CN109052314B - Method for stripping multilayer two-dimensional material - Google Patents
Method for stripping multilayer two-dimensional material Download PDFInfo
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- CN109052314B CN109052314B CN201811083699.7A CN201811083699A CN109052314B CN 109052314 B CN109052314 B CN 109052314B CN 201811083699 A CN201811083699 A CN 201811083699A CN 109052314 B CN109052314 B CN 109052314B
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
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Abstract
The invention discloses a method for stripping a multilayer two-dimensional material, which comprises the following steps: providing a first chelant and a second chelant, the first chelant having a greater ability to chelate metal ions than the second chelant; under the vacuum condition, mixing a plurality of layers of two-dimensional materials with the first chelating agent and non-ionic water, and stirring to enable the first chelating agent to be inserted between layers of the plurality of layers of two-dimensional materials to obtain a mixed solution; and adding a second chelating agent chelated with metal ions into the mixed solution, and stirring for a preset time under a preset temperature condition to separate the layers of the two-dimensional materials in the mixed solution. The method is simple, environment-friendly and easy to realize, has high stripping efficiency, and can quickly prepare the single-layer or few-layer two-dimensional material.
Description
Technical Field
The invention relates to the field of two-dimensional material preparation, in particular to a method for stripping a multilayer two-dimensional material.
Background
A two-dimensional material refers to a material in which electrons are free to move only in two dimensions, on a non-nanoscale (1-100 nm) such as a nano-film, a superlattice, a quantum well, etc. The chemistry of two-dimensional materials varies significantly with the number of layers, and existing two-dimensional materials typically exist in a multi-layer stack, i.e., layers of two-dimensional material are held together by van der waals interactions. The single-layer or few-layer two-dimensional material has ultrahigh electric conductivity, ultrahigh heat conductivity and ultrahigh mechanical strength, and is called as the king of materials. Therefore, the research and development work of single-layer or few-layer two-dimensional materials is very important in all countries.
The methods commonly used in the market today for the preparation of single or few layer two-dimensional materials are mainly redox and gas-image deposition methods. However, the redox method uses a large amount of strong acid and strong base, and pollutes the environment; the weather deposition method is very costly and yields are low.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a method for peeling off a multi-layer two-dimensional material, which aims to solve the problems of low efficiency, high cost and easy environmental pollution in the preparation of a single-layer or few-layer two-dimensional material in the prior art.
The technical scheme of the invention is as follows:
a method of exfoliating a multi-layer two-dimensional material comprising the steps of:
providing a first chelant and a second chelant, the first chelant having a greater ability to chelate metal ions than the second chelant;
under the vacuum condition, mixing a plurality of layers of two-dimensional materials with the first chelating agent and non-ionic water, and stirring to enable the first chelating agent to be inserted between layers of the plurality of layers of two-dimensional materials to obtain a mixed solution;
mixing the second chelating agent with metal ions to prepare a second chelating agent chelated with the metal ions;
and adding the second chelating agent chelated with the metal ions into the mixed solution, and stirring for a preset time under a preset temperature condition to separate the layers of the two-dimensional materials in the mixed solution.
The method for stripping the multilayer two-dimensional material is characterized in that the first chelating agent is one or more of aminotrimethylene phosphoric acid, ethylene diamine tetra methylene sodium phosphate, hydroxyethylidene diphosphonic acid, diethylenetriamine pentamethylene phosphonic acid, sodium polyacrylate, ethylenediamine dipentyl sodium acetate, sodium tripolyphosphate, sodium pyrophosphate, trisodium phosphate, sodium citrate, sodium gluconate, potassium sodium tartrate, 2-phosphate-1, 2, 4-tricarboxylic acid butane, 2-hydroxyphosphoric acid acetic acid, hexamethylene tetramethyene phosphonic acid and bis-1, 6-hexylidene triamine pentamethylene phosphonic acid.
The method for stripping the multilayer two-dimensional material is characterized in that the second chelating agent is one or more of sodium diacetate, sodium polyaspartate, sodium polyepoxysuccinate, maleic acid-acrylic acid copolymer, pentasodium diethylenetriamine pentaacetate, sodium nitrilotriacetate, sodium nitrilo-diacetate and sodium silicate.
The method for stripping the multilayer two-dimensional material is characterized in that the metal ions are one or more of iron, copper, zinc, calcium, manganese, magnesium, titanium, cobalt, nickel, strontium and chromium.
The method for peeling off the multilayer two-dimensional material, wherein the second chelating agent that chelates with metal ions is added to the mixed solution, further comprising the steps of:
and adjusting the pH value of the mixed solution to be 1-12.
The method for stripping the multilayer two-dimensional material is characterized in that the multilayer two-dimensional material is one or more of crystalline flake graphite, crystalline flake graphene, phosphorus, silicon carbide and boron nitride.
The method for stripping the multilayer two-dimensional material is characterized in that the preset temperature is 60-80 ℃, and the preset time is 1-2 h.
The method for stripping the multilayer two-dimensional material comprises the steps of adding the second chelating agent chelated with the metal ions into the mixed solution, stirring for a preset time under a preset temperature condition, and enabling the multilayer two-dimensional material in the mixed solution to be separated from layer to layer, wherein the stirring speed is 300-5000 revolutions per second.
Has the advantages that: the invention provides a method for stripping a multilayer two-dimensional material, which comprises the steps of inserting a first chelating agent between layers of the multilayer two-dimensional material in advance, mixing a second chelating agent chelated with metal ions with the multilayer two-dimensional material, stirring under a heating condition to enable the chelated metal ions in the second chelating agent to be separated from the first chelating agent and be chelated with the first chelating agent, wherein in the process that the metal ions are separated from the first chelating agent and are chelated with the first chelating agent, due to the fact that the metal ions have larger mass, energy can be generated when the metal ions collide with each other, Van der Waals force between the layers of the multilayer two-dimensional material is damaged, so that the layers are stripped, and the two-dimensional material with the smaller number of layers is obtained.
Drawings
FIG. 1 is a flow chart of a preferred embodiment of a method for peeling a multilayer two-dimensional material according to the present invention.
FIG. 2 is a schematic diagram of a multi-layer two-dimensional material release process of the present invention.
Detailed Description
The present invention provides a method for peeling off a multilayer two-dimensional material, and the present invention will be described in further detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a flow chart of a preferred embodiment of a method for peeling off a multi-layer two-dimensional material according to the present invention, wherein the method comprises the following steps:
s10, providing a first chelating agent and a second chelating agent, the first chelating agent having a greater ability to chelate metal ions than the second chelating agent;
s20, mixing the multilayer two-dimensional material, the first chelating agent and non-ionic water under a vacuum condition, and stirring to enable the first chelating agent to be inserted between layers of the multilayer two-dimensional material to obtain a mixed solution;
s30, mixing the second chelating agent with metal ions to prepare a second chelating agent chelated with the metal ions;
and S40, adding the second chelating agent chelated with the metal ions into the mixed solution, and stirring for a preset time under a preset temperature condition to enable the layers of the two-dimensional materials in the mixed solution to be separated layer by layer.
In this embodiment, a first chelating agent is mixed with the multilayer two-dimensional material and the non-ionic water in advance, and the first chelating agent is inserted between layers of the multilayer two-dimensional material during stirring to obtain a mixed solution; and adding a second chelating agent chelated with metal ions, which is prepared in advance, into the mixed solution, wherein the metal ions chelated in the second chelating agent can be separated and chelated with the first chelating agent by stirring under the heating condition because the metal ions chelated in the second chelating agent have higher metal ion chelating capacity than the second chelating agent, as shown in fig. 2, because the metal ions have larger mass, in the process of separating and chelating with the first chelating agent, the metal ions can generate energy when colliding with each other, so that the van der waals force between layers of the multilayer two-dimensional material is damaged, the multilayer two-dimensional material is separated from layer to layer, and the two-dimensional material with fewer layers is obtained.
The method for stripping the multilayer two-dimensional material is simple, environment-friendly and easy to implement, has high stripping efficiency, and can be used for quickly preparing the single-layer or few-layer two-dimensional material.
In a preferred embodiment, the metal ion chelating capacity of the first chelating agent is greater than that of the second chelating agent, the metal chelating capacity of the chelating agent is related to the alkalinity of the ligand and the acidity of the salt forming group, the coordination atoms of the basic functional group are nitrogen, sulfur, oxygen and the like, the electronegativity of the coordination atoms is decreased in the order of nitrogen, sulfur and oxygen, so that the basic coordination capacity is increased in the order of nitrogen, sulfur and oxygen; on the other hand, since the stronger the acidic groups (COOH, OH, and SH) in the chelating agent, the greater the tendency to form a metal ion chelate, the more the chelating agent is acidic by introducing electronegative groups to appropriate positions, and the metal ion chelating ability of the chelating agent can be improved. Preferably, the first chelating agent is one or more of aminotrimethylene phosphoric acid, sodium ethylene diamine tetra methylene phosphate, hydroxyethylidene diphosphonic acid, diethylenetriamine pentamethylene phosphonic acid, sodium polyacrylate, sodium ethylenediamine dipentyl acetate, sodium tripolyphosphate, sodium pyrophosphate, trisodium phosphate, sodium citrate, sodium gluconate, potassium sodium tartrate, 2-phospho-1, 2, 4-butane tricarboxylate, 2-hydroxyphosphonoacetic acid, hexamethylene tetramethyene phosphonic acid, bis 1, 6-hexamethylene triamine pentamethylene phosphonic acid, and the like, but is not limited thereto. Preferably, the second chelating agent is one or more of, but not limited to, sodium diacetate, sodium polyaspartate, sodium polyepoxysuccinate, maleic acid-acrylic acid copolymer, pentasodium diethylenetriaminepentaacetate, sodium nitrilotriacetate, sodium nitrilo-diacetate, and sodium silicate.
In a preferred embodiment, the metal ion is one or more of iron, copper, zinc, calcium, manganese, magnesium, titanium, cobalt, nickel, strontium and chromium.
In a preferred embodiment, the first chelating agent is hydroxyethylidene diphosphonic acid, the second chelating agent is sodium nitrilo diacetate, and the second chelating agent chelates iron ions. Because the iron ion chelating ability of the hydroxyethylidene diphosphonic acid is stronger than that of the sodium nitrilodiacetate, if the first chelating agent and the second chelating agent chelated with the iron ions are stirred, the iron ions are separated from the second chelating agent, and the separated iron ions are chelated with the first chelating agent.
In a preferred embodiment, in order to prevent the multilayer two-dimensional material from being oxidized, in this embodiment, the first chelating agent, the multilayer two-dimensional material and the non-ionic water are preferably mixed under vacuum, and the mixture solution is obtained by stirring the mixture so that the first chelating agent is inserted between layers of the multilayer two-dimensional material.
In a preferred embodiment, when the second chelating agent that chelates with metal ions is added to the mixed solution, the method further comprises the steps of: and adjusting the pH value of the mixed solution to be 1-12. Within this Ph range, the metal ion is more readily dissociated from the second chelating agent and re-chelated with the first chelating agent.
Preferably, when the second chelating agent chelating metal ions is added to the mixed solution, it is stirred at 60 to 80 ℃ for 1 to 2 hours. Under the condition of 60-80 ℃, the mobility of metal ions can be increased, so that the metal ions are more easily separated from the second chelating agent, and the separated metal ions can be fully chelated with the first chelating agent by stirring for 1-2 h.
More preferably, when the second chelating agent chelated with the metal ions and the mixed solution are stirred, the stirring speed is 300-.
In a preferred embodiment, the multilayer two-dimensional material is one or more of flake graphite, flake graphene, phosphorus, silicon carbide, and boron nitride, but is not limited thereto.
Preferably, the multilayer two-dimensional material is a two-dimensional material with the number of layers greater than 3, and the few-layer two-dimensional material is a two-dimensional material with the number of layers less than or equal to 3, such as a three-layer two-dimensional material, a two-layer two-dimensional material, and a single-layer two-dimensional material.
The method of the invention for stripping a multilayer two-dimensional material is further illustrated by the following specific examples:
example 1
1) Mixing a plurality of layers of two-dimensional materials with amino trimethylene phosphate and non-ionic water under a vacuum condition, and stirring to enable the amino trimethylene phosphate to be inserted between layers of the plurality of layers of two-dimensional materials to obtain a mixed solution;
2) mixing the sodium diacetylamide tetraacetate with the copper ions to prepare the sodium diacetylamide tetraacetate chelating the copper ions;
3) adding the copper ion-chelated sodium diacetylamide tetraacetate into the mixed solution, and stirring at 60 ℃ for 1h at a stirring speed of 1000 revolutions per second to separate the copper ions from the sodium diacetylamide tetraacetate, wherein the separated copper ions and the amino trimethylene phosphoric acid undergo a chelation reaction again, and in the reaction process, the copper ions collide with each other to generate energy, and the energy causes Van der Waals force between layers of the multilayer two-dimensional material to be destroyed, so that the multilayer two-dimensional material in the mixed solution is separated from layer to layer, and a single-layer or few-layer two-dimensional material is obtained.
Example 2
1) Mixing a plurality of layers of two-dimensional materials with hydroxyethylidene diphosphonic acid and non-ionic water under a vacuum condition, and stirring to enable the hydroxyethylidene diphosphonic acid to be inserted between layers of the plurality of layers of two-dimensional materials to obtain a mixed solution;
2) mixing sodium nitrilo diacetate with iron ions to prepare the sodium nitrilo diacetate chelated with the iron ions;
3) adding the sodium nitrilo-diacetate chelating the iron ions into the mixed solution, stirring at the stirring speed of 2000 rpm for 2h at the temperature of 70 ℃, so that the iron ions are separated from the sodium nitrilo-diacetate, and the separated iron ions are subjected to a chelating reaction with the hydroxyethylidene diphosphonic acid again, wherein in the reaction process, the iron ions collide with each other to generate energy, and the energy causes van der Waals force between layers of the multilayer two-dimensional material to be damaged, so that the multilayer two-dimensional material in the mixed solution is subjected to layer-to-layer separation, and a single-layer or few-layer two-dimensional material is obtained.
Example 3
1) Mixing a multilayer two-dimensional material, diethylenetriamine pentamethylene phosphonic acid and non-ionic water under a vacuum condition, and stirring to enable the diethylenetriamine pentamethylene phosphonic acid to be inserted between layers of the multilayer two-dimensional material to obtain a mixed solution;
2) mixing the sodium polyaspartate with zinc ions to prepare the sodium polyaspartate chelated with the zinc ions;
3) adding the sodium polyaspartate chelating the zinc ions into the mixed solution, stirring for 1.5h at the stirring speed of 3000 revolutions per second at the temperature of 75 ℃, so that the zinc ions are separated from the sodium polyaspartate, and then the separated zinc ions and diethylenetriamine pentamethylene phosphonic acid generate a chelating reaction, in the reaction process, the zinc ions generate energy due to collision, and the energy causes van der Waals force between layers of the multilayer two-dimensional material to be destroyed, so that the multilayer two-dimensional material in the mixed solution is separated from layer to layer, and a single-layer or few-layer two-dimensional material is obtained.
Example 4
1) Mixing a plurality of layers of two-dimensional materials with sodium citrate and non-ionic water under a vacuum condition, and stirring to enable the sodium citrate to be inserted between the layers of the plurality of layers of two-dimensional materials to obtain a mixed solution;
2) mixing the diethylenetriaminepentaacetic acid pentasodium with calcium ions to prepare the diethylenetriaminepentaacetic acid pentasodium chelated with the calcium ions;
3) adding the calcium ion chelated diethylene triamine pentaacetic acid pentasodium into the mixed solution, stirring for 1.5h at the condition of 75 ℃ at the stirring speed of 3000 r/s, so that the calcium ions are separated from the diethylene triamine pentaacetic acid pentasodium, and then the separated calcium ions and the sodium citrate are subjected to chelation reaction, in the reaction process, the calcium ions generate energy due to collision, and the energy causes van der Waals force between layers of the multilayer two-dimensional material to be damaged, so that the multilayer two-dimensional material in the mixed solution is separated from layer to layer, and a single-layer or few-layer two-dimensional material is obtained.
In summary, the invention provides a method for peeling off a multilayer two-dimensional material, which includes inserting a first chelating agent between layers of the multilayer two-dimensional material in advance, mixing a second chelating agent chelating metal ions with the multilayer two-dimensional material, stirring under heating to separate the metal ions chelated in the second chelating agent from the first chelating agent, wherein in the process of separating and chelating the metal ions with the first chelating agent, the metal ions have a larger mass and generate energy when colliding with each other, so that van der waals force between the layers of the multilayer two-dimensional material is damaged, so that the layers fall off, and further the two-dimensional material with a smaller number of layers is obtained.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (3)
1. A method of exfoliating a multilayer two dimensional material comprising the steps of:
providing a first chelant and a second chelant, the first chelant having a greater ability to chelate metal ions than the second chelant;
under the vacuum condition, mixing a plurality of layers of two-dimensional materials with the first chelating agent and non-ionic water, stirring to enable the first chelating agent to be inserted between layers of the plurality of layers of two-dimensional materials to obtain a mixed solution, and adjusting the Ph value of the mixed solution to be 1-12;
mixing the second chelating agent with metal ions to prepare a second chelating agent chelated with the metal ions;
adding the second chelating agent chelated with the metal ions into the mixed solution, and stirring for 1-2h at the temperature of 60-80 ℃ to separate the layers of the multilayer two-dimensional material in the mixed solution;
the first chelating agent is one or more of aminotrimethylene phosphoric acid, ethylene diamine tetra methylene sodium phosphate, hydroxyethylidene diphosphonic acid, diethylenetriamine penta methylene phosphonic acid, sodium polyacrylate, ethylene diamine dipentyl sodium acetate, sodium tripolyphosphate, sodium pyrophosphate, trisodium phosphate, sodium citrate, sodium gluconate, potassium sodium tartrate, 2-phosphoric acid-1, 2, 4-tricarboxylic acid butane, 2-hydroxyphosphoric acid acetic acid, hexamethylene diamine tetra methylene phosphonic acid and bis-1, 6-hexamethylene triamine penta methylene phosphonic acid; the second chelating agent is one or more of sodium diacetate, sodium polyaspartate, polyepoxysuccinic acid sodium, maleic acid-acrylic acid copolymer, diethylene triamine pentaacetic acid pentasodium, nitrilo trisacetic acid sodium, nitrilo diacetic acid sodium and sodium silicate; the metal ions are one or more of copper, zinc, calcium, manganese, magnesium, titanium, cobalt, nickel, strontium and chromium.
2. The method of exfoliating a multilayer two-dimensional material as claimed in claim 1, wherein said multilayer two-dimensional material is one or more of flake graphite, flake graphene, phosphorus, silicon carbide, and boron nitride.
3. The method for peeling off a multilayer two-dimensional material as claimed in claim 1, wherein the step of adding the second chelating agent chelating with metal ions to the mixed solution and stirring for a predetermined time under a predetermined temperature condition to cause layer-to-layer separation of the multilayer two-dimensional material in the mixed solution is performed at a stirring speed of 300-.
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| JP2007137990A (en) * | 2005-11-17 | 2007-06-07 | Toei Kasei Kk | Exfoliating agent for organic silicon-based coat or metallic oxide-based coat and method for exfoliating the coat |
| US9991391B2 (en) * | 2008-07-25 | 2018-06-05 | The Board Of Trustees Of The Leland Stanford Junior University | Pristine and functionalized graphene materials |
| CN102701187B (en) * | 2011-07-13 | 2016-03-09 | 华东理工大学 | Graphene prepared by a kind of preparation method of Graphene and use the method |
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| WO2015189335A1 (en) * | 2014-06-12 | 2015-12-17 | Centre National De La Recherche Scientifique - Cnrs - | Aqueous and organic suspensions of exfoliated nanocarbon materials, method for making same and uses thereof |
| CN107032339B (en) * | 2017-06-20 | 2018-03-20 | 成都新柯力化工科技有限公司 | It is a kind of based on the electrostatic repulsion method that continuously stripping prepares graphene |
| CN107879333A (en) * | 2017-11-09 | 2018-04-06 | 哈尔滨万鑫石墨谷科技有限公司 | The high quality delamination material that a kind of stripping means of stratified material and stripping obtain |
| CN108249428B (en) * | 2018-01-23 | 2020-02-07 | 福州大学 | Method for preparing single-layer graphene based on electrolyte solvent hot-insertion lithium stripping |
| CN108264040A (en) * | 2018-01-26 | 2018-07-10 | 天元羲王控股有限公司 | Iron ion graphene production technology based on the reaction of multiphase quantum self coupling |
| CN108314022B (en) * | 2018-03-27 | 2020-06-05 | 广东聚石化学股份有限公司 | Method for preparing graphene by directly stripping ionic liquid |
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| CN108423669A (en) * | 2018-06-16 | 2018-08-21 | 西南交通大学 | The method that stripping method prepares graphene nanometer sheet |
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