CN106744817A - A kind of method that single SWCN is peeled off into SWCN tube bank - Google Patents
A kind of method that single SWCN is peeled off into SWCN tube bank Download PDFInfo
- Publication number
- CN106744817A CN106744817A CN201611096459.1A CN201611096459A CN106744817A CN 106744817 A CN106744817 A CN 106744817A CN 201611096459 A CN201611096459 A CN 201611096459A CN 106744817 A CN106744817 A CN 106744817A
- Authority
- CN
- China
- Prior art keywords
- swcn
- walled carbon
- carbon nanotubes
- tube bank
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009830 intercalation Methods 0.000 claims abstract description 5
- 230000002687 intercalation Effects 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 239000002109 single walled nanotube Substances 0.000 abstract description 49
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 23
- 229910021641 deionized water Inorganic materials 0.000 description 23
- 239000012982 microporous membrane Substances 0.000 description 12
- 239000006228 supernatant Substances 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000013517 stratification Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Landscapes
- Battery Electrode And Active Subsutance (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明提供一种将单壁碳纳米管管束剥离成单根离散的单壁碳纳米管的方法，涉及纳米材料制备科学技术领域。本发明利用高锰酸钾与浓硫酸插层氧化作用，对单壁碳纳米管束进行插层剥离，得到了具有水溶性的单根离散单壁碳纳米管。该单壁碳纳米管不是管束型的，而是以单根的形式存在的，其管径为1‑2nm。
The invention provides a method for stripping single-wall carbon nanotube bundles into single discrete single-wall carbon nanotubes, and relates to the scientific and technical field of nanomaterial preparation. The invention utilizes the intercalation oxidation of potassium permanganate and concentrated sulfuric acid to perform intercalation and peeling off of single-wall carbon nanotube bundles, and obtains single discrete single-wall carbon nanotubes with water solubility. The single-wall carbon nanotubes are not bundled, but exist in a single form, and the diameter of the single-walled carbon nanotubes is 1-2nm.
Description
技术领域technical field
本发明涉及纳米材料制备科学技术领域，特别是将单壁碳纳米管管束剥离成单根离散的单壁碳纳米管的方法。The invention relates to the technical field of nanomaterial preparation, in particular to a method for stripping single-wall carbon nanotube bundles into single discrete single-wall carbon nanotubes.
背景技术Background technique
单壁碳纳米管(single-walled carbon nanotubes,SWCNTs)是一种具有单层管壁的一维管状结构的碳纳米材料。单壁碳纳米管有着优异的物理、化学特性，在力学、电学、光学以及电子学等领域具有广阔的应用前景。当前我们所获得的单壁碳纳米管并不是以单根离散的形式存在的，而是管与管之间通过六角密堆形成管束的形式存在的。这些管束中管与管之间具有强烈的范德华力作用，很难将其剥离，同时也非常难以分散在水中。这种状态不但不能充分发挥单壁碳纳米本身的一些优异性能本身的一些优异性能(如光学特性)，而且还会限制碳纳米管的在一些领域的应用，如作为药物传输载体的应用。因此，需要将单壁碳纳米管管束剥离成单根离散型的单壁碳纳米管，并使其具有较好的水溶性。目前，将单壁碳纳米管管束分散成单根单壁碳纳米管最常用方法是超高速离心辅助的超声分散法。这种方法往往需要大型的离心设备装置、操作比较复杂而且处理起来也比较耗时。而且这种方法在超声阶段为了将单壁碳碳纳米管分散而必须引入一些表面活性剂、聚合物等，这往往给碳纳米管后续的处理以及应用带来的困难。同时，这种方法需要用超高速离心(通常50000转以上)对样品进行提取，每次处理量也非常的少(通常在微克量级)，在实际应用中也难以推广。因此，发明一种将单壁碳纳米管管束剥离成单根离散的单壁碳纳米管的方法具有重要的现实意义。Single-walled carbon nanotubes (SWCNTs) are carbon nanomaterials with a one-dimensional tubular structure with a single wall. Single-walled carbon nanotubes have excellent physical and chemical properties, and have broad application prospects in the fields of mechanics, electricity, optics, and electronics. At present, the single-walled carbon nanotubes we have obtained do not exist in the form of a single discrete one, but in the form of tube bundles formed by hexagonal close-packing between tubes. There is a strong van der Waals force between the tubes in these tube bundles, it is difficult to peel them off, and it is also very difficult to disperse them in water. This state not only cannot give full play to some excellent properties of single-walled carbon nanometers (such as optical properties), but also limits the application of carbon nanotubes in some fields, such as the application as a drug delivery carrier. Therefore, it is necessary to peel off the single-walled carbon nanotube bundles into single discrete single-walled carbon nanotubes and make them have better water solubility. At present, the most commonly used method for dispersing single-walled carbon nanotube bundles into single single-walled carbon nanotubes is the ultrasonic dispersion method assisted by ultrahigh-speed centrifugation. This method often requires large centrifuge equipment, complicated operation and time-consuming processing. Moreover, this method must introduce some surfactants, polymers, etc. in order to disperse the single-walled carbon nanotubes in the ultrasonic stage, which often brings difficulties to the subsequent processing and application of the carbon nanotubes. At the same time, this method needs to use ultra-high-speed centrifugation (usually above 50,000 rpm) to extract the sample, and the amount of each treatment is also very small (usually in the order of micrograms), and it is difficult to promote in practical applications. Therefore, it is of great practical significance to invent a method for stripping single-walled carbon nanotube bundles into single discrete single-walled carbon nanotubes.
发明内容Contents of the invention
本发明的目的就是针对现有技术的一些不足，提供一种将单壁碳纳米管管束剥离成单根离散的单壁碳纳米管的方法。The object of the present invention is to provide a method for stripping single-walled carbon nanotube bundles into single discrete single-walled carbon nanotubes to solve some deficiencies in the prior art.
本发明是通过以下技术方案实现的，本发明利用高锰酸钾与浓硫酸插层氧化作用，对单壁碳纳米管束进行插层剥离，得到了具有水溶性的单根离散单壁碳纳米管。The present invention is achieved through the following technical scheme. The present invention utilizes the intercalation oxidation of potassium permanganate and concentrated sulfuric acid to carry out intercalation and stripping of single-walled carbon nanotube bundles, and obtains a single discrete single-walled carbon nanotube with water solubility .
本发明的方法包括如下步骤：Method of the present invention comprises the steps:
将初始的单壁碳纳米管固体和高锰酸钾固体以一定的配比分别加入到过量的浓硫酸溶液中，得到的反应混合液置于40-70℃的水浴中持续搅拌反应1-6h，将反应完的混合液用去离子水稀释，再加入过量双氧水溶液还原除去生成的二氧化锰固体，经过微孔滤膜过滤以及稀盐酸溶液的洗涤后，得到的固体再用去离子水通过高速离心洗涤至上层清液为中性(PH＝6-7)，然后取下层固体加去离子水充分搅拌后，进一步离心后，取上层均一、稳定的溶液，即得到具有高分散性的单根单壁碳纳米管水溶液。将该溶液过滤后收集到的黑色固体即为单根的(非管束型的)单壁碳纳米管。Add the initial single-walled carbon nanotube solid and potassium permanganate solid to excess concentrated sulfuric acid solution in a certain ratio, and place the obtained reaction mixture in a water bath at 40-70°C for 1-6 hours with continuous stirring , dilute the reacted mixed solution with deionized water, add excess hydrogen peroxide solution to reduce and remove the generated manganese dioxide solid, filter through microporous membrane and wash with dilute hydrochloric acid solution, and then pass the obtained solid through deionized water High-speed centrifugation and washing until the supernatant is neutral (PH=6-7), then remove the lower layer of solids and add deionized water to fully stir, and after further centrifugation, take the upper layer of a uniform and stable solution to obtain a highly dispersible mono Single-walled carbon nanotubes in aqueous solution. The black solid collected after filtering the solution is single (non-bundled) single-walled carbon nanotubes.
附图说明Description of drawings
图1为原始单壁碳纳米管的扫描电镜照片。Figure 1 is a scanning electron micrograph of pristine single-walled carbon nanotubes.
图2为原始单壁碳纳米管管束的高分辨透射电镜照片Figure 2 is a high-resolution transmission electron micrograph of the original single-walled carbon nanotube bundles
图3为单根离散的单壁碳纳米管扫描探针显微镜照片。Fig. 3 is a scanning probe microscope photo of a single discrete single-walled carbon nanotube.
图4为单根的非管束型的单壁碳纳米管扫描电镜照片。Fig. 4 is a scanning electron micrograph of a single non-bundle single-walled carbon nanotube.
图5为单根的非管束型的单壁碳纳米管透射电镜照片。Fig. 5 is a transmission electron micrograph of a single non-bundle single-walled carbon nanotube.
图6为单根离散的单壁碳纳米管扫描探针显微镜照片。Fig. 6 is a scanning probe microscope photo of a single discrete single-walled carbon nanotube.
图7为单根离散的单壁碳纳米管扫描探针显微镜照片。Fig. 7 is a scanning probe microscope photo of a single discrete single-walled carbon nanotube.
具体实施方式detailed description
实例1：Example 1:
将初始的单壁碳纳米管(图1和图2)0.1克以及0.2克的高锰酸钾固体依次加入到盛有10ml的浓硫酸(98％)的烧杯中，充分搅拌均匀后，置于40℃的恒温水浴锅中搅拌处理3小时，待冷却至室温后，用约100ml的去离子水稀释，并不断搅拌，再加入约10ml的30％双氧水溶液，搅拌反应15分钟后，用微孔滤膜过滤。得到的黑色固体直接倒入100ml的4％的稀盐酸中搅拌洗涤，再用微孔滤膜过滤，并用去离子水过滤洗涤，得到的黑色固体再倒入到200ml的去离子水中充分搅拌后，用离心机在14000转下离心30分钟，分层后，倒掉上层清液，并继续往离心管中加入适量的去离子水充分搅拌洗涤然后再次离心，分层，倒掉上层清液，如此反复离心洗涤4-6次，最后将得到的离心沉降物收集并加入约200ml的去离子水，搅拌30分钟后，得到的分散液用离心机在14000转下离心30分钟后，小心提取收集上层分散溶液，收集到分散溶液即为高分散的单根单壁碳纳米管水溶液。溶液中分散的单壁碳纳米管是单根的离散的，其管径为1-2nm(图3)。将该溶液用微孔滤膜过滤后收集到的黑色固体放在干燥箱中烘干即得到单根的非管束型的单壁碳纳米管(图4)。0.1 grams of initial single-walled carbon nanotubes (Fig. 1 and Fig. 2) and 0.2 grams of potassium permanganate solids were successively added to a beaker filled with 10 ml of concentrated sulfuric acid (98%), after fully stirring, place Stir in a constant temperature water bath at 40°C for 3 hours. After cooling to room temperature, dilute with about 100ml of deionized water and keep stirring, then add about 10ml of 30% hydrogen peroxide solution, and stir for 15 minutes. Membrane filtration. The obtained black solid is directly poured into 100ml of 4% dilute hydrochloric acid, stirred and washed, then filtered with a microporous membrane, and washed with deionized water, and the obtained black solid is poured into 200ml of deionized water and fully stirred. Use a centrifuge to centrifuge at 14,000 rpm for 30 minutes. After stratification, pour off the supernatant, and continue to add an appropriate amount of deionized water to the centrifuge tube to fully stir and wash, then centrifuge again, separate layers, and pour off the supernatant. Repeated centrifugation and washing for 4-6 times, finally collected the centrifuge sediment and added about 200ml of deionized water, stirred for 30 minutes, centrifuged the obtained dispersion at 14000 rpm for 30 minutes, carefully extracted and collected the upper layer Dispersion solution, the dispersion solution collected is a highly dispersed single single-walled carbon nanotube aqueous solution. The single-walled carbon nanotubes dispersed in the solution are single and discrete, with a diameter of 1-2 nm (Fig. 3). The black solid collected after filtering the solution with a microporous membrane was placed in a drying oven to dry to obtain a single non-tubular single-walled carbon nanotube ( FIG. 4 ).
实施例2：Example 2:
将初始的单壁碳纳米管0.1克以及0.1克的高锰酸钾固体依次加入到盛有10ml的浓硫酸(98％)的烧杯中，充分搅拌均匀后，置于50℃的恒温水浴锅中搅拌处理6小时，待冷却至室温后，用约100ml的去离子水稀释，并不断搅拌，再加入约10ml的30％双氧水溶液，搅拌反应15分钟后，用微孔滤膜过滤。得到的黑色固体直接倒入100ml的4％的稀盐酸中搅拌洗涤，再用微孔滤膜过滤，并用去离子水过滤洗涤，得到的黑色固体再倒入到200ml的去离子水中充分搅拌后，用离心机在14000转下离心30分钟，分层后，倒掉上层清液，并继续往离心管中加入适量的去离子水充分搅拌洗涤然后再次离心，分层，倒掉上层清液，如此反复离心洗涤4-6次，最后将得到的离心沉降物收集并加入约200ml的去离子水，搅拌30分钟后，得到的分散液用离心机在14000转下离心30分钟后，小心提取收集上层分散溶液，收集到分散溶液即为高分散的单根单壁碳纳米管水溶液。溶液中分散的单壁碳纳米管是单根的离散的。(图5)将该溶液用微孔滤膜过滤后收集到的黑色固体放在干燥箱中烘干即得到单根的非管束型的单壁碳纳米管。Add 0.1 grams of initial single-walled carbon nanotubes and 0.1 grams of potassium permanganate solids to a beaker filled with 10 ml of concentrated sulfuric acid (98%) in turn, stir well, and place in a constant temperature water bath at 50°C Stir for 6 hours. After cooling to room temperature, dilute with about 100ml of deionized water and keep stirring. Then add about 10ml of 30% hydrogen peroxide solution. After stirring for 15 minutes, filter with a microporous membrane. The obtained black solid is directly poured into 100ml of 4% dilute hydrochloric acid, stirred and washed, then filtered with a microporous membrane, and washed with deionized water, and the obtained black solid is poured into 200ml of deionized water and fully stirred. Use a centrifuge to centrifuge at 14,000 rpm for 30 minutes. After stratification, pour off the supernatant, and continue to add an appropriate amount of deionized water to the centrifuge tube to fully stir and wash, then centrifuge again, separate layers, and pour off the supernatant. Repeated centrifugation and washing for 4-6 times, finally collected the centrifuge sediment and added about 200ml of deionized water, stirred for 30 minutes, centrifuged the obtained dispersion at 14000 rpm for 30 minutes, carefully extracted and collected the upper layer Dispersion solution, the dispersion solution collected is a highly dispersed single single-walled carbon nanotube aqueous solution. The single-walled carbon nanotubes dispersed in the solution are single and discrete. (FIG. 5) The black solid collected after filtering the solution with a microporous membrane was dried in a drying oven to obtain a single non-bundle single-walled carbon nanotube.
实施例3：Example 3:
将初始的单壁碳纳米管0.1克以及0.4克的高锰酸钾固体依次加入到盛有10ml的浓硫酸(98％)的烧杯中，充分搅拌均匀后，置于40℃的恒温水浴锅中搅拌处理1小时，待冷却至室温后，用约100ml的去离子水稀释，并不断搅拌，再加入约10ml的30％双氧水溶液，搅拌反应15分钟后，用微孔滤膜过滤。得到的黑色固体直接倒入100ml的4％的稀盐酸中搅拌洗涤，再用微孔滤膜过滤，并用去离子水过滤洗涤，得到的黑色固体再倒入到200ml的去离子水中充分搅拌后，用离心机在14000转下离心30分钟，分层后，倒掉上层清液，并继续往离心管中加入适量的去离子水充分搅拌洗涤然后再次离心，分层，倒掉上层清液，如此反复离心洗涤4-6次，最后将得到的离心沉降物收集并加入约200ml的去离子水，搅拌30分钟后，得到的分散液用离心机在4000转下离心30分钟后，小心提取收集上层分散溶液，收集到分散溶液即为高分散的单根单壁碳纳米管水溶液。溶液中分散的单壁碳纳米管是单根的离散的。(图6)将该溶液用微孔滤膜过滤后收集到的黑色固体放在干燥箱中烘干即得到单根的非管束型的单壁碳纳米管。Add 0.1 grams of initial single-walled carbon nanotubes and 0.4 grams of potassium permanganate solids into a beaker filled with 10 ml of concentrated sulfuric acid (98%) in turn, stir well, and place in a constant temperature water bath at 40°C Stir for 1 hour, after cooling to room temperature, dilute with about 100ml of deionized water, and keep stirring, then add about 10ml of 30% hydrogen peroxide solution, stir for 15 minutes, then filter with a microporous membrane. The obtained black solid is directly poured into 100ml of 4% dilute hydrochloric acid, stirred and washed, then filtered with a microporous membrane, and washed with deionized water, and the obtained black solid is poured into 200ml of deionized water and fully stirred. Use a centrifuge to centrifuge at 14,000 rpm for 30 minutes. After stratification, pour off the supernatant, and continue to add an appropriate amount of deionized water to the centrifuge tube to fully stir and wash, then centrifuge again, separate layers, and pour off the supernatant. Repeated centrifugation and washing for 4-6 times, finally collected the obtained centrifugal sediment and added about 200ml of deionized water, stirred for 30 minutes, centrifuged the obtained dispersion at 4000 rpm for 30 minutes, carefully extracted and collected the upper layer Dispersion solution, the dispersion solution collected is a highly dispersed single single-walled carbon nanotube aqueous solution. The single-walled carbon nanotubes dispersed in the solution are single and discrete. (FIG. 6) The black solid collected after filtering the solution with a microporous membrane was dried in a drying oven to obtain a single non-bundle single-walled carbon nanotube.
实施例4：Example 4:
将初始的单壁碳纳米管0.1克以及0.1克的高锰酸钾固体依次加入到盛有10ml的浓硫酸(98％)的烧杯中，充分搅拌均匀后，置于70℃的恒温水浴锅中搅拌处理1小时，待冷却至室温后，用约100ml的去离子水稀释，并不断搅拌，再加入约10ml的30％双氧水溶液，搅拌反应15分钟后，用微孔滤膜过滤。得到的黑色固体直接倒入100ml的4％的稀盐酸中搅拌洗涤，再用微孔滤膜过滤，并用去离子水过滤洗涤，得到的黑色固体再倒入到200ml的去离子水中充分搅拌后，用离心机在14000转下离心30分钟，分层后，倒掉上层清液，并继续往离心管中加入适量的去离子水充分搅拌洗涤然后再次离心，分层，倒掉上层清液，如此反复离心洗涤4-6次，最后将得到的离心沉降物收集并加入约200ml的去离子水，搅拌30分钟后，得到的分散液用离心机在14000转下离心30分钟后，小心提取收集上层分散溶液，收集到分散溶液即为高分散的单根单壁碳纳米管水溶液。溶液中分散的单壁碳纳米管是单根的离散的。(图7)将该溶液用微孔滤膜过滤后收集到的黑色固体放在干燥箱中烘干即得到单根的非管束型的单壁碳纳米管。Add 0.1 grams of initial single-walled carbon nanotubes and 0.1 grams of potassium permanganate solids into a beaker filled with 10 ml of concentrated sulfuric acid (98%) in turn, stir well, and place in a constant temperature water bath at 70°C Stir for 1 hour, after cooling to room temperature, dilute with about 100ml of deionized water, and keep stirring, then add about 10ml of 30% hydrogen peroxide solution, stir for 15 minutes, then filter with a microporous membrane. The obtained black solid is directly poured into 100ml of 4% dilute hydrochloric acid, stirred and washed, then filtered with a microporous membrane, and washed with deionized water, and the obtained black solid is poured into 200ml of deionized water and fully stirred. Use a centrifuge to centrifuge at 14,000 rpm for 30 minutes. After stratification, pour off the supernatant, and continue to add an appropriate amount of deionized water to the centrifuge tube to fully stir and wash, then centrifuge again, separate layers, and pour off the supernatant. Repeated centrifugation and washing for 4-6 times, finally collected the centrifuge sediment and added about 200ml of deionized water, stirred for 30 minutes, centrifuged the obtained dispersion at 14000 rpm for 30 minutes, carefully extracted and collected the upper layer Dispersion solution, the dispersion solution collected is a highly dispersed single single-walled carbon nanotube aqueous solution. The single-walled carbon nanotubes dispersed in the solution are single and discrete. (FIG. 7) The black solid collected after filtering the solution with a microporous membrane was dried in a drying oven to obtain a single non-bundle single-walled carbon nanotube.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096459.1A CN106744817B (en) | 2016-12-02 | 2016-12-02 | A method of by single-walled carbon nanotube tube bank removing at single single-walled carbon nanotube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096459.1A CN106744817B (en) | 2016-12-02 | 2016-12-02 | A method of by single-walled carbon nanotube tube bank removing at single single-walled carbon nanotube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106744817A true CN106744817A (en) | 2017-05-31 |
| CN106744817B CN106744817B (en) | 2019-05-28 |
Family
ID=58883092
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611096459.1A Active CN106744817B (en) | 2016-12-02 | 2016-12-02 | A method of by single-walled carbon nanotube tube bank removing at single single-walled carbon nanotube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106744817B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118723978A (en) * | 2023-03-30 | 2024-10-01 | 中国科学院福建物质结构研究所 | A method for purifying single-walled carbon nanotubes |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328276A (en) * | 2008-07-24 | 2008-12-24 | 同济大学 | A preparation method of single-walled carbon nanotube-polymer conductive composite film |
| CN102791617A (en) * | 2010-01-25 | 2012-11-21 | 得克萨斯A&M大学体系 | Dispersion and recovery of unbundled nanotubes |
| CN104724691A (en) * | 2013-12-23 | 2015-06-24 | 北京阿格蕾雅科技发展有限公司 | Method for raising dispersibility of single-walled carbon nanotubes |
| US20160347619A1 (en) * | 2015-05-29 | 2016-12-01 | National Taiwan University Of Science And Technology | Modified Graphene, Method for Producing a Modified Graphene and Applications Thereof |
-
2016
- 2016-12-02 CN CN201611096459.1A patent/CN106744817B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328276A (en) * | 2008-07-24 | 2008-12-24 | 同济大学 | A preparation method of single-walled carbon nanotube-polymer conductive composite film |
| CN102791617A (en) * | 2010-01-25 | 2012-11-21 | 得克萨斯A&M大学体系 | Dispersion and recovery of unbundled nanotubes |
| CN104724691A (en) * | 2013-12-23 | 2015-06-24 | 北京阿格蕾雅科技发展有限公司 | Method for raising dispersibility of single-walled carbon nanotubes |
| US20160347619A1 (en) * | 2015-05-29 | 2016-12-01 | National Taiwan University Of Science And Technology | Modified Graphene, Method for Producing a Modified Graphene and Applications Thereof |
Non-Patent Citations (1)
| Title |
|---|
| NINA I. KOVTYUKHOVA ET AL.，: "Individual Single-Walled Nanotubes and Hydrogels Made by Oxidative Exfoliation of Carbon Nanotube Ropes", 《JOURNAL OF AMERICAN CHEMISTRY SOCIETY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118723978A (en) * | 2023-03-30 | 2024-10-01 | 中国科学院福建物质结构研究所 | A method for purifying single-walled carbon nanotubes |
| CN118723978B (en) * | 2023-03-30 | 2025-11-14 | 中国科学院福建物质结构研究所 | A purification method for single-walled carbon nanotubes |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106744817B (en) | 2019-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | Soluble ultra-short single-walled carbon nanotubes | |
| JP5613230B2 (en) | Graphene nanoribbons produced from carbon nanotubes by alkali metal exposure | |
| CN103692763B (en) | A kind of stripping means of two-dimensional layer nano material | |
| CN100486890C (en) | Electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method | |
| CN109437154B (en) | A method for preparing energy band controllable carbon quantum dots using coal as raw material | |
| CN101229918A (en) | A method for oxidation modification of carbon nanotubes | |
| CN102674334A (en) | Preparation method of graphene with nano ferroferric oxide precipitated on surface | |
| CN102350234B (en) | Dispersion method for carbon nanotubes | |
| KR20140068853A (en) | Nanoplate-nanotube composites, methods for production thereof and products obtained therefrom | |
| CN101173117A (en) | Preparation method of manganese dioxide-coated carbon nanotube core-shell composite material | |
| Liu et al. | Additive‐free dispersion of single‐walled carbon nanotubes and its application for transparent conductive films | |
| CN106744913A (en) | A kind of method that utilization cryptocrystalline graphite largely prepares graphene oxide quantum dot | |
| Ansón-Casaos et al. | Optical absorption response of chemically modified single-walled carbon nanotubes upon ultracentrifugation in various dispersants | |
| CN106430153A (en) | Preparing method of ultrashort carbon nano tube with high dispersibility | |
| CN101863463A (en) | A kind of preparation method of water-dispersible carbon nanotube | |
| CN105502340A (en) | Preparation method of fluorescent carbon dots | |
| CN103172048A (en) | Preparation method of water-soluble carbon nanotube | |
| CN100447075C (en) | A kind of highly water-soluble carbon nanotube and preparation method thereof | |
| CN100528312C (en) | Method of dispersing carbon nano-tube with nano particle permeation technique | |
| CN105540567A (en) | Single multi-wall carbon nanotube dispersion liquid and preparation method thereof | |
| CN106744817A (en) | A kind of method that single SWCN is peeled off into SWCN tube bank | |
| CN104528687A (en) | Method for reversibly regulating and controlling agglomeration and dispersion of single-walled carbon nanotubes (SWNTs) by virtue of electrochemical oxidation-reduction | |
| KR101738343B1 (en) | Nano ring carbon nano tube using nano oxide particle-template and fabrication method of the same | |
| CN107226468A (en) | A kind of improvement Hummers methods prepare the method and its obtained graphene oxide of graphene oxide | |
| CN105271194A (en) | Preparation method of graphene quantum dots containing methoxyl |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |