CN109052314A - A method of removing multilayer two-dimension material - Google Patents
A method of removing multilayer two-dimension material Download PDFInfo
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- CN109052314A CN109052314A CN201811083699.7A CN201811083699A CN109052314A CN 109052314 A CN109052314 A CN 109052314A CN 201811083699 A CN201811083699 A CN 201811083699A CN 109052314 A CN109052314 A CN 109052314A
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- multilayer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
- B81C1/0038—Processes for creating layers of materials not provided for in groups B81C1/00357 - B81C1/00373
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention discloses a kind of method for removing multilayer two-dimension material, wherein comprising steps of providing the first chelating agent and the second chelating agent, the ability of the first chelant ties metal ion is greater than the ability of the second chelant ties metal ion;Under vacuum conditions, multilayer two-dimension material is mixed with first chelating agent and nonionic water, stirring makes first chelating agent be inserted into the multilayer two-dimension material between layers, obtains mixed solution;The second chelating agent for having chelated metal ion is added in the mixed solution, stirs the predetermined time under predetermined temperature, makes the separation of multilayer two-dimension material generation between layers in the mixed solution.The simple and environmentally-friendly easy realization of the method for the present invention, and charge stripping efficiency is high, and single layer or few layer two-dimensional material can quickly be made.
Description
Technical field
The present invention relates to two-dimensional material preparation field more particularly to a kind of methods for removing multilayer two-dimension material.
Background technique
Two-dimensional material refer to electronics only can on the non-nanosize (1-100nm) of two dimensions free movement material,
Such as nano thin-film, superlattices, Quantum Well etc..The chemical property of two-dimensional material shows significantly not with the difference of the number of plies
Together, existing two-dimensional material usually exists in a manner of multilayer stacking, i.e., two-dimensional material passes through Van der Waals between layers
Interaction is combined together.And the two-dimensional material of single layer or few layer has the electric conductivity of superelevation, the heating conduction of superelevation
With the mechanical strength of superelevation, it is referred to as the king of material.Therefore every country all pays much attention to single layer or lacks layer two-dimensional material
Development work.
The method for commonly preparing single layer or few layer two-dimensional material on the market now is mainly that oxidation-reduction method and meteorology are heavy
Area method.However, oxidation-reduction method will use a large amount of strong acid and strong base, environment is polluted;And vapor phase deposition rule cost is very high, and
And yield is very low.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of sides for removing multilayer two-dimension material
Method, it is intended to which solving the prior art, there are low efficiencys, at high cost and environment easy to pollute preparing single layer or few layer two-dimensional material
Problem.
Technical scheme is as follows:
A method of removing multilayer two-dimension material, wherein comprising steps of
The first chelating agent and the second chelating agent are provided, the ability of the first chelant ties metal ion is greater than second chela
The ability of mixture chelated metal ions;
Under vacuum conditions, multilayer two-dimension material is mixed with first chelating agent and nonionic water, stirring makes described the
One chelating agent is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
Second chelating agent is mixed with metal ion, the second chelating agent with metal ion-chelant is made;
Second chelating agent with metal ion-chelant is added in the mixed solution, is stirred under predetermined temperature pre-
It fixes time, makes the separation of multilayer two-dimension material generation between layers in the mixed solution.
The method of the removing multilayer two-dimension material, wherein first chelating agent is aminotrimethylene phosphate, ethylenediamine
Four methene sodium phosphates, 1-hydroxy ethylidene-1,1-diphosphonic acid, diethylene triamine pentamethylene phosphonic, Sodium Polyacrylate, the adjacent phenyl second of ethylenediamine two
Sour sodium, sodium tripolyphosphate, sodium pyrophosphate, tertiary sodium phosphate, sodium citrate, sodium gluconate, sodium potassium tartrate tetrahydrate, phosphate -1 2-,
2,4- butane tricarboxylates, 2- di guanidine-acetic acid, oneself is two by four methylenephosphonic acids and double 1,6- hexamethylene triamine, five methylenephosphonic acids
One of or it is a variety of.
The method of the removing multilayer two-dimension material, wherein second chelating agent is diacetayl amide tetraacethyl sodium, poly- day
Aspartic acid sodium, polyepoxy sodium succinate, maleic acid-acrylic acid copolymer, five sodium of diethylene triamine pentacetic acid (DTPA), nitrilotriacetic acid
Sodium, one of sub- nitrogen base sodium diacelate and sodium metasilicate or a variety of.
It is described removing multilayer two-dimension material method, wherein the metal ion be iron, copper, zinc, calcium, manganese, magnesium, titanium,
Cobalt, nickel, one of strontium and chromium or a variety of.
The method of the removing multilayer two-dimension material, wherein second chelating agent with metal ion-chelant is added
When the mixed solution, further comprise the steps of:
The Ph value for adjusting the mixed solution is 1-12.
The method of the removing multilayer two-dimension material, wherein the multilayer two-dimension material is crystalline flake graphite, crystalline flake graphite
One of alkene, phosphorus, silicon carbide and boron nitride are a variety of.
The method of the removing multilayer two-dimension material, wherein the predetermined temperature is 60-80 DEG C, and the predetermined time is
1-2h。
The method of the removing multilayer two-dimension material, wherein second chelating agent with metal ion-chelant is added
In the mixed solution, the predetermined time is stirred under predetermined temperature, sends out the multilayer two-dimension material in the mixed solution
In the step of raw separation between layers, the mixing speed is 300-5000 revolutions per seconds.
The utility model has the advantages that the present invention provides a kind of method for removing multilayer two-dimension material, by advance inserting the first chelating agent
Enter to the multilayer two-dimension material between layers, then by the second chelating agent for having chelated metal ion and the multilayer two
Tie up material mixing, in a heated condition stirring make the metal ion chelated in the second chelating agent be detached from and with first chelating agent
Chelating, the metal ion is during occurring disengaging and with the first chelant ties, since the quality of metal ion compares
Greatly, energy can be generated in mutual collision, is destroyed so as to cause the Van der Waals force of multilayer two-dimension material between layers, from
And layer is caused to fall off, and then obtain the less two-dimensional material of the number of plies.
Detailed description of the invention
Fig. 1 is a kind of flow chart for the method preferred embodiment for removing multilayer two-dimension material of the present invention.
Fig. 2 is multilayer two-dimension material stripping process schematic diagram of the present invention.
Specific embodiment
The present invention provides a kind of method for removing multilayer two-dimension material, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
Referring to Fig. 1, Fig. 1 is a kind of process of method preferred embodiment for removing multilayer two-dimension material provided by the invention
Figure, wherein as shown, comprising steps of
S10, the first chelating agent and the second chelating agent are provided, the ability of the first chelant ties metal ion is greater than described the
The ability of two chelant ties metal ions;
S20, under vacuum conditions, multilayer two-dimension material is mixed with first chelating agent and nonionic water, and stirring makes institute
It states the first chelating agent and is inserted into the multilayer two-dimension material between layers, obtain mixed solution;
S30, second chelating agent is mixed with metal ion, the second chelating agent with metal ion-chelant is made;
S40, second chelating agent with metal ion-chelant is added in the mixed solution, is stirred under predetermined temperature
The predetermined time is mixed, the separation of multilayer two-dimension material generation between layers in the mixed solution is made.
In the present embodiment, the first chelating agent is mixed with the multilayer two-dimension material and nonionic water in advance,
So that first chelating agent is inserted into the multilayer two-dimension material between layers in whipping process, obtains mixed solution;
Previously prepared the second chelating agent with metal ion-chelant is added in the mixed solution again, due to the first chelant ties
The ability of metal ion is greater than the ability of the second chelant ties metal ion, and therefore, stirring can make in a heated condition
The metal ion that is chelated in second chelating agent be detached from and with first chelant ties, as shown in Fig. 2, due to metal ion
Quality is bigger, and for the metal ion during disengaging occurring and with the first chelant ties, the metal ion is in phase
Energy mutually can be generated when collision, is corrupted such that multilayer two so as to cause the Van der Waals force of multilayer two-dimension material between layers
The separation of material generation between layers is tieed up, and then obtains the less two-dimensional material of the number of plies.
The simple and environmentally-friendly easy realization of method of removing multilayer two-dimension material provided in this embodiment, and charge stripping efficiency is high, it can
Quickly obtained single layer or few layer two-dimensional material.
In a preferred embodiment, the metal ion chelating capacity of first chelating agent is greater than the second chelating agent
Metal ion chelating capacity, the metal chelation abilities of chelating agent were both related with the alkaline size of its dentate, also and at alkali
The Acidity of group is related, and the coordination atom of usual basic functionality is nitrogen, sulphur, oxygen etc., their electronegativity is suitable by nitrogen sulphur oxygen
Sequence is successively successively decreased, therefore its alkaline coordination ability is incremented by successively by nitrogen sulphur oxygen sequence;On the other hand, the acidic groups in chelating agent
Group (COOH, OH and SH) is stronger, then the trend for forming chelate of metal ion is bigger, therefore, on the appropriate location of chelating agent
The group for introducing electronegativity increases its acidity, so that it may improve the metal ion chelating capacity of the chelating agent.Preferably, institute
Stating the first chelating agent is aminotrimethylene phosphate, ethylenediamine tetraacetic methene sodium phosphate, 1-hydroxy ethylidene-1,1-diphosphonic acid, five first of diethylenetriamine
Fork phosphonic acids, Sodium Polyacrylate, the adjacent sodium of ethylenediamine two, sodium tripolyphosphate, sodium pyrophosphate, tertiary sodium phosphate, sodium citrate,
Sodium gluconate, sodium potassium tartrate tetrahydrate, 2- phosphate -1,2,4- butane tricarboxylate, 2- di guanidine-acetic acid, oneself two press four methenes
One of phosphonic acids and double 1,6- hexamethylene triamine, five methylenephosphonic acids etc. are a variety of, but not limited to this.Preferably, second chela
Mixture is diacetayl amide tetraacethyl sodium, poly (sodium aspartate), polyepoxy sodium succinate, maleic acid-acrylic acid copolymer, divinyl
Pentetate Pentasodium, sodium nitrilo triacetate, one of sub- nitrogen base sodium diacelate and sodium metasilicate or a variety of, but be not limited to
This.
In a preferred embodiment, the metal ion be iron, copper, zinc, calcium, manganese, magnesium, titanium, cobalt, nickel, strontium and
One of chromium is a variety of.
In a preferred embodiment, first chelating agent is 1-hydroxy ethylidene-1,1-diphosphonic acid, second chelating agent
For sub- nitrogen base sodium diacelate, and second chelant ties iron ion.Due to 1-hydroxy ethylidene-1,1-diphosphonic acid chelates ferric ions
Ability is better than the ability of the sub- nitrogen base sodium diacelate chelates ferric ions, if at this time by first chelating agent and the chelating
Second chelating agent of iron ion is stirred, then iron ion is detached from second chelating agent, and the iron ion after disengaging will
With first chelant ties.
In a preferred embodiment, to prevent the multilayer two-dimension materials from oxidizing, the present embodiment preferably exists
Under vacuum condition, first chelating agent, multilayer two-dimension material are mixed with nonionic water, stirring inserts first chelating agent
Enter to the multilayer two-dimension material between layers, obtains mixed solution.
In a preferred embodiment, described mix is being added with the second chelating agent of metal ion-chelant by described
When solution, further comprising the steps of: and adjusting the Ph value of the mixed solution is 1-12.Within the scope of the Ph value, the metal ion is more
Be easy be detached from second chelating agent, and again with the first chelant ties.
Preferably, when the mixed solution is added in second chelating agent with metal ion-chelant, then in 60-80
1-2h is stirred under conditions of DEG C.Under the conditions of 60-80 DEG C, the activity performance of metal ion can be increased, so that metal ion
It is more easily detached from the second chelating agent, stirs 1-2h, the metal ion being detached from can be made sufficiently to send out with first chelating agent
Raw chelating.
It is furthermore preferred that when being stirred to the second chelating agent and mixed solution that have chelated metal ion, the stirring
Speed is 300-5000 revolutions per seconds, and the charge stripping efficiency of multilayer two-dimension material can be promoted in the mixing speed.
In a preferred embodiment, the multilayer two-dimension material is crystalline flake graphite, crystalline flake graphite alkene, phosphorus, carbonization
One of silicon and boron nitride are a variety of, but not limited to this.
Preferably, the multilayer two-dimension material is the two-dimensional material that the number of plies is greater than 3, and few layer two-dimensional material is that the number of plies is small
In the two-dimensional material for being equal to 3, for example, three layers of two-dimensional material, two layers of two-dimensional material, single layer two-dimensional material.
It is further explained below by the specific embodiment method for removing multilayer two-dimension material a kind of to the present invention
Illustrate:
Embodiment 1
1), under vacuum conditions, multilayer two-dimension material is mixed with aminotrimethylene phosphate and nonionic water, stirring makes described
Aminotrimethylene phosphate is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
2) diacetayl amide tetraacethyl sodium is mixed with copper ion, the diacetayl amide tetraacethyl sodium of chelating copper ion is made;
3), the diacetayl amide tetraacethyl sodium of the chelating copper ion is added in the mixed solution, under conditions of 60 DEG C, with
1000 revolutions per seconds of mixing speed stirs 1h, so that the copper ion is detached from the diacetayl amide tetraacethyl sodium, after disengaging
Copper ion again with the aminotrimethylene phosphate occur chelatropic reaction, in the reaction process, the copper ion mutually it
Between energy is generated because colliding, this energy causes the Van der Waals force of multilayer two-dimension material to be between layers destroyed, from
And make the separation of multilayer two-dimension material generation between layers in the mixed solution, obtain the two-dimentional material of single layer or few layer
Material.
Embodiment 2
1), under vacuum conditions, multilayer two-dimension material is mixed with 1-hydroxy ethylidene-1,1-diphosphonic acid and nonionic water, stirring makes described
1-hydroxy ethylidene-1,1-diphosphonic acid is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
2) sub- nitrogen base sodium diacelate is mixed with iron ion, the sub- nitrogen base sodium diacelate of chelates ferric ions is made;
3), the sub- nitrogen base sodium diacelate of the chelates ferric ions is added in the mixed solution, under conditions of 70 DEG C, with
2000 revolutions per seconds of mixing speed stirs 2h, so that the iron ion is detached from the sub- nitrogen base sodium diacelate, after disengaging
Again with the 1-hydroxy ethylidene-1,1-diphosphonic acid chelatropic reaction occurs for iron ion, and in the reaction process, the iron ion is from each other
Energy is generated because colliding, this energy causes the Van der Waals force of multilayer two-dimension material to be between layers destroyed, thus
So that separation between layers occurs for the multilayer two-dimension material in the mixed solution, the two-dimentional material of single layer or few layer is obtained
Material.
Embodiment 3
1) multilayer two-dimension material is mixed with diethylene triamine pentamethylene phosphonic and nonionic water, under vacuum conditions, is stirred
So that the diethylene triamine pentamethylene phosphonic is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
2) poly (sodium aspartate) is mixed with zinc ion, the poly (sodium aspartate) of chelated zinc ions is made;
3), the poly (sodium aspartate) of the chelated zinc ions is added in the mixed solution, under conditions of 75 DEG C, with 3000
Revolutions per second mixing speed stir 1.5h so that the zinc ion is detached from the poly (sodium aspartate), the zinc after disengaging from
With diethylene triamine pentamethylene phosphonic chelatropic reaction occurs for son again, and in the reaction process, the zinc ion is from each other because of hair
Life collides and generates energy, and this energy causes the Van der Waals force of multilayer two-dimension material to be between layers destroyed, so that
Separation between layers occurs for the multilayer two-dimension material in the mixed solution, obtains the two-dimensional material of single layer or few layer.
Embodiment 4
1), under vacuum conditions, multilayer two-dimension material is mixed with sodium citrate and nonionic water, stirring makes the citric acid
Sodium is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
2) five sodium of diethylene triamine pentacetic acid (DTPA) is mixed with calcium ion, the diethylene triamine pentacetic acid (DTPA) five of chelating calcium ion is made
Sodium;
3), five sodium of diethylene triamine pentacetic acid (DTPA) of the chelating calcium ion is added in the mixed solution, in 75 DEG C of condition
Under, 1.5h is stirred with 3000 revolutions per seconds of mixing speed, so that the calcium ion and five sodium of diethylene triamine pentacetic acid (DTPA) occur
It is detached from, with sodium citrate chelatropic reaction occurs for the calcium ion after disengaging again, and in the reaction process, the calcium ion is from each other
Energy is generated because colliding, this energy causes the Van der Waals force of multilayer two-dimension material to be between layers destroyed, thus
So that separation between layers occurs for the multilayer two-dimension material in the mixed solution, the two-dimentional material of single layer or few layer is obtained
Material.
In conclusion the present invention provides a kind of method for removing multilayer two-dimension material, by advance inserting the first chelating agent
Enter to the multilayer two-dimension material between layers, then by the second chelating agent for having chelated metal ion and the multilayer two
Tie up material mixing, in a heated condition stirring make the metal ion chelated in the second chelating agent be detached from and with first chelating agent
Chelating, the metal ion is during occurring disengaging and with the first chelant ties, since the quality of metal ion compares
Greatly, energy can be generated in mutual collision, is destroyed so as to cause the Van der Waals force of multilayer two-dimension material between layers, from
And layer is caused to fall off, and then obtain the less two-dimensional material of the number of plies.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (8)
1. a kind of method for removing multilayer two-dimension material, which is characterized in that comprising steps of
The first chelating agent and the second chelating agent are provided, the ability of the first chelant ties metal ion is greater than second chela
The ability of mixture chelated metal ions;
Under vacuum conditions, multilayer two-dimension material is mixed with first chelating agent and nonionic water, stirring makes described the
One chelating agent is inserted into the multilayer two-dimension material between layers, obtains mixed solution;
Second chelating agent is mixed with metal ion, the second chelating agent with metal ion-chelant is made;
Second chelating agent with metal ion-chelant is added in the mixed solution, is stirred under predetermined temperature pre-
It fixes time, makes the separation of multilayer two-dimension material generation between layers in the mixed solution.
2. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that first chelating agent is amino
Three methene phosphoric acid, ethylenediamine tetraacetic methene sodium phosphate, 1-hydroxy ethylidene-1,1-diphosphonic acid, diethylene triamine pentamethylene phosphonic, Sodium Polyacrylate,
The adjacent sodium of ethylenediamine two, sodium tripolyphosphate, sodium pyrophosphate, tertiary sodium phosphate, sodium citrate, sodium gluconate, tartaric acid
Potassium sodium, 2- phosphate -1,2,4- butane tricarboxylate, 2- di guanidine-acetic acid, oneself two by four methylenephosphonic acids and double 1,6- it is sub- oneself
One of five methylenephosphonic acid of base triamine is a variety of.
3. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that second chelating agent is diethyl
Amide tetraacethyl sodium, poly (sodium aspartate), polyepoxy sodium succinate, maleic acid-acrylic acid copolymer, diethylene triamine pentacetic acid (DTPA)
Five sodium, sodium nitrilo triacetate, one of sub- nitrogen base sodium diacelate and sodium metasilicate or a variety of.
4. according to claim 1 remove multilayer two-dimension material method, which is characterized in that the metal ion be iron, copper,
Zinc, calcium, manganese, magnesium, titanium, cobalt, nickel, one of strontium and chromium or a variety of.
5. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that will described and metal ion-chelant
The second chelating agent be added the mixed solution when, further comprise the steps of:
The Ph value for adjusting the mixed solution is 1-12.
6. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that the multilayer two-dimension material is squama
One of piece graphite, crystalline flake graphite alkene, phosphorus, silicon carbide and boron nitride are a variety of.
7. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that the predetermined temperature is 60-80
DEG C, the predetermined time is 1-2h.
8. removing the method for multilayer two-dimension material according to claim 1, which is characterized in that will described and metal ion-chelant
The second chelating agent be added in the mixed solution, stir the predetermined time under predetermined temperature, make in the mixed solution
Multilayer two-dimension material the step of separation between layers occurs in, the mixing speed is 300-5000 revolutions per seconds.
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CN111320150A (en) * | 2020-04-17 | 2020-06-23 | 四川大学 | Method for preparing hexagonal boron nitride nanosheets by ion insertion ultrasonic stripping of alkali metal salt |
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CN108423667A (en) * | 2018-05-29 | 2018-08-21 | 李训祺 | A kind of graphene production technology |
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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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CN111137866A (en) * | 2020-01-10 | 2020-05-12 | 中国南方电网有限责任公司电网技术研究中心 | Method for preparing boron nitride nanosheet by efficiently stripping h-BN |
CN111320150A (en) * | 2020-04-17 | 2020-06-23 | 四川大学 | Method for preparing hexagonal boron nitride nanosheets by ion insertion ultrasonic stripping of alkali metal salt |
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