CN105536585B - A kind of carbon nano tube dispersion method - Google Patents
A kind of carbon nano tube dispersion method Download PDFInfo
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- CN105536585B CN105536585B CN201510963821.XA CN201510963821A CN105536585B CN 105536585 B CN105536585 B CN 105536585B CN 201510963821 A CN201510963821 A CN 201510963821A CN 105536585 B CN105536585 B CN 105536585B
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Abstract
本发明公开了一种碳纳米管分散方法，属于新材料领域。工艺包括以下步骤：(1)将碳纳米管与粘合剂混合；(2)将混合物压制成电极；(3)用此电极与直流电源的负极相连，用金属等材质做电源正极电极；(4)将电源正、负极电极保持一定距离；(5)接通电源，使电路两电极间产生一定强度的电弧、等离子体、电火花等电致热源，在高温作用下，碳纳米管所吸收的粘合剂发生相变使碳纳米管得到有效分散。本发明的有益效果是，提供了一种分散效果明显且易实现规模化制备的碳纳米管分散方法。
The invention discloses a method for dispersing carbon nanotubes, which belongs to the field of new materials. The process includes the following steps: (1) mixing carbon nanotubes with a binder; (2) pressing the mixture into an electrode; (3) connecting the electrode to the negative pole of a DC power supply, and using metal or other materials as the positive electrode of the power supply; ( 4) Keep the positive and negative electrodes of the power supply at a certain distance; (5) Turn on the power supply to generate electric heat sources such as electric arcs, plasmas, and electric sparks of a certain intensity between the two electrodes of the circuit. Under the action of high temperature, the carbon nanotubes absorb The binder undergoes a phase change to effectively disperse the carbon nanotubes. The invention has the beneficial effects of providing a carbon nanotube dispersion method with obvious dispersion effect and easy realization of large-scale preparation.
Description
技术领域：Technical field:
本发明属于新材料领域，涉及一种碳纳米管的分散方法。The invention belongs to the field of new materials and relates to a method for dispersing carbon nanotubes.
背景技术：Background technique:
碳纳米管，是石墨片按照一定螺旋角卷曲而成的、直径为纳米级的管状物质。其有非常 大的长径比，沿着长度方向的热交换性能较好，而其垂直方向的热交换性能较低，利用其各 向异性通过合适的取向，可以获得具有优越导热性能的复合材料。但由于碳纳米管间具有较 强的范德华力，再加上其非常大的长径比，导致其在生产使用过程中极易发生团聚从而降低 其性能。而在使用时，往往要将碳纳米管的团聚体充分分散才能达到理想的使用效果。Carbon nanotubes are tubular substances with nanoscale diameters formed by curling graphite sheets according to a certain helical angle. It has a very large aspect ratio, and the heat exchange performance along the length direction is better, while the heat exchange performance in the vertical direction is lower. Using its anisotropy and proper orientation, composite materials with excellent thermal conductivity can be obtained . However, due to the strong van der Waals force between carbon nanotubes and its very large aspect ratio, it is easy to agglomerate during production and use, thereby reducing its performance. When in use, it is often necessary to fully disperse the aggregates of carbon nanotubes to achieve the ideal use effect.
碳纳米管的优异性能使其在军工、航天及民用生产企业有着广泛的应用前景，比如飞机 隐形材料的涂覆，航天材料中添加碳纳米管以增强其机械性能而且质量较轻，以及民用的一 些高分子橡胶材料，手机屏等材料的应用。但碳纳米管的团聚效应影响了其优异性能的发挥， 现阶段我国碳纳米管研究领域主要的分散手段包括研磨、超声波分散、强酸碱处理，但是这 些方法仅限于实验室研究阶段，大规模的生产分散好的碳纳米管至今还未有效的解决。欧美 等国对碳纳米管的研究要领先于我们，但是他们对于技术的封锁使我们无法获得有效分散的 方法，本申请所提出的一种碳纳米管的分散方法旨在寻求一种可大规模生产分散碳纳米管的 方法，打破发达国家对于分散碳纳米管方法的壁垒，为我国碳纳米管的研究出一份力，使碳 纳米管在军工、航天等领域能够广泛的应用。The excellent performance of carbon nanotubes makes it widely used in military, aerospace and civil production enterprises, such as the coating of aircraft stealth materials, adding carbon nanotubes to aerospace materials to enhance their mechanical properties and light weight, and civilian Application of some polymer rubber materials, mobile phone screens and other materials. However, the agglomeration effect of carbon nanotubes affects its excellent performance. At present, the main dispersion methods in the research field of carbon nanotubes in my country include grinding, ultrasonic dispersion, and strong acid-base treatment. However, these methods are limited to the laboratory research stage, and large-scale The production of dispersed carbon nanotubes has not been effectively solved so far. Europe and the United States and other countries are ahead of us in research on carbon nanotubes, but their blockade of technology prevents us from obtaining an effective dispersion method. A carbon nanotube dispersion method proposed in this application aims to seek a large-scale The method of producing dispersed carbon nanotubes breaks the barriers of developed countries to the method of dispersing carbon nanotubes, contributes to the research of carbon nanotubes in my country, and enables carbon nanotubes to be widely used in military, aerospace and other fields.
发明内容：Invention content:
针对上述现有分散技术的不足，本发明提供了一种分散更为彻底和快捷并可满足产业化 的碳纳米管分散方法。Aiming at the deficiencies of the above-mentioned existing dispersion technology, the present invention provides a carbon nanotube dispersion method which is more thorough and quicker and can satisfy industrialization.
本发明所采用的分散技术方案是：首先是配制用于分散的碳纳米管与粘合剂的混合物， 其配方为一定比例的碳纳米管和粘合剂。将纳米材料与粘合剂以一定比例混合，然后用机械 加压将混合物压制成一定形状的固态、半固态电极，用所制得的碳纳米管混合物电极与直流 电源的一极相连(以与电源负极相连为宜)，之后用石墨、金属等材质制成的电源另一极与碳 纳米管混合物组成的电极保持一定的微小距离。接通电源，接通电路使两电极间产生一定强 度的电弧、等离子体、电火花等电致热源，利用上述热源所产生的高温施加于碳纳米管混合 物电极表面，在高温作用下，碳纳米管所吸收的粘合剂发生相变，通过体积的迅速扩大以分 散碳纳米管团聚体。在上述热源附近由气流装置所产生气流将所分散在气相空间的碳纳米管 运输至除杂装置以脱去碳纳米管所附着的残余粘合剂，再由气流牵引至收集或是进一步加工 的区域。The dispersion technical solution adopted in the present invention is as follows: firstly, the mixture of carbon nanotubes and binder for dispersion is prepared, and the formula is a certain proportion of carbon nanotubes and binder. Mix nanomaterials and binders in a certain ratio, then use mechanical pressure to press the mixture into a solid and semi-solid electrode of a certain shape, and use the prepared carbon nanotube mixture electrode to connect with one pole of the DC power supply (to be connected with It is advisable that the negative pole of the power supply is connected), and then the other pole of the power supply made of materials such as graphite and metal and the electrode composed of the carbon nanotube mixture keep a certain small distance. Turn on the power supply and turn on the circuit to generate a certain intensity of electric heat sources such as arcs, plasmas, and electric sparks between the two electrodes. The high temperature generated by the above heat sources is applied to the surface of the carbon nanotube mixture electrode. Under the action of high temperature, the carbon nanotubes The binder absorbed by the tube undergoes a phase transition, which disperses the carbon nanotube aggregates through rapid volume expansion. The airflow generated by the airflow device near the above heat source transports the carbon nanotubes dispersed in the gas phase space to the impurity removal device to remove the residual binder attached to the carbon nanotubes, and then is drawn by the airflow to the collection or further processing area.
其制备工艺包括以下步骤：Its preparation process comprises the following steps:
(1)将准备分散的碳纳米管与一定比例的粘合剂中的一种或几种均匀混合，混合比例以 使最终均匀混合物成结块状形貌为宜；(1) uniformly mixing the carbon nanotubes to be dispersed with one or more of the binders in a certain proportion, the mixing ratio is advisable to make the final homogeneous mixture into an agglomerated morphology;
(2)通过机械挤压等方法将所得均匀混合物压制成具有一定形貌的固态或半固态电极；(2) Press the obtained homogeneous mixture into a solid or semi-solid electrode with a certain shape by mechanical extrusion or other methods;
(3)用此电极与直流电源的负极相连，用石墨、金属等材质制成的电极与直流电源的正 极相连；(3) Connect this electrode to the negative pole of the DC power supply, and connect the electrode made of graphite, metal and other materials to the positive pole of the DC power supply;
(4)将步骤(3)所述相连有直流电源正、负极的电极保持一定的距离；(4) Keep a certain distance from the electrodes connected with the positive and negative poles of the DC power supply described in step (3);
(5)接通电源，使电路两电极间产生一定强度的电弧、等离子体、电火花等电致热源， 利用该热源所产生的高温施加于碳纳米管混合物电极表面，在高温作用下，碳纳米管所吸收 的粘合剂发生相变，体积迅速扩大使碳纳米管得到有效分散；(5) Turn on the power supply, so that electric heat sources such as electric arcs, plasmas, and electric sparks of a certain intensity are generated between the two electrodes of the circuit, and the high temperature generated by the heat source is applied to the surface of the carbon nanotube mixture electrode. The binder absorbed by the nanotubes undergoes a phase change, and the volume rapidly expands to effectively disperse the carbon nanotubes;
(6)在步骤(5)所述电致热源附近由气流装置所产生气流将所分散在气相空间的碳纳 米管运输至除杂装置以脱去碳纳米管所附着的残余粘合剂；(6) The carbon nanotubes dispersed in the gas phase space are transported to the impurity removal device by the airflow generated by the airflow device near the electric heat source described in step (5) to remove the residual adhesive attached by the carbon nanotubes;
(7)通过由气流牵引所分散的碳纳米管至收集或是进一步加工的区域。(7) By dragging the dispersed carbon nanotubes to the collection or further processing area by the airflow.
本发明的有益效果是，提供了一种分散效果明显且可实现规模化制备的碳纳米管分散方 法。The beneficial effect of the present invention is that it provides a carbon nanotube dispersion method which has obvious dispersion effect and can realize large-scale preparation.
附图说明：Description of drawings:
附图1是本发明的生产工艺流程图。Accompanying drawing 1 is production process flowchart of the present invention.
具体实施方式：Detailed ways:
下面结合附图1对本发明做进一步说明，具体的实施方法：The present invention will be further described below in conjunction with accompanying drawing 1, concrete implementation method:
本发明提供了一种分散效果明显且可实现规模化制备的碳纳米管分散方法。首先是配置 用于分散的碳纳米管与粘合剂的混合物，其配方为一定比例的碳纳米管和粘合剂。将纳米材 料与粘合剂以一定比例混合，然后用机械加压将混合物压制成一定形状的固态、半固态电极， 用所制得的碳纳米管混合物电极与直流电源的一极相连(以与电源负极相连为宜)，之后用石 墨、金属等材质制成的电源另一极与碳纳米管混合物组成的电极保持一定的微小距离。接通 电源，接通电路使两电极间产生一定强度的电弧、等离子体、电火花等电致热源，利用上述 热源所产生的高温施加于碳纳米管混合物电极表面，在高温作用下，碳纳米管所吸收的粘合 剂发生相变，通过体积的迅速扩大以分散碳纳米管团聚体。在上述热源附近由气流装置所产 生气流将所分散在气相空间的碳纳米管运输至除杂装置以脱去碳纳米管所附着的残余粘合 剂，再由气流牵引至收集或是进一步加工的区域。其制备工艺包括以下步骤：The invention provides a carbon nanotube dispersion method with obvious dispersion effect and large-scale preparation. The first is to configure the mixture of carbon nanotubes and binder for dispersion, and its formula is a certain proportion of carbon nanotubes and binder. Mix nanomaterials and binders in a certain ratio, then use mechanical pressure to press the mixture into a solid and semi-solid electrode of a certain shape, and use the prepared carbon nanotube mixture electrode to connect with one pole of the DC power supply (to be connected with It is advisable that the negative pole of the power supply is connected), and then the other pole of the power supply made of materials such as graphite and metal and the electrode composed of the carbon nanotube mixture keep a certain small distance. Turn on the power supply and turn on the circuit to generate a certain intensity of electric heat sources such as arcs, plasmas, and electric sparks between the two electrodes. The high temperature generated by the above heat sources is applied to the surface of the carbon nanotube mixture electrode. Under the action of high temperature, the carbon nanotubes The binder absorbed by the tube undergoes a phase transition, which disperses the carbon nanotube aggregates through rapid volume expansion. The airflow generated by the airflow device near the above heat source transports the carbon nanotubes dispersed in the gas phase space to the impurity removal device to remove the residual binder attached to the carbon nanotubes, and then is drawn by the airflow to the collection or further processing area. Its preparation process comprises the following steps:
(1)将准备分散的碳纳米管与一定比例的粘合剂中的一种或几种均匀混合，混合比例以 使最终均匀混合物成结块状形貌为宜；(1) uniformly mixing the carbon nanotubes to be dispersed with one or more of the binders in a certain proportion, the mixing ratio is advisable to make the final homogeneous mixture into an agglomerated morphology;
(2)通过机械挤压等方法将所得均匀混合物压制成具有一定形貌的固态或半固态电极；(2) Press the obtained homogeneous mixture into a solid or semi-solid electrode with a certain shape by mechanical extrusion or other methods;
(3)用此电极与直流电源的负极相连，用石墨、金属等材质制成的电极与直流电源的正 极相连；(3) Connect this electrode to the negative pole of the DC power supply, and connect the electrode made of graphite, metal and other materials to the positive pole of the DC power supply;
(4)将步骤(3)所述相连有直流电源正、负极的电极保持一定的距离；(4) Keep a certain distance from the electrodes connected with the positive and negative poles of the DC power supply described in step (3);
(5)接通电源，使电路两电极间产生一定强度的电弧、等离子体、电火花等电致热源， 利用该热源所产生的高温施加于碳纳米管混合物电极表面，在高温作用下，碳纳米管所吸收 的粘合剂发生相变，体积迅速扩大使碳纳米管得到有效分散；(5) Turn on the power supply, so that electric heat sources such as electric arcs, plasmas, and electric sparks of a certain intensity are generated between the two electrodes of the circuit, and the high temperature generated by the heat source is applied to the surface of the carbon nanotube mixture electrode. The binder absorbed by the nanotubes undergoes a phase change, and the volume rapidly expands to effectively disperse the carbon nanotubes;
(6)在步骤(5)所述电致热源附近由气流装置所产生气流将所分散在气相空间的碳纳 米管运输至除杂装置以脱去碳纳米管所附着的残余粘合剂；(6) The carbon nanotubes dispersed in the gas phase space are transported to the impurity removal device by the airflow generated by the airflow device near the electric heat source described in step (5) to remove the residual adhesive attached by the carbon nanotubes;
(7)通过由气流牵引所分散的碳纳米管至收集或是进一步加工的区域。(7) By dragging the dispersed carbon nanotubes to the collection or further processing area by the airflow.
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| CN106219509A (en) * | 2016-06-20 | 2016-12-14 | 青岛科技大学 | A kind of carbon nano tube dispersion method |
| CN106082173B (en) * | 2016-06-20 | 2019-06-28 | 青岛科技大学 | A kind of carbon nano tube dispersion method |
| CN106006607A (en) * | 2016-06-20 | 2016-10-12 | 青岛科技大学 | Gas-phase dispersed carbon nanotube capturing and collecting device |
| CN106188682B (en) * | 2016-06-20 | 2019-08-23 | 青岛科技大学 | A kind of method that the nanotube dispersion of gas phase dispersion prepares Carbon Nanotubes/natural Rubber Composites |
| CN106082174B (en) * | 2016-06-20 | 2019-06-28 | 青岛科技大学 | A kind of carbon nanotube dispersal device |
| CN106906642A (en) * | 2017-03-28 | 2017-06-30 | 青岛科技大学 | A kind of device that carbon fiber surface modification is carried out by rapid attachment two-phase layer CNT |
| CN106955629B (en) * | 2017-03-28 | 2022-07-15 | 青岛科技大学 | A nanomaterial dispersing device |
| CN106978718B (en) * | 2017-03-28 | 2019-08-27 | 青岛科技大学 | A surface modification method for carbon fiber to quickly attach double-phase layer carbon nanotubes |
| CN107604675B (en) * | 2017-09-14 | 2020-02-07 | 青岛科技大学 | Contact end treatment method for oriented carbon nanotube modified carbon fiber surface based on gas-phase carbon nanotube dispersed mist |
| CN112176718A (en) * | 2019-07-01 | 2021-01-05 | 青岛科技大学 | Preparation process of carbon fiber with carbon nano tube embedded on surface |
| CN113088086B (en) * | 2021-04-07 | 2022-08-30 | 青岛科技大学 | Filling method of directionally reinforced organic silicone grease based on carbon nano tube/nano silicon carbide gas-phase dispersed mist |
| CN113083121B (en) * | 2021-04-07 | 2022-11-22 | 青岛科技大学 | A filling device for directionally reinforced silicone grease based on carbon nanotube/nano-silicon carbide gas-phase dispersed mist |
| CN113809305B (en) * | 2021-09-17 | 2022-12-27 | 青岛科技大学 | Preparation method and device of tin/carbon nanotube composite material |
| CN115536008B (en) * | 2022-09-05 | 2024-03-01 | 烟台大学 | Miniature continuous carbon nanotube gas-phase dispersing equipment |
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