CN104003375A - Preparation method for small-size graphene - Google Patents
Preparation method for small-size graphene Download PDFInfo
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- CN104003375A CN104003375A CN201410186353.5A CN201410186353A CN104003375A CN 104003375 A CN104003375 A CN 104003375A CN 201410186353 A CN201410186353 A CN 201410186353A CN 104003375 A CN104003375 A CN 104003375A
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Abstract
A disclosed preparation method for small-size graphene comprises the steps: step 1, mixing a graphite powder raw material and a solvent to obtain a graphite mixed solution; step 2, putting the solution in a container, and fixedly arranging a homogenizing head of a stator-rotor apparatus of a stator-rotor mixer below the liquid level; step 3, starting a cooling system and the stator-rotor mixer for processing; and step 4, performing standing processing or centrifugation separation on the prepared solution to remove incompletely-peeled particles, and collecting the supernatant to obtain a stable dispersion solution of small-size graphene. According to the preparation method, a rotor rotating with a high speed drives a fluid to have a high-speed motion, so that high velocity gradient and high shear force are generated, and also graphite sheets are subjected to peeling and refining because the high-speed fluid bumps bosses of a hole wall of a stator, and the prepared graphene is small in dimension, concentrated in distribution and high in single-layer ratio. The method has the characteristics of small equipment investment, low raw material cost, simple, easy and practicable operation and impressive output, and is suitable for large-scale industrialized production as well as laboratory research.
Description
Technical field
The present invention relates to a kind of preparation method of small size Graphene, specifically relate to the technology that a kind of hydrokinetics that utilizes high speed rotating rotor to produce is prepared Graphene in solution, belong to Graphene preparing technical field.
Background technology
Grapheme material is since Novselove and Geim obtain 2010 annual Nobel Prizes in physics, obtained unprecedented development, because of its unique excellent properties in each side such as physics, chemistry, electricity, mechanics, in fields such as novel material, new forms of energy, microelectronics, demonstrated out huge application prospect.Yet the most important prerequisite that realizes Graphene large-scale application is, develop low-costly and in high volume, free of contamination Graphene technology of preparing.Equally, the low-cost and pollution-less technology of preparing in enormous quantities of Graphene is also one of key problem about this material foundation research and commercial application.
Novoselov and Geim, employing micromechanics cleavage technology in 2004, separate graphene film with adhesive tape sticking technology from highly oriented pyrolytic graphite (HOPG).Although the method can be prepared the high-quality graphene that lateral dimension reaches tens microns, efficiency and output are extremely low, only limit to the fundamental research in laboratory.The main stream approach that at present prepared by Graphene belongs to chemical technology category, mainly comprise the methods such as substrate grown, substrate extension, chemical vapour deposition and redox graphene, first three methods shows advantage in electronic devices and components application, but exist temperature pressure to control to require high, high quality substrate, Graphene and substrate separation to be difficult to the severe condition such as control, be difficult to reach the object of a large amount of simple and easy production Graphenes, especially cannot meet the commercial application demand of grapheme material.In addition, graphene oxide method of reducing based on liquid phase process, although be the effective way of macroscopic preparation of graphene, the method complex process, condition is wayward, preparation cost is higher, repeatability is poor, the graphene oxide of reduction and pure Graphene still difference to some extent in performance, and reduction efficiency is lower, chemical reagent used is mostly poisonous, is difficult to meet low-cost green application needs.And in liquid phase, directly peel off the method that common crystalline graphite is prepared Graphene, cheap with its crystalline graphite powder raw material, related solvents and mechanical stripping equipment, solvent can green non-pollution feature, show simple and easy green, low cost, high-level efficiency, prepare in enormous quantities the advantage of Graphene.In this respect, what extensively adopt at present is ultrasonic cavitation technology, utilizes the liquid cavitation of ultrasonic generation to realize peeling off graphite.Yet this method is followed the violent process that also has localized hyperthermia's high pressure of cavitation, can cause the defect of Graphene larger, has reduced the quality of its prepared Graphene, has affected the performance of Graphene.In addition, it is longer that ultrasonic cavitation technology is prepared the needed time of Graphene, and capacity usage ratio is lower.Therefore, develop the preparation method of the Graphene that can realize large-scale industrial production, seem particularly important.
At present, although big size graphene is considered to prepare the ideal material of transparent conductive film, nanoelectronic components and parts and matrix material etc., small size Graphene is too in biomaterial, chemical/biological sensors, the aspect such as optoelectronic device, transparent conductive film has represented huge application potential, especially utilizing Graphene inkjet technology (Graphene size is below 1 micron conventionally) to manufacture novel conductive film, is the most promising technology of Graphene industrial applications.The preparation of small size Graphene at present and the larger difficulty of separated existence, preparation method mainly comprises the methods such as chemical tailoring, mechanical mill, high speed centrifugation, but these methods all have larger shortcoming, prepared Graphene defect is large, performance lower (especially electric property), yield poorly, preparation cost is high.Therefore, exploitation can realize the small size Graphene technology of preparing of large-scale industrial production, has very important significance equally.
Summary of the invention
Object: the preparation method who the object of the present invention is to provide a kind of small size Graphene, the hydrokinetics that the method mainly utilizes high speed rotating rotor to produce is processed Graphite Powder 99, prepared Graphene size is little and distribute to concentrate, individual layer ratio is higher, quality product is high, is a kind of simple and easy, low-cost, high-level efficiency, prepares in enormous quantities the excellent process of small size Graphene.
Technical scheme: above-mentioned purpose of the present invention is achieved by following technical solution:
The preparation method of a kind of small size Graphene of the present invention, the method concrete steps are as follows:
Step 1, by Graphite Powder 99 raw material and solvent, obtains graphite mixing solutions;
Step 2, puts into container by solution, the homogeneous head of the rotor-stator device of rotor-stator mixing tank (also claiming high-shear homogenizer, high-shear emulsion machine) is fixed on below liquid level simultaneously;
Step 3, opens cooling system and makes solution remain on certain temperature, opens rotor-stator mixing tank simultaneously and carries out high speed processing;
Step 4, carries out standing processing or centrifugation preparing solution, removes the particle of not peeling off completely, thereby collect supernatant liquor, obtains stable small size graphene dispersing solution.
Wherein, in above-mentioned steps one, described solvent is one or more mixing in water and organic solvent, the mixture of ethanol, acetone, Virahol and water preferably, wherein organic solvent ratio is 10%-90% (note: prepare two-dimensional nano powder number of patent application in water and organic solvent mixing solutions and be respectively: 201210177012.2,2012100148902.2);
Wherein, in above-mentioned steps one, described graphite raw material is not limit, preferably micro crystal graphite, crystalline flake graphite, expansible black lead, high orientation pyrolytic graphite;
Wherein, in above-mentioned steps one, the starting point concentration of described graphite mixing solutions is not limit, and preferred concentration is 1-30mg/ml;
Wherein, in above-mentioned steps two, in described rotor-stator device, the hole shape of stator surface is not limit, preferably circular hole;
Wherein, in above-mentioned steps two, described rotor-stator device rotor shape is not limit, preferably blade type;
Wherein, in above-mentioned steps two, the rotor in described rotor-stator device and the gap size between stator are 0.1 millimeter to 30 centimetres, and preferably gap is 0.5-10 millimeter;
Wherein, in above-mentioned steps two, the homogeneous head of described rotor-stator device need to be fixed on below liquid level, and preferred position is the following central position of liquid level;
Wherein, in above-mentioned steps three, described unlatching rotor-stator mixing tank carries out high speed processing; The rotating speed of its treating processes rotor-stator mixing tank is that 2000-25000 turns, and preferred rotating speed is that 8000-15000 turns;
Wherein, in above-mentioned steps three, described cooling system is that circulating liquid is cooling, a kind of in but of air cooling and electricity refrigeration, preferably circulating water;
Wherein, in above-mentioned steps three, described treating processes solution maintains the temperature at 0-80 ℃, and preferred solution temperature is 15-35 ℃;
Wherein, in above-mentioned steps four, described time of repose 0.5-20 hour, described centrifugal treating acceleration is 25-5000g, centrifugation time 30-200 minute, and preferred time of repose is 0.5-5 hour, preferred centrifugal acceleration is 35-500g, and preferred centrifugation time is 30-60 minute.
The invention has the beneficial effects as follows:
(1) hydrodynamic method that the present invention utilizes high speed rotating rotor to produce is prepared small size Graphene.First-selected electric motor rotor driven is made high speed rotating with respect to stator, and then rotor promotes graphite mixing solutions high speed rotating together, produces high-speed gradient and high shear force is peeled off graphite in the gap between stator and rotor; The boss generation high-speed impacts of while high-velocity fluid and stator hole wall etc., further make graphite flake peel off and refinement.The beneficial effect of maximum of the present invention is, by case study on implementation 1, prepare almost all Graphene lateral dimensions be all less than 1 μ m, lamellar spacing is less than 3nm, and distribution of sizes concentrates, individual layer ratio is high.
(2) the method preparation process is relatively gentle, can obtain high-quality graphene, and overcome the destruction of current main preparation methods to laminated structure, as having produced the environment such as High Temperature High Pressure at tiny area, ultrasonic cavitation easily destroys graphene-structured, as chemical graft method has been introduced oxy radical in graphene-structured.
(3) the method is prepared Graphene, efficient fast, technique is simple, easy and simple to handle, with low cost, without accurately controlling processing parameter, preparation time is short, pollutes etc., easily expands scale, can realize the suitability for industrialized production of high-quality graphene.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) of the inventive method.
Fig. 2 (a) is not for assembling pictorial diagram completely for generation of the little gap rotor-stator device of high speed rotating fluid in case study on implementation 1.
Fig. 2 (b) is not for assembling pictorial diagram completely for generation of the large gap rotor-stator device of high speed rotating fluid in case study on implementation 1.
Fig. 3 (a) is for generation of the rotor-stator internal mixer section of structure of high rotating fluid in case study on implementation 2.
Fig. 3 (b) is for generation of the rotor-stator mixing tank force diagram of high rotating fluid in case study on implementation 2.
Fig. 4 (a) is the atomic force microscopy of the prepared Graphene of the little gap of the inventive method rotor-stator device.
Fig. 4 (b) is the transmission electron microscope photo of the prepared Graphene of the little gap of the inventive method rotor-stator device.
Fig. 5 (a) is the prepared graphene film layer thickness statistical graph of the little gap of the inventive method rotor-stator device.(data are added up 1000 graphene sheet layers altogether)
Fig. 5 (b) is the prepared graphene sheet layer mean sizes statistical graph of the little gap of the inventive method rotor-stator device.(data are added up 1000 graphene sheet layers altogether)
Fig. 6 (a) is the atomic force microscopy of the prepared Graphene of the large gap of the inventive method rotor-stator device.
Fig. 6 (b) is the transmission electron microscope photo of the prepared Graphene of the large gap of the inventive method rotor-stator device.
Fig. 7 (a) is the prepared graphene film layer thickness statistical graph of the large gap of the inventive method rotor-stator device.Data are added up 1000 graphene sheet layers altogether.
Fig. 7 (b) is the prepared graphene sheet layer mean sizes statistical graph of the large gap of the inventive method rotor-stator device.Data are added up 1000 graphene sheet layers altogether.
Embodiment
See Fig. 1, below in conjunction with embodiment, the present invention will be further described.
Embodiment 1, in the mixed solvent at 30% volume ratio Virahol and water, utilizes present method to prepare small size Graphene for embodiment.The little gap rotor-stator device of rotor-stator mixing tank that is used for producing high speed rotating fluid is in kind as shown in Fig. 2 (a), and concrete technology step is as follows:
Step 1: take the crystalline graphite powder 3.5g that particle diameter is less than 100 microns, be dispersed in the 30% volume ratio Virahol of 700mL and the mixed solvent of water, obtain the graphite dispersing solution that concentration is 5mg/ml;
Step 2: packing the graphite dispersing solution preparing into diameter is in the cylindrical tank of 10 centimetres, and the rotor-stator device of rotor-stator mixing tank is put into the central position below liquid level of solution;
Step 3: ON cycle cooling water system, makes the graphite dispersing solution in container remain on approximately 25 ℃ of room temperatures; By present method, process graphite dispersing solution 1 hour, rotor speed is 9000 to turn; Standing 1 hour of dispersion liquid after treatment, then upper strata dispersion liquid is taken out;
Step 4: the upper strata dispersion liquid taking out is packed in tophan pot, then with the centrifugal acceleration centrifugal treating 30min of 45g; After centrifuging treatment, collect supernatant liquid, obtain small size Graphene stable dispersions.
The atomic force microscope of the small size Graphene obtaining and transmission electron microscope photo are as shown in Fig. 4 (a), (b), and lamellar spacing and lamella size statistical graph are as shown in Fig. 5 (a), (b).
Embodiment 2, in the mixing solutions at water and ethanol, utilize present method to prepare small size Graphene for embodiment, the rotor-stator device of large gap rotor-stator mixing tank that is used for producing high speed rotating fluid is in kind as shown in Fig. 2 (b), and Fig. 3 (a), (b) are for generation of rotor-stator internal mixer section of structure and the force diagram of high rotating fluid in case study on implementation 2.
Concrete technology step is as follows:
Step 1: the mixing solutions 700mL of configuration water and ethanol, ethanol massfraction is 40%, and all the other are deionized water, and the crystalline graphite powder 7g that particle diameter is less than to 100 microns is scattered in wherein, obtains the graphite dispersing solution that concentration is 5mg/ml,
Step 2: it is in the cylindrical tank of 9.5 centimetres that the graphite dispersing solution preparing is transferred to diameter, and rotor-stator device is fixed on to the central position below liquid level;
Step 3: ON cycle cooling water system, makes the graphite dispersing solution in container remain on approximately 25 ℃ of room temperatures; By present method, process graphite dispersing solution 1 hour, rotor speed is 9000 to turn; Standing 1 hour of dispersion liquid after treatment, then upper strata dispersion liquid is taken out;
Step 4: the upper strata dispersion liquid taking out is packed in tophan pot, then with the centrifugal acceleration centrifugal treating 30min of 64g; After centrifuging treatment, collect supernatant liquid, obtain small size Graphene stable dispersions.
The atomic force microscopy of the small size Graphene obtaining is as shown in Fig. 6 (a), (b), and lamellar spacing and lamella size statistical graph are as shown in Fig. 7 (a), (b).
From above-described embodiment, lesser trochanter and little gap are more suitable for preparing small size Graphene.
Obviously, above-mentioned case study on implementation of the present invention is only used to clearly demonstrate example of the present invention, and the not restriction to embodiments of the present invention.For the those of ordinary skill in described field, can also make on the basis of the above description other multi-form variation or changes.Here cannot give all embodiments exhaustive, every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention amplifies out or change that belong to.
Claims (10)
1. a preparation method for small size Graphene, is characterized in that: the method concrete steps are as follows:
Step 1, by Graphite Powder 99 raw material and solvent, obtains graphite mixing solutions;
Step 2, puts into container by solution, the homogeneous head of the rotor-stator device of rotor-stator mixing tank is fixed on below liquid level simultaneously;
Step 3, opens cooling system and makes solution remain on certain temperature, opens rotor-stator mixing tank simultaneously and carries out high speed processing;
Step 4, carries out standing processing or centrifugation preparing solution, removes the particle of not peeling off completely, thereby collect supernatant liquor, obtains stable small size graphene dispersing solution.
2. the preparation method of a kind of small size Graphene according to claim 1, it is characterized in that: the solvent described in step 1 is one or more mixing in water and organic solvent, the mixture of ethanol, acetone, Virahol and water preferably, wherein organic solvent ratio is 10%-90%; Graphite raw material described in step 1 is not limit, preferably micro crystal graphite, crystalline flake graphite, expansible black lead, high orientation pyrolytic graphite.
3. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: the graphite mixing solutions starting point concentration described in step 1 is not limit, and preferred concentration is 1-30mg/ml.
4. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: in the device of rotor-stator described in step 2, the hole shape of stator surface is not limit, preferably circular hole; Rotor-stator device rotor shape is not limit, preferably blade type.
5. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: the rotor in the device of rotor-stator described in step 2 and the gap size between stator are 0.1 millimeter to 30 centimetres, and preferably gap is 0.5-10 millimeter.
6. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: the homogeneous head of the device of rotor-stator described in step 2 need to be fixed on below liquid level, and preferred position is the following central position of liquid level.
7. the preparation method of a kind of small size Graphene according to claim 1, it is characterized in that: described in step 3, open rotor-stator mixing tank and carry out high speed processing, the rotating speed of its treating processes rotor-stator mixing tank is that 2000-25000 turns, and preferred rotating speed is that 8000-15000 turns.
8. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: cooling system described in step 3 is that circulating liquid is cooling, a kind of in but of air cooling and electricity refrigeration, preferably circulating water.
9. the preparation method of a kind of small size Graphene according to claim 1, is characterized in that: the solution for the treatment of processes described in step 3 maintains the temperature at 0-80 ℃, and preferred solution temperature is 15-35 ℃.
10. the preparation method of a kind of small size Graphene according to claim 1, it is characterized in that: the 0.5-20 hour of time of repose described in step 4, described centrifugal treating acceleration is 25-5000g, centrifugation time 30-200 minute, preferred time of repose is 0.5-5 hour, preferred centrifugal acceleration is 35-500g, and preferred centrifugation time is 30-60 minute.
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| CN104370283A (en) * | 2014-10-23 | 2015-02-25 | 江阴碳谷科技有限公司 | Graphene stripping kettle, graphene production system and graphene production method |
| CN104772064A (en) * | 2015-03-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Method for preparing grapheme dispersion liquid |
| CN105731439A (en) * | 2016-01-28 | 2016-07-06 | 桐乡市合诚自动化技术有限公司 | Impinging-stream 3-Mach graphene production line |
| CN105800545A (en) * | 2016-03-18 | 2016-07-27 | 北京化工大学 | Method for preparing two-dimensional material through stripping |
| CN106672954A (en) * | 2017-01-20 | 2017-05-17 | 北京航空航天大学 | Method for preparing graphene two-dimensional material through liquid-phase stripping |
| CN106865530A (en) * | 2016-12-23 | 2017-06-20 | 成都新柯力化工科技有限公司 | A kind of method that stripping prepares the high-speed mixer of Graphene and its peels off Graphene |
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| CN104772064A (en) * | 2015-03-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Method for preparing grapheme dispersion liquid |
| CN107624105B (en) * | 2015-06-24 | 2021-08-31 | 嘉泉大学校产学协力团 | Preparation method and preparation device of high-quality graphene by utilizing shear flow |
| CN107624105A (en) * | 2015-06-24 | 2018-01-23 | 嘉泉大学校产学协力团 | Utilize the high-quality graphene preparation method and preparation facilities of shear flow |
| CN114572972A (en) * | 2015-10-13 | 2022-06-03 | 托马仕有限责任公司 | Apparatus and method for mass production of atomically thin two-dimensional materials including graphene |
| US11584650B2 (en) * | 2015-12-14 | 2023-02-21 | Baoshan Iron & Steel Co., Ltd. | Graphene oxide and method of production thereof |
| CN105731439A (en) * | 2016-01-28 | 2016-07-06 | 桐乡市合诚自动化技术有限公司 | Impinging-stream 3-Mach graphene production line |
| CN105800545A (en) * | 2016-03-18 | 2016-07-27 | 北京化工大学 | Method for preparing two-dimensional material through stripping |
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| CN108264039A (en) * | 2017-01-04 | 2018-07-10 | 中原大学 | To prepare the method for graphene |
| CN106672954A (en) * | 2017-01-20 | 2017-05-17 | 北京航空航天大学 | Method for preparing graphene two-dimensional material through liquid-phase stripping |
| CN106995212A (en) * | 2017-05-05 | 2017-08-01 | 李源作 | A kind of mechanical shearing peels off the dilute method of production graphite |
| CN109179383A (en) * | 2018-01-17 | 2019-01-11 | 中原大学 | Graphene structure, method for preparing graphene and lithium ion battery electrode |
| CN109179383B (en) * | 2018-01-17 | 2020-12-29 | 中原大学 | Graphene structure, method for preparing graphene and lithium ion battery electrode |
| CN108358196A (en) * | 2018-04-21 | 2018-08-03 | 广东明路电力电子有限公司 | Graphene sorting process |
| CN108795393A (en) * | 2018-06-08 | 2018-11-13 | 东莞市鸿亿导热材料有限公司 | A kind of production method of carbon fiber flexible graphite tablets |
| CN108795393B (en) * | 2018-06-08 | 2021-01-29 | 东莞市鸿亿导热材料有限公司 | Method for manufacturing carbon fiber flexible graphite sheet |
| CN109607520A (en) * | 2018-12-28 | 2019-04-12 | 福建翔丰华新能源材料有限公司 | A kind of small size single-layer graphene and preparation method thereof |
| CN109607520B (en) * | 2018-12-28 | 2022-09-20 | 福建翔丰华新能源材料有限公司 | Small-size single-layer graphene and preparation method thereof |
| CN109502576A (en) * | 2019-01-07 | 2019-03-22 | 江苏省特种设备安全监督检验研究院 | The sealed helical flow field graphene nanometer sheet preparation facilities of ultrahigh speed and preparation method |
| CN111484005A (en) * | 2020-01-17 | 2020-08-04 | 北京清烯科技有限公司 | A device for high-efficient manufacturing large tracts of land graphite alkene |
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