CN201399315Y - A device for purifying and separating graphene oxide by microporous method - Google Patents
A device for purifying and separating graphene oxide by microporous method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 47
- 229910021389 graphene Inorganic materials 0.000 title claims description 45
- 239000012528 membrane Substances 0.000 claims abstract description 37
- 239000011148 porous material Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000012216 screening Methods 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- -1 200 mesh graphite Chemical compound 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
Description
技术领域 technical field
本实用新型涉及纯化分离的氧化石墨烯在电子领域的一个具体应用，尤其涉及一种用微孔法纯化分离氧化石墨烯的装置。The utility model relates to a specific application of purified and separated graphene oxide in the electronic field, in particular to a device for purifying and separating graphene oxide by a micropore method.
背景技术 Background technique
目前在电子领域普遍采用的硅材料，其尺寸小于10纳米时，用它制造出的晶体管稳定性变差，10纳米成为硅材料技术无法再发挥作用的小型化极限。石墨烯是目前发现的最薄、强度最大、导电性能最好的材料，可以被刻成尺寸不到1个分子大小的单电子晶体管。而晶体管的尺寸越小，其性能越好。石墨烯高度稳定，即使被切成1纳米宽的元件，导电性也很好。此外，石墨烯单电子晶体管可在室温下工作。石墨烯晶体管展示出优点和良好性能，石墨烯可能最终会替代硅。而在目前制备石墨烯的三种主要方法(微机械剥离法、外延生长法和氧化法)中，氧化法是能实现石墨烯大规模制备的有效方法。但是氧化法制备的石墨烯在反应过程中不可避免的带进了一些杂质元素和官能团，这些杂质和官能团的存在对石墨烯在电子器件等领域的应用带来了一定的困难。另外由于原料石墨的晶粒分布的影响，比如200目的石墨，其物理意义是大于200目的粒径占50％，小于200目的粒径也占50％。因此通过对杂质和官能团的初级纯化后，需要实现对石墨烯在几何尺寸和厚度的进一步纯化分离，以满足石墨烯在电子领域的应用需求。At present, the silicon material commonly used in the electronic field, when its size is less than 10 nanometers, the stability of transistors manufactured with it will deteriorate, and 10 nanometers has become the miniaturization limit where silicon material technology can no longer function. Graphene is the thinnest, strongest, and best conductive material found so far, and it can be carved into a single-electron transistor with a size less than 1 molecule. And the smaller the size of the transistor, the better its performance. Graphene is highly stable and conducts electricity well even when sliced into 1-nanometer-wide elements. In addition, graphene single-electron transistors can operate at room temperature. Graphene transistors show advantages and good performance, and graphene may eventually replace silicon. Among the three main methods for preparing graphene (micromechanical exfoliation method, epitaxial growth method and oxidation method), the oxidation method is an effective method for large-scale preparation of graphene. However, the graphene prepared by the oxidation method inevitably brings in some impurity elements and functional groups during the reaction process. The existence of these impurities and functional groups brings certain difficulties to the application of graphene in electronic devices and other fields. In addition, due to the influence of the grain distribution of raw graphite, such as 200 mesh graphite, its physical meaning is that the particle size larger than 200 mesh accounts for 50%, and the particle size smaller than 200 mesh also accounts for 50%. Therefore, after primary purification of impurities and functional groups, it is necessary to further purify and separate graphene in terms of geometric size and thickness, so as to meet the application requirements of graphene in the electronic field.
发明内容 Contents of the invention
本实用新型的目的就是为了克服上述现有技术存在的缺陷而提供一种操作简单、成本低廉、效率高效的微孔法纯化分离氧化石墨烯的装置。The purpose of this utility model is to provide a device for purifying and separating graphene oxide with simple operation, low cost and high efficiency in order to overcome the above-mentioned defects in the prior art.
本实用新型的目的可以通过以下技术方案来实现：一种微孔法纯化分离氧化石墨烯的装置，其特征在于，该装置包括力单元、磁单元、筛分单元，所述的力单元包括圆筒、气压计和通气口，所述的通气口设置在圆筒上，气压计设置在通气口上，所述的磁单元包括电磁铁和磁转子，磁转子设置在小圆筒滤器内，电磁铁设置在圆筒底部，所述的筛分单元包括小圆筒滤器和滤膜，滤膜置于小圆筒滤器内，小圆筒滤器置于圆筒内。The purpose of the utility model can be achieved through the following technical solutions: a device for purifying and separating graphene oxide by microporous method, characterized in that the device includes a force unit, a magnetic unit, and a screening unit, and the force unit includes a circular cylinder, air gauge and air vent, the air vent is arranged on the cylinder, the air gauge is arranged on the air vent, the magnetic unit includes an electromagnet and a magnetic rotor, the magnetic rotor is arranged in the small cylinder filter, and the electromagnet Set at the bottom of the cylinder, the screening unit includes a small cylinder filter and a filter membrane, the filter membrane is placed in the small cylinder filter, and the small cylinder filter is placed in the cylinder.
所述的圆筒高20-30cm，直径为50-60cm。The cylinder is 20-30cm high and 50-60cm in diameter.
所述的电磁铁为环形电磁铁，其直径略小于圆筒直径。The electromagnet is an annular electromagnet whose diameter is slightly smaller than that of the cylinder.
所述的电磁铁的直径为40-58cm。The diameter of the electromagnet is 40-58cm.
所述的磁转子为小圆筒滤器直径的四分之一。The magnetic rotor is a quarter of the diameter of the small cylinder filter.
所述的小圆筒滤器为可装卸的小圆筒滤器，该小圆筒滤器与圆筒通过螺纹铆接。The small cylinder filter is a detachable small cylinder filter, and the small cylinder filter is riveted with the cylinder through threads.
所述的小圆筒滤器的直径为5-30cm。The diameter of the small cylinder filter is 5-30cm.
所述的滤膜为微孔型滤膜，其孔径为450-1200nm。The filter membrane is a microporous filter membrane with a pore diameter of 450-1200nm.
所述的滤膜包括WC型微孔滤膜。The filter membrane includes WC type microporous filter membrane.
与现有技术相比，本实用新型微孔分离纯化氧化石墨烯装置，装置简单、使用方便、高效，解决了石墨烯几何尺寸上的窄化分离纯化，可满足不同的应用需求，适合工业化生产。Compared with the prior art, the microporous separation and purification graphene oxide device of the utility model is simple, easy to use, and efficient, and solves the narrow separation and purification of graphene geometric size, which can meet different application requirements and is suitable for industrial production .
附图说明 Description of drawings
图1为本实用新型微孔法纯化分离氧化石墨烯的装置的结构示意图。Fig. 1 is a structural schematic diagram of a device for purifying and separating graphene oxide by the microporous method of the present invention.
具体实施方式 Detailed ways
下面结合附图和具体实施例对本实用新型进行详细说明。The utility model will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
实施例1Example 1
如图1所示，一种微孔法纯化分离氧化石墨烯的装置，该装置包括力单元、磁单元、筛分单元，所述的力单元包括高30cm、直径60cm的圆筒1、气压计2和通气口3，所述的通气口3设置在圆筒1上，气压计2设置在通气口3上，所述的磁单元包括环形电磁铁4和磁转子5，磁转子5设置在小圆筒滤器6内，其直径为7.5cm，电磁铁4设置在圆筒1底部，其直径为58cm，所述的筛分单元包括小圆筒滤器6和滤膜7，滤膜7置于小圆筒滤器6内，小圆筒滤器6置于圆筒1内，小圆筒滤器6与圆筒1通过螺纹铆接。As shown in Figure 1, a device for purifying and separating graphene oxide by microporous method, the device includes a force unit, a magnetic unit, and a screening unit, and the described force unit includes a cylinder 1 with a height of 30 cm and a diameter of 60 cm, a barometer 2 and vent 3, the vent 3 is set on the cylinder 1, the barometer 2 is set on the vent 3, the magnetic unit includes an annular electromagnet 4 and a magnetic rotor 5, and the magnetic rotor 5 is set on a small In the cylinder filter 6, its diameter is 7.5cm, and the electromagnet 4 is arranged on the bottom of the cylinder 1, and its diameter is 58cm. The described screening unit includes a small cylinder filter 6 and a filter membrane 7, and the filter membrane 7 is placed in a small cylinder filter 6. Inside the cylinder filter 6, a small cylinder filter 6 is placed in the cylinder 1, and the small cylinder filter 6 and the cylinder 1 are riveted with threads.
纯化的氧化石墨烯的制备技术路线如下：The preparation technical route of the graphene oxide of purification is as follows:
通入气体(如氮气、氩气等)排出圆筒1内的空气。选择直径为30cm的小圆筒滤器6和相应的滤膜7(孔径为1200nm)，将初级纯化的氧化石墨烯溶胶倒入小圆筒滤器6内，开启电源，控制磁转子的转速为1000转/分。继续通入气体，使筒内的压强保持在1.2大气压。待溶液滤完后，开启出口8，让滤液流出，卸下小圆筒滤器6，取出滤膜7，得到横向尺寸均匀一致的石墨烯片。统计结果分析表明，产物中横向尺寸小于1200nm石墨烯片微乎其微，横向平均尺寸在1200nm以上的接近百分之百。Gas (such as nitrogen, argon, etc.) is introduced to discharge the air in the cylinder 1 . Select a small cylinder filter 6 with a diameter of 30cm and a corresponding filter membrane 7 (pore size is 1200nm), pour the primary purified graphene oxide sol into the small cylinder filter 6, turn on the power, and control the rotating speed of the magnetic rotor to 1000 rpm /point. Continue to feed the gas to keep the pressure in the cylinder at 1.2 atmospheres. After the solution is filtered, the outlet 8 is opened to allow the filtrate to flow out, the small cylinder filter 6 is removed, and the filter membrane 7 is taken out to obtain graphene sheets with uniform transverse dimensions. Analysis of statistical results shows that the graphene sheets with a lateral size smaller than 1200nm in the product are negligible, and nearly 100% of the products have a lateral average size larger than 1200nm.
实施例2Example 2
参见图1，一种微孔法纯化分离氧化石墨烯的装置，该装置包括力单元、磁单元、筛分单元，所述的力单元包括高20cm、直径50cm的圆筒、气压计和通气口，所述的通气口设置在圆筒上，气压计设置在通气口上，所述的磁单元包括环形电磁铁和磁转子，磁转子设置在圆筒内，其直径为5cm，电磁铁设置在圆筒底部，其直径为40cm，所述的筛分单元包括小圆筒滤器和滤膜，滤膜置于小圆筒滤器内，小圆筒滤器置于圆筒内，小圆筒滤器与圆筒通过螺纹铆接。Referring to Fig. 1, a device for purifying and separating graphene oxide by micropore method, the device includes a force unit, a magnetic unit, and a screening unit, and the force unit includes a cylinder with a height of 20 cm and a diameter of 50 cm, an air gauge and a vent , the air vent is arranged on the cylinder, the air gauge is arranged on the air vent, the magnetic unit includes a ring electromagnet and a magnetic rotor, the magnetic rotor is arranged in the cylinder, and its diameter is 5cm, and the electromagnet is arranged in the circular Cylinder bottom, its diameter is 40cm, and described screening unit comprises small cylindrical filter and filter membrane, and filter membrane is placed in small cylindrical filter, and small cylindrical filter is placed in cylinder, and small cylindrical filter and cylinder Riveted by thread.
通入气体(如氮气、氩气等)排出圆筒内的空气。选择直径为20cm的小圆筒滤器和相应的滤膜(孔径为1000nm)，将实施例1中的滤液倒入滤器内。开启电源，控制磁转子的转速为1000转/分。继续通入气体，使筒内的压强保持在1.5大气压。待溶液滤完后，开启出口，让滤液流出。卸下滤器，取出滤膜，得到横向尺寸均匀一致的石墨烯片。统计结果分析表明，产物中横向尺寸小于1000nm石墨烯片微乎其微，横向平均尺寸在1000～1200nm以上的接近百分之百。Introduce gas (such as nitrogen, argon, etc.) to discharge the air in the cylinder. Select a small cylindrical filter with a diameter of 20 cm and a corresponding filter membrane (with a pore size of 1000 nm), and pour the filtrate in Example 1 into the filter. Turn on the power supply, and control the rotational speed of the magnetic rotor to be 1000 rpm. Continue to feed the gas to keep the pressure in the cylinder at 1.5 atmospheres. After the solution is filtered, open the outlet to let the filtrate flow out. Remove the filter and take out the filter membrane to obtain graphene sheets with uniform lateral dimensions. Analysis of statistical results shows that the graphene sheets with a lateral size smaller than 1000nm in the product are negligible, and nearly 100% of the products have an average lateral size of more than 1000-1200nm.
实施例3Example 3
通入气体(如氮气、氩气等)排出圆筒内的空气。选择直径为15cm的小圆筒滤器和相应的滤膜(孔径为800nm)，将实施例2中的滤液倒入滤器内。开启电源，控制磁转子的转速为1000转/分。继续通入气体，使筒内的压强保持在1.2大气压。待溶液滤完后，开启出口，让滤液流出。卸下滤器，取出滤膜，得到横向尺寸均匀一致的石墨烯片。统计结果分析表明，产物中横向尺寸小于800nm石墨烯片微乎其微，横向平均尺寸在800～1000nm以上的接近百分之百。Introduce gas (such as nitrogen, argon, etc.) to discharge the air in the cylinder. Select a small cylindrical filter with a diameter of 15 cm and a corresponding filter membrane (pore size of 800 nm), and pour the filtrate in Example 2 into the filter. Turn on the power supply, and control the rotational speed of the magnetic rotor to be 1000 rpm. Continue to feed the gas to keep the pressure in the cylinder at 1.2 atmospheres. After the solution is filtered, open the outlet to let the filtrate flow out. Remove the filter and take out the filter membrane to obtain graphene sheets with uniform lateral dimensions. Analysis of statistical results shows that the graphene sheets with a lateral size smaller than 800nm in the product are negligible, and nearly 100% of the products have a lateral average size of more than 800-1000nm.
实施例4Example 4
通入气体(如氮气、氩气等)排出圆筒内的空气。选择直径为5cm的小圆筒滤器和相应的滤膜(孔径为450nm)，将实施例3中的滤液倒入滤器内。开启电源，控制磁转子的转速为1000转/分。继续通入气体，使筒内的压强保持在1.5大气压。待溶液滤完后，开启出口，让滤液流出。卸下滤器，取出滤膜，得到横向尺寸均匀一致的石墨烯片。统计结果分析表明，产物中横向尺寸小于450nm石墨烯片微乎其微，横向平均尺寸在450～800nm以上的接近百分之百。Introduce gas (such as nitrogen, argon, etc.) to discharge the air in the cylinder. Select a small cylindrical filter with a diameter of 5 cm and a corresponding filter membrane (pore size of 450 nm), and pour the filtrate in Example 3 into the filter. Turn on the power supply, and control the rotational speed of the magnetic rotor to be 1000 rpm. Continue to feed the gas to keep the pressure in the cylinder at 1.5 atmospheres. After the solution is filtered, open the outlet to let the filtrate flow out. Remove the filter and take out the filter membrane to obtain graphene sheets with uniform lateral dimensions. Analysis of statistical results shows that the graphene sheets with a lateral size smaller than 450nm in the product are negligible, and nearly 100% of the products have an average lateral size of more than 450-800nm.
实施例5Example 5
一种微孔法纯化分离氧化石墨烯的装置，该装置包括力单元、磁单元、筛分单元，所述的力单元包括高25cm、直径55cm的圆筒、气压计和通气口，所述的通气口设置在圆筒上，气压计设置在通气口上，所述的磁单元包括环形电磁铁和磁转子，磁转子设置在小圆筒滤器内，磁转子为小圆筒滤器直径的四分之一，电磁铁设置在圆筒底部，所述的筛分单元包括小圆筒滤器和滤膜，滤膜为WC型微孔滤膜，置于小圆筒滤器内，小圆筒滤器置于圆筒内，小圆筒滤器与圆筒通过螺纹铆接。A device for purifying and separating graphene oxide by microporous method, the device includes a force unit, a magnetic unit, and a sieving unit, and the force unit includes a cylinder with a height of 25 cm and a diameter of 55 cm, an air gauge and an air vent. The air vent is arranged on the cylinder, and the air gauge is arranged on the air vent. The magnetic unit includes a ring electromagnet and a magnetic rotor. The magnetic rotor is arranged in the small cylinder filter, and the magnetic rotor is a quarter of the diameter of the small cylinder filter. 1. The electromagnet is set at the bottom of the cylinder. The screening unit includes a small cylinder filter and a filter membrane. The filter membrane is a WC type microporous filter membrane, which is placed in the small cylinder filter. In the cylinder, the small cylinder filter and the cylinder are riveted by threads.
采用上述装置进行微孔法纯化分离氧化石墨烯的步骤如下：The steps of adopting the above-mentioned device to purify and separate graphene oxide by microporous method are as follows:
1)向圆筒缓慢的通入氮气，排尽圆筒的空气；1) Slowly inject nitrogen into the cylinder to exhaust the air in the cylinder;
2)将经过初级纯化但尺寸分布不均的氧化石墨烯溶胶倒进装有滤膜的小圆筒滤器内，关闭出口，开启电源，控制圆筒的气压在1.2～2个大气压之间，磁转子在电磁场的作用下转动搅拌，控制磁转子的转速为1000转/分，使石墨烯溶胶不粘黏在滤膜上；2) Pour the graphene oxide sol that has undergone primary purification but with uneven size distribution into a small cylinder filter equipped with a filter membrane, close the outlet, turn on the power supply, and control the air pressure of the cylinder between 1.2 and 2 atmospheres. The rotor rotates and stirs under the action of the electromagnetic field, and the speed of the magnetic rotor is controlled to 1000 rpm, so that the graphene sol does not stick to the filter membrane;
3)打开出口，使圆筒内气压与外界大气压平衡，放出滤液；3) Open the outlet to balance the air pressure in the cylinder with the external atmospheric pressure, and release the filtrate;
4)卸下小圆筒滤器，取出滤膜，用去离子水洗涤滤膜。4) Remove the small cylinder filter, take out the filter membrane, and wash the filter membrane with deionized water.
所述的步骤(2)中的滤膜可以根据需要进行微孔尺寸的选择。滤膜，比如WC型微孔滤膜，在使用之前应在70℃的去离子水中浸泡4个小时以上，使用前再用适量新鲜的去离子水冲洗1～2次，然后再装入已洗过的小圆筒滤器中备用。The filter membrane in the step (2) can be selected according to the needs of the pore size. Filter membranes, such as WC microporous membranes, should be soaked in deionized water at 70°C for more than 4 hours before use, rinsed with an appropriate amount of fresh deionized water for 1 or 2 times before use, and then put into the washed Reserve in a small cylindrical filter.
所述的步骤(2)中的小圆筒滤器可以自由装卸，滤器的直径可以随微孔滤膜的直径而改变替换，可以根据需要选择不同直径的滤器，而小圆筒与大圆筒之间所连接的螺纹直径不变。The small cylinder filter in the described step (2) can be freely loaded and unloaded, and the diameter of the filter can be changed and replaced with the diameter of the microporous filter membrane, and filters of different diameters can be selected as required, and between the small cylinder and the large cylinder The diameter of the thread to be connected does not change.
所述的步骤(3)中的滤液可以根据需要选择不同的小圆筒滤器和相应的滤膜循环过滤，以得到不同尺寸分布的石墨烯。The filtrate in the described step (3) can select different small cylindrical filters and corresponding filter membranes to circulate and filter according to needs, so as to obtain graphene with different size distributions.
Claims (9)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118872A (en) * | 2014-08-04 | 2014-10-29 | 湖南元素密码石墨烯研究院（有限合伙） | Method and device for purifying oxidized graphene/graphene solution |
| CN109019580A (en) * | 2018-09-27 | 2018-12-18 | 深圳天元羲王材料科技有限公司 | A kind of graphene purifying plant and method |
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2009
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118872A (en) * | 2014-08-04 | 2014-10-29 | 湖南元素密码石墨烯研究院（有限合伙） | Method and device for purifying oxidized graphene/graphene solution |
| CN109019580A (en) * | 2018-09-27 | 2018-12-18 | 深圳天元羲王材料科技有限公司 | A kind of graphene purifying plant and method |
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