conductivity. At the same time, the thickness and density of the composite film can be controlled: a slicer is used to precisely control the thickness of the film in a wide range; the density of carbon nanotubes in the composite film can be adjusted by changing the synthesis conditions of the carbon nanotube array or compressing the carbon nanotubes The volume of the array is implemented. The prepared composite film has high light transmittance, excellent flexibility and deformation ability. The invention has simple operation and good controllability, and the prepared composite film can be used as an excellent transparent and flexible electrode to replace traditional conductive glass and be used in multiple fields.

Figure 201110229604

Description

A kind of preparation method of aligned carbon nanotube/composite membrane of polymer
Technical field
The invention belongs to the carbon nano-tube film preparing technical field, be specially a kind of preparation method of aligned carbon nanotube/composite membrane of polymer.
Background technology
Transparent and flexible electro-conductive material has in the preparation of new devices such as Foldable display screen, flexible solar battery and thin film transistor extremely widely to be used 1-2Traditional preparation method is with the adulterated In of Sn 2O 3(ITO) deposit on the flexible substrates.Since ITO resource-constrained, preparation condition are harsh and rigidity greatly, not acidproof 3, therefore, be badly in need of working out the novel equivalent material that can satisfy requirements at the higher level at present.
In recent years, the research of carbon nanotube (CNT)/composite membrane of polymer causes great concern 4-5This is because CNTs has superior mechanical property and electric property; And polymkeric substance can provide good flexible and transparent.Seek out all carbon nano-tube/polymer composite film materials preferably of the transparency, flexibility and electroconductibility, a kind of simple effective method is exactly directly to utilize the carbon nano pipe array of orientation to prepare composite package.For example there is report to adopt CNT sheet (CNT sheet) to prepare the CNT/ composite membrane of polymer 6Since in the CNT sheet that can prepare at present CNTs length be 1 mm, electric charge can only conduct through front and back adjacent C NTs in the film, the big limitations of its contact resistance the raising of composite package specific conductivity.Therefore; The present invention adopts section method to prepare aligned carbon nanotube/composite membrane of polymer; Through regulating the method for slicing machine parameter and compressed carbon nano-tube array, realized that the prepared composite film has good electrical conductivity, the transparency and flexible to the thickness of composite package and effective control of density.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with excellent conductive capability, flexibility and transparent aligned carbon nanotube/composite membrane of polymer.
The preparation method of aligned carbon nanotube/composite membrane of polymer that the present invention proposes, concrete steps are following:
The first, preparation carbon nano pipe array/polymkeric substance composite block
Carbon nano pipe array is immersed in polymkeric substance performed polymer, monomer, fused solution or the solution, adopt situ aggregation method, melting and solidification method or solution to volatilize method, under the situation that does not change the carbon nanotube orientation, obtain the composite block of polymkeric substance and carbon nano pipe array;
The second, carbon nano pipe array/polymkeric substance composite block is cut into slices
Carbon nano pipe array/polymkeric substance composite block is fixed on the slicing machine, makes blade plane parallel with the carbon nanotube orientation, cut into slices, being prepared into thickness range is the parallel-oriented carbon nano-tube/polymer composite package of 50 nm ~ 50 μ m.
The composite package of the present invention's preparation, wherein carbon nanotube is parallel to film surface, and uniform distribution makes film surface have splendid conductivity.
The parallel-oriented carbon nano-tube/polymer composite package of the present invention preparation, its thickness and density are to certain influence that has of the specific conductivity of film and light transmission.Therefore, suitably control the thickness and the density of composite package.
1, about the control of composite package thickness
The composite package thickness range is 50 nm ~ 50 μ m, and its concrete thickness can be through regulating the slicing machine parameter or using different slicing machines to control.
2, about the control of composite package density
The control of composite package density mainly is the density control to carbon nano pipe array.The carbon nano pipe array that uses among the present invention can adopt chemical Vapor deposition process synthetic.The density control method of this carbon nano pipe array is following:
The first, control through the synthesis condition that changes carbon nano pipe array, adopting structure such as the catalyzer when the synthesizing carbon nanotubes array is Si/SiO 2/ Al 2O 3During the matrix material of/Fe, the thickness range of Fe can be controlled in 0.5-3 nm, Al 2O 3The thickness range of layer is 0.5 ~ 30 nm.The flow range of ethene, argon gas, hydrogen is respectively 60-290 sccm, 400-620 sccm and 20-48 sccm.Temperature of reaction and reaction time range were respectively 500 ~ 900 ℃, 5 ~ 100 minutes.The height of the carbon nano pipe array of preparation can be 0.5 ~ 5 millimeter, and density range is 10 10~ 10 11Cm -2
The second, be the power of 10 ~ 100 N through the carbon nano pipe array both sides being applied pair of vertical in the size of carbon nanotube orientation, carbon nano pipe array increases because of smaller volume density, and the variation range of its density is 1 ~ 100 times.Thereby can further the density of carbon nano pipe array be brought up to 10 10~ 10 13Cm -2
The inventive method is prepared into parallel-oriented carbon nano-tube/polymer composite package, and has realized the height control to film thickness and density, thereby has realized the effective regulation and control to the specific conductivity and the light transmission of film.
Among the present invention, using density is 10 10~ 10 13Cm -2Carbon nano pipe array, can be prepared into density is 10 10~ 10 13Cm -2The carbon nano-tube/polymer composite package; The composite package gauge control is 50 nm ~ 50 μ m.Then the transmittance of this composite package is 95 ~ 0%, and specific conductivity is 10 2~ 10 3S/cm.In addition, this composite package has excellent flexibility and deformability.This composite package is used for the counter electrode of solar cell, and prepared cell demonstrates good performance.The characteristics that the present invention has is simple to operate, controllability is good, the prepared thickness and the aligned carbon nanotube/composite membrane of polymer of controllable density are expected to replace conventional conductive glass as good transparent, flexible electrode and are used for a plurality of fields.
Description of drawings
Fig. 1, wherein, a, b are respectively the stereoscan photograph and the transmission electron microscope photo of the low density orientation CNT/ epoxy resin composite membrane of uncompressed, and c, d are respectively the high power and the low power stereoscan photograph of the high-density orientation CNT/ epoxy resin composite membrane after compressing 4 times.
Fig. 2, wherein, a is the photo of orientation CNT/ epoxy resin composite membrane in deformation process, b is the light transmission photo of the orientation CNT/ epoxy resin composite membrane of different thickness on the sheet glass.
Fig. 3; Wherein, A; B is respectively that orientation CNT/ epoxy resin composite membrane is parallel to the carbon nanotube direction on the film surface and at the resistance on two surfaces up and down of the film change curve with angle of bend, c, d be respectively that composite package is parallel to the carbon nanotube direction on the film surface and at the resistance on two surfaces up and down of film with crooked (0 ~ 180 o) change curve of cycle index.
Fig. 4 illustrates for flow process of the present invention.
Embodiment
The detailed process of preparation is following:
The first, aligned carbon nanotube array synthetic.
Chemical Vapor deposition process is adopted in the preparation of carbon nano pipe array.At first on silicon chip, successively deposit one deck Al through the electron beam evaporation deposition appearance 2O 3With one deck Fe, obtaining structure is Si/SiO 2/ Al 2O 3The catalyzer of (0.5 ~ 30 nm)/Fe (0.5 ~ 3 nm).Then catalyzer is put into tube furnace; And feed hydrogen, argon gas; Then temperature was elevated to 500 ~ 900 ℃ and constant temperature 0.5 ~ 5 minute, treats to feed carbon source ethene after the catalyzer slaking, the therein ethylene flow is 60-290 sccm; Argon flow amount is 400-620 sccm, and hydrogen flowing quantity is 20-48 sccm.Continuation constant temperature can grow on silicon chip after 5 ~ 100 minutes and highly be 0.5 ~ 5 millimeter, and density is 10 10~ 10 11Cm -2Carbon nano pipe array, carbon nanotube is height-oriented in this array, and purity is high, decolorizing carbon is less.
The second, the compressed carbon nano-tube array.
Through the carbon nano pipe array both sides are applied pair of vertical in carbon nanotube orientation, size is the power of 10 ~ 100 N, carbon nano pipe array original because of the compression volume becomes 1 ~ 1/100, density is increased to 1 ~ 100 times before the compression.
The 3rd, the preparation of carbon nano pipe array/epoxy resin composite block
The preparation of embedding stoste: the prescription that embedding is used is classical " EPON 812 " prescription, and the present invention fills a prescription with this and is the basis, has increased an amount of toughner.The method of concrete preparation is: at first, and configuration solution A and solution B.A liquid by epoxy resin (SPI-Pon 812) and dodecenylsuccinic acid acid anhydride (DDSA) by volume the ratio of 62:100 form; B liquid is made up of epoxy resin (SPI-Pon 812) and 100: 89 by volume ratio of methyl carbic anhydride (NMA).A liquid for preparing and B liquid made homodisperse in ultrasonic 10-30 minute in the ultrasonic cleaning machine the inside.Toughner is the DT-2 type that chemical institute is bought from the southeast, Shenyang City.(A liquid: the volume ratio of B liquid=2:8) is mixed with 2:8 with A liquid and B liquid then; The toughner that adds A liquid and B liquid TV 10% then; 1%～2% curing catalyst 2,4,6 three (dimethylamino methyl) phenol (DMP-30) that adds TV at last; Ultrasonic 10-30 minute, thorough mixing.Obtain embedding stoste at last.
The infiltration of epoxy resin: at first join reagent 1; Reagent 2; Reagent 3 and reagent 4. reagent 1 are according to acetone: the ratio preparation of embedding stoste (volume ratio)=10:1 to 2:1; Reagent 2 is according to acetone: the ratio preparation of embedding stoste (volume ratio)=2:1 to 1:2, reagent 3 are according to acetone: the ratio preparation of embedding stoste (volume ratio)=1:2 to 1:10, reagent 4 is pure embedding stoste.Then carbon nano pipe array is immersed in the reagent 1, soaked 3-24 hour, be transferred to then in the reagent 2, soaked 3-24 hour, then be transferred in the reagent 3, soaked 3-24 hour, be transferred at last in the reagent 4, soaked 12-36 hour.
Embedding is solidified: put into the mould that oneself needs the embedding shape to the sample that in reagent 4, soaked 24 hours, inject embedding stoste then, 60 degrees centigrade of curing 36 hours under the normal pressure can obtain with the good carbon nano pipe array of epoxy resin embedding in the polymerization case.
The 4th, carbon nano pipe array/epoxy resin composite block is cut into slices.
Carbon nano pipe array/epoxy resin composite block is repaired, used Lycra ultramicrotome or semithin section machine to cut into slices then, obtain the carbon nano-tube/polymer composite package of different thickness.The thickness range of section is 50 nanometers to 100 micron.
The structure of composite package characterizes through transmitted electron Electronic Speculum (TEM, JEOL JEM-2100F operating voltage 200 kV) and sem (SEM, Hitachi FE-SEM S-4800 operating voltage 1 kV).
Reference
[1] Rogers,?J.?A.,?Someya,?T.,?Huang,?Y.?G.?Science?2010,?327(5973):1603.
[2] Baca,?A.?J.,?Ahn,?J.?H.,?Sun,?Y.?G.,?Meitl,?M.?A.,?Menard,?E.,?Kim,?H.?S.,?Choi,?W.?M.,?Kim,?D.?H.,?Huang,?Y.,?Rogers,?J.?A.?Angewandte?Chemie-International?Edition?2008,?47(30):?5524.
[3] Huang,?Y.?Y.,?Terentjev,?E.?M.?Acs?Nano?2011,?5(3):?2082.
[4] Hu,?L.?B.,?Hecht,?D.?S.,?Gruner,?G.?Chemical?Reviews?2010,?110(10):?5790.
[5] Hecht,?D.?S.,?Hu,?L.?B.,?Irvin,?G.?Advanced?Materials?2011,?23(13):?1482.
[6]?Peng,?H.?S.?Journal?of?the?American?Chemical?Society?2008,?130(1):?42.。

Claims (3)

1.一种取向碳纳米管/聚合物复合膜的制备方法，其特征在于具体步骤如下： 1. a preparation method of oriented carbon nanotube/polymer composite film, is characterized in that concrete steps are as follows: 第一，制备碳纳米管阵列/聚合物复合块体 First, the preparation of carbon nanotube array/polymer composite bulk 将碳纳米管阵列浸入聚合物预聚体、单体、熔融液或溶液中，采用原位聚合法、熔融固化法或溶液挥干法，在不改变碳纳米管取向的情况下得到聚合物与碳纳米管阵列的复合块体； The carbon nanotube array is immersed in the polymer prepolymer, monomer, melt or solution, and the polymer and Composite blocks of carbon nanotube arrays; 第二，对碳纳米管阵列/聚合物复合块体进行切片 Second, slice the CNT array/polymer composite bulk 将碳纳米管阵列/聚合物复合块体固定在切片机上，使刀片平面与碳纳米管取向平行，进行切片，制备得厚度范围为50 nm~50 μm的平行取向的碳纳米管/聚合物复合膜。 Fix the carbon nanotube array/polymer composite block on a microtome, make the blade plane parallel to the carbon nanotube orientation, and slice it to prepare a parallel-oriented carbon nanotube/polymer composite with a thickness ranging from 50 nm to 50 μm. membrane. 2.根据权利要求1所述的取向碳纳米管/聚合物复合膜的制备方法，其特征在于 2. the preparation method of aligned carbon nanotube/polymer composite film according to claim 1, is characterized in that 所述复合膜的具体厚度，通过调节切片机参数或使用不同的切片机来控制。 The specific thickness of the composite film is controlled by adjusting the slicer parameters or using different slicers. 3.根据权利要求1所述的取向碳纳米管/聚合物复合膜的制备方法，其特征在于 3. the preparation method of aligned carbon nanotube/polymer composite film according to claim 1, is characterized in that 通过控制碳纳米管阵列密度来控制复合膜密度，所述碳纳米管阵列采用化学气相沉积法合成，其密度控制方法如下：  The density of the composite film is controlled by controlling the density of the carbon nanotube array. The carbon nanotube array is synthesized by chemical vapor deposition, and the density control method is as follows: 第一、通过改变碳纳米管阵列的合成条件来控制，当合成碳纳米管阵列的催化剂采用结构为Si/SiO2/Al2O3/Fe的复合材料时，Fe的厚度范围控制在0.5-3 nm，Al2O3层的厚度范围为0.5~30 nm；乙烯、氩气、氢气的流量范围分别为60-290 sccm、400-620 sccm和20-48 sccm；反应温度和反应时间范围分别为500~900℃、5~100分钟；制备的碳纳米管阵列的高度可为0.5~5毫米，密度范围为1010~1011 cm-2； First, it is controlled by changing the synthesis conditions of the carbon nanotube array. When the catalyst for the synthesis of the carbon nanotube array is a composite material with a structure of Si/SiO 2 /Al 2 O 3 /Fe, the thickness range of Fe is controlled within 0.5- 3 nm, the thickness of the Al 2 O 3 layer ranges from 0.5 to 30 nm; the flow ranges of ethylene, argon and hydrogen are 60-290 sccm, 400-620 sccm and 20-48 sccm respectively; the reaction temperature and reaction time ranges are respectively 500~900°C, 5~100 minutes; the height of the prepared carbon nanotube array can be 0.5~5 mm, and the density range is 10 10 ~10 11 cm -2 ; 第二、通过对碳纳米管阵列两侧施加一对垂直于碳纳米管取向的大小为10~100 N的力，碳纳米管阵列因体积变小而密度增加，其密度的变化范围为1~100倍，从而进一步将碳纳米管阵列的密度提高到1010 ~1013 cm-2。 Second, by applying a pair of 10-100 N forces perpendicular to the orientation of the carbon nanotubes on both sides of the carbon nanotube array, the density of the carbon nanotube array increases due to the decrease in volume, and the density ranges from 1 to 100 N. 100 times, thereby further increasing the density of the carbon nanotube array to 10 10 ~10 13 cm -2 .
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CN102731949A (en) * 2012-05-29 2012-10-17 复旦大学 Highly oriented carbon nano-tube/polymer composite film, and preparation method and application thereof
CN102774828A (en) * 2012-07-13 2012-11-14 复旦大学 Preparation method of controllable-dimension graphene nanobelts
CN103273661A (en) * 2013-06-27 2013-09-04 中国兵器工业集团第五三研究所 In-plane oriented carbon nano tube reinforced resin film and preparation method thereof
CN103964413A (en) * 2014-04-17 2014-08-06 北京大学 Method for improving carbon nano tube parallel array density
CN104600334A (en) * 2015-01-07 2015-05-06 复旦大学 Fiber-shaped electrochemical luminescence battery and preparation method thereof
CN106585061A (en) * 2016-12-06 2017-04-26 厦门世纳芯科技有限公司 High-quality quantum dot fluorescent thin-film material and preparation method thereof
CN109455693A (en) * 2018-12-07 2019-03-12 深圳烯湾科技有限公司 Modified carbon nano-tube array, carbon nano-tube fibre and its preparation method and application
CN110527296A (en) * 2018-05-24 2019-12-03 厦门大学 A kind of dynamic nano channel and its preparation, test method
CN111298666A (en) * 2020-03-16 2020-06-19 中国人民解放军火箭军工程设计研究院 Hollow fiber forward osmosis composite membrane containing oriented carbon nanotubes and preparation method thereof
CN113214603A (en) * 2021-05-12 2021-08-06 云南中烟工业有限责任公司 Carbon nanotube epoxy resin composite material electrode, preparation method and application thereof
CN119012673A (en) * 2024-10-25 2024-11-22 浙江绿色理想科技有限公司 Anti-radiation shielding type electrical control cabinet

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CN102731949A (en) * 2012-05-29 2012-10-17 复旦大学 Highly oriented carbon nano-tube/polymer composite film, and preparation method and application thereof
CN102731949B (en) * 2012-05-29 2014-07-09 复旦大学 Highly oriented carbon nano-tube/polymer composite film, and preparation method and application thereof
CN102774828A (en) * 2012-07-13 2012-11-14 复旦大学 Preparation method of controllable-dimension graphene nanobelts
CN103273661A (en) * 2013-06-27 2013-09-04 中国兵器工业集团第五三研究所 In-plane oriented carbon nano tube reinforced resin film and preparation method thereof
CN103964413B (en) * 2014-04-17 2016-04-27 北京大学 A kind of method improving carbon nanotube parallel array density
CN103964413A (en) * 2014-04-17 2014-08-06 北京大学 Method for improving carbon nano tube parallel array density
CN104600334A (en) * 2015-01-07 2015-05-06 复旦大学 Fiber-shaped electrochemical luminescence battery and preparation method thereof
CN106585061A (en) * 2016-12-06 2017-04-26 厦门世纳芯科技有限公司 High-quality quantum dot fluorescent thin-film material and preparation method thereof
CN110527296A (en) * 2018-05-24 2019-12-03 厦门大学 A kind of dynamic nano channel and its preparation, test method
CN110527296B (en) * 2018-05-24 2022-05-10 厦门大学 Dynamic nano-channel and preparation and test method thereof
CN109455693A (en) * 2018-12-07 2019-03-12 深圳烯湾科技有限公司 Modified carbon nano-tube array, carbon nano-tube fibre and its preparation method and application
CN111298666A (en) * 2020-03-16 2020-06-19 中国人民解放军火箭军工程设计研究院 Hollow fiber forward osmosis composite membrane containing oriented carbon nanotubes and preparation method thereof
CN113214603A (en) * 2021-05-12 2021-08-06 云南中烟工业有限责任公司 Carbon nanotube epoxy resin composite material electrode, preparation method and application thereof
CN119012673A (en) * 2024-10-25 2024-11-22 浙江绿色理想科技有限公司 Anti-radiation shielding type electrical control cabinet

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Application publication date: 20120328